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Sample records for mg-based amorphous ball-milled

  1. Ball-milling-induced crystallization and ball-milling effect on thermal crystallization kinetics in an amorphous FeMoSiB alloy

    International Nuclear Information System (INIS)

    Guo, F.Q.; Lu, K.

    1997-01-01

    Microstructure evolution in a melt-spun amorphous Fe 77.2 Mo 0.8 Si 9 B 13 alloy subjected to high-energy ball milling was investigated by means of X-ray diffraction (XRD), a transmission electron microscope (TEM), and a differential scanning calorimeter (DSC). It was found that during ball milling, crystallization occurs in the amorphous ribbon sample with precipitation of an α-Fe solid solution, and the amorphous sample crystallizes completely into a single α-Fe nanostructure (rather than α-Fe and borides as in the usual thermal crystallization products) when the milling time exceeds 135 hours. The volume fraction of material crystallized was found to be approximately proportional to the milling time. The fully crystallized sample with a single α-Fe nanophase exhibits an intrinsic thermal stability against phase separation upon annealing at high temperatures. The ball-milling effect on the subsequent thermal crystallization of the amorphous phase in an as-milled sample was studied by comparison of the crystallization products and kinetic parameters between the as-quenched amorphous sample and the as-milled sample was studied by comparison of the crystallization products and kinetic parameters between the as-quenched amorphous sample and the as-milled partially crystallized samples. The crystallization temperatures and activation energies for the crystallization processes of the residual amorphous phase were considerably decreased due to ball milling, indicating that ball milling has a significant effect on the depression of thermal stability of the residual amorphous phase

  2. Effect of the milling energy on the production and thermal stability of amorphous Mg50Ni50

    International Nuclear Information System (INIS)

    Guzman, D.; Ordonez, S.; Serafini, D.; Rojas, P.; Bustos, O.

    2009-01-01

    The effect of milling energy on the amorphisation process and subsequent thermal crystallization of Mg 50 Ni 50 was investigated. The amorphous Mg 50 Ni 50 was produced using a planetary mill (medium energy) with a ball to material weight ratio of 13:1, and a SPEX mill (high energy) with a ball to material weight ratio of 20:1. The results obtained by means of X-ray diffraction showed that it is possible to obtain an amorphous Mg 50 Ni 50 alloy, through both milling processes, starting of Ni powders and Mg turnings. However, the amorphisation process requires more time in the planetary mill (80-90 h) than in the SPEX mill (15-20 h), due to the difference in energy level and milling mechanism between these mills. The phase evolution during the amorphisation process is practically independent of the mill energy. In this way, it was observed that the mill conditions promoted an extensive refinement of the microstructure during the first hours of milling. The defects produced during this time led to the amorphisation of part of the system. This amorphous precursor suffers a mechanically induced crystallization into Mg 2 Ni, which is subsequently destabilized into amorphous Mg 50 Ni 50 . Based on the results obtained, it is proposed that the formation of amorphous precursor during mechanical milling of Mg and Ni is a characteristic of the Mg-Ni system, over a wide composition range, rather than of a particular composition. In relation to the thermal crystallization of the amorphous produced, the results of the differential thermal analysis applied to the amorphous samples showed that the formation enthalpy for both amorphous is the same, however, the amorphous produced in a planetary mill presented higher crystallization temperatures and apparent activation energies than the amorphous produced in a SPEX mill. The last behavior would be related with iron contamination coming from the erosion of the milling media. Finally, it is possible to conclude, that under the

  3. Amorphous phase formation in intermetallic Mg2Ni alloy synthesized by ethanol wet milling

    International Nuclear Information System (INIS)

    Wang, H.-W.; Chyou, S.-D.; Wang, S.-H.; Yang, M.-W.; Hsu, C.-Y.; Tien, H.-C.; Huang, N.-N.

    2009-01-01

    The hydriding/dehydriding properties of an intermetallic Mg 2 Ni alloy synthesized by wet ball milling in ethanol have been investigated. The appearance of the particle surface after different milling methods is one obvious difference. The alloyed powders prepared by either dry milling or wet milling under ethanol were characterized for phase content by X-ray diffractometer (XRD). The results show that two broad diffuse peaks, which are an ionic-organic-Mg amorphous material, appear in addition to the nickel element peaks. This unexpected amorphous phase has the special hydrogen absorbing/desorbing features.

  4. Hydrogen sorption properties of ball-milled Mg-C nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Spassov, Tony; Zlatanova, Zlatina; Spassova, Maya; Todorova, Stanislava [Faculty of Chemistry, University of Sofia ' ' St.Kl.Ohridski' ' , 1 James Bourchier str. 1164 Sofia (Bulgaria)

    2010-10-15

    MgH{sub 2} 75 at.%-C 25 at.% composites are synthesized by ball milling using different kinds of carbon additives: carbon black (CB), nanodiamonds (ND) and amorphous carbon soot (AC). X-ray diffraction analysis showed that the MgH{sub 2} phase in the as-obtained composite powders is nanocrystalline (80-100 nm). The SEM observations revealed that the samples consist of 5-15 {mu}m MgH{sub 2} particles, surrounded and in some cases coated by carbon flakes. The composite containing nanodiamonds revealed strong decrease of the MgH{sub 2} decomposition temperature with more than 100 C, compared to ball-milled pure MgH{sub 2}. Important issue of the present study is also the low temperature hydriding of the ball-milled Mg-C nanocomposites, investigated by high-pressure DSC. The process starts at about 200 C for all materials studied, but the hydriding mechanism looks different for the composites with different kinds of carbon additives. Whereas for Mg-carbon black it takes place in a relatively narrow temperature range, expressed by a single exothermic peak (200-300 C) for the other two composites the hydriding is a multi-step process, featured by two overlapped exothermic peaks for Mg-nanodiamonds and by two well separated exothermic effects (at about 300 C and 400 C) for Mg-amorphous carbon soot. The observed difference in the hydriding behavior of the Mg-C composites is attributed to the different kind of carbon component, which is supposed to play a catalytic role as well as protects magnesium from oxidation. The incorporation of carbon into the MgH{sub 2} particles results in the formation of high density of defects (dislocations and grain boundaries), which is supposed to be among the most possible reasons for the decreased hydride decomposition temperature. The Mg-C nanocomposites show reproducible hydriding/dehydriding behavior (thermodynamics and kinetics) during multiple cycling. Among the composites in the present study ''Mg-carbon black

  5. Improved hydrogen sorption kinetics in wet ball milled Mg hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Meng, Li

    2011-05-04

    In this work, wet ball milling method is used in order to improve hydrogen sorption behaviour due to its improved microstructure of solid hydrogen materials. Compared to traditional ball milling method, wet ball milling has benefits on improvement of MgH{sub 2} microstructure and further influences on its hydrogen sorption behavior. With the help of solvent tetrahydrofuran (THF), wet ball milled MgH{sub 2} powder has much smaller particle size and its specific surface area is 7 times as large as that of dry ball milled MgH{sub 2} powder. Although after ball milling the grain size is decreased a lot compared to as-received MgH{sub 2} powder, the grain size of wet ball milled MgH{sub 2} powder is larger than that of dry ball milled MgH{sub 2} powder due to the lubricant effect of solvent THF during wet ball milling. The improved particle size and specific surface area of wet ball milled MgH{sub 2} powder is found to be determining its hydrogen sorption kinetics especially at relatively low temperatures. And it also shows good cycling sorption behavior, which decides on its industrial applicability. With three different catalysts MgH{sub 2} powder shows improved hydrogen sorption behavior as well as the cyclic sorption behavior. Among them, the Nb{sub 2}O{sub 5} catalyst is found to be the most effective one in this work. Compared to the wet ball milled MgH{sub 2} powder, the particle size and specific surface area of the MgH{sub 2} powder with catalysts are similar to the previous ones, while the grain size of the MgH{sub 2} with catalysts is much finer. In this case, two reasons for hydrogen sorption improvement are suggested: one is the reduction of the grain size. The other may be as pointed out in some literatures that formation of new oxidation could enhance the hydrogen sorption kinetics, which is also the reason why its hydrogen capacity is decreased compared to without catalysts. After further ball milling, the specific surface area of wet ball milled Mg

  6. Effect of the milling conditions on the degree of amorphization of selenium by milling in a planetary ball mill

    International Nuclear Information System (INIS)

    Ksiazek, K; Wacke, S; Gorecki, T; Gorecki, Cz

    2007-01-01

    The effect of the milling parameters (rotation speed of the milling device and duration of milling) on the phase composition of the products of milling of fully crystalline selenium has been investigated. The milling was conducted using a planetary micromill and the phase composition of the milling products was determined by differential thermal analysis. It has been found that ball milling leads to the partial amorphization of the starting crystalline material. The content of amorphous phase in the milling products depends, in a rather complicated way, on the milling parameters. At the milling parameters adopted in the present study, the milling product was never fully amorphous. The complicated way the milling parameters affect the content of amorphous phase in the milling products is a result of competition of two processes: amorphization due to deformation and refinement of grains of milled material and crystallization of the already produced amorphous material at the cost of heat evolved in the milling vial during the milling process

  7. Partial amorphization of an α-FeCr alloy by ball-milling

    International Nuclear Information System (INIS)

    Loureiro, J. M.; Costa, B. F. O.; Caer, G. Le; Delcroix, P.

    2008-01-01

    The structural changes of near-equiatomic α-FeCr alloys, ground in a vibratory mill in vacuum and in argon, were followed as a function of milling time. An amorphous phase forms in both cases but at a much faster rate when milling in argon than when milling in vacuum. Amorphisation by ball-milling of α-FeCr alloys is deduced to be an intrinsic phenomenon which is however speeded-up by oxygen. The amorphous phase crystallizes into a bcc Cr-rich phase and a bcc Fe-rich phase when annealed for short times.

  8. Dehydriding and re-hydriding properties of high-energy ball milled LiBH{sub 4}+MgH{sub 2} mixtures

    Energy Technology Data Exchange (ETDEWEB)

    Crosby, Kyle; Shaw, Leon L. [Department of Chemical, Materials and Biomolecular Engineering, University of Connecticut, 97 North Eagleville Road, U-3136, Storrs, CT 06269 (United States)

    2010-07-15

    Here we report the first investigation of the dehydriding and re-hydriding properties of 2LiBH{sub 4} + MgH{sub 2} mixtures in the solid state. Such a study is made possible by high-energy ball milling of 2LiBH{sub 4}+MgH{sub 2} mixtures at liquid nitrogen temperature with the addition of graphite. The 2LiBH{sub 4}+MgH{sub 2} mixture ball milled under this condition exhibits a 5-fold increase in the released hydrogen at 265 C when compared with ineffectively ball milled counterparts. Furthermore, both LiBH{sub 4} and MgH{sub 2} contribute to hydrogen release in the solid state. The isothermal dehydriding/re-hydriding cycles at 265 C reveal that re-hydriding is dominated by re-hydriding of Mg. These unusual phenomena are explained based on the formation of nanocrystalline and amorphous phases, the increased defect concentration in crystalline compounds, and possible catalytic effects of Mg,MgH{sub 2} and LiBH{sub 4} on their dehydriding and re-hydriding properties. (author)

  9. Effect of ball mill treatment on kinetics of amorphous Ni78Si10B12 alloy crystallization

    International Nuclear Information System (INIS)

    Tomilin, I.A.; Mochalova, T.Yu.; Kaloshkin, S.D.; Kostyukovich, T.G.; Lopatina, E.A.

    1993-01-01

    The effect of the parameters of Ni 78 Si 10 B 12 alloy amorphous strip milling in a ball planetary mill on the stability of powder amorphous state, crytallization kinetics and dispersity is studied by the methods of differential scanning microcaloremetry and X-ray diffraction analysis. Energy intensity of milling conditions is assessed. An increase of input energy results in a decrease of activation energy of powder crystallization. Strip milling parameters which enable to avaintain the amorphous state of the material are determined

  10. Electrochemical properties of the ball-milled LaMg10NiMn alloy with Ni powders

    International Nuclear Information System (INIS)

    Wang Yi; Wang Xin; Gao Xueping; Shen Panwen

    2008-01-01

    The electrochemical characteristics of the ball-milled LaMg 10 NiMn alloys with Ni powders were investigated. It was found that the ball-milled LaMg 10 NiMn + 150 wt.% Ni composite exhibited higher first discharge capacity and better cycle performance. By means of the analysis of electrochemical impedance spectra (EIS), it was shown that the existence of manganese in LaMg 10 NiMn alloy increased the electrocatalytic activity due to its catalytic effect, and destabilized metal hydrides, and so reduced the hydrogen diffusion resistance. These contributed to the higher discharge capacity of the ball-milled LaMg 10 NiMn-Ni composite. According to the analytical results of X-ray diffraction (XRD), EIS and steady-state polarization (SSP) experiments, the inhibition of metal corrosion is not the main reason for the better cycle performance. The main reason is that the electrochemical reaction resistance of the ball-milled LaMg 10 NiMn-Ni composite is always lower than that of the ball-milled LaMg 10 Ni 2 -Ni composite because the former one contains manganese, which is a catalyst for the electrode reaction

  11. Refinement of Crystalline Boron and the Superconducting Properties of MgB2 by Attrition Ball Milling

    International Nuclear Information System (INIS)

    Lee, J. H.; Shin, S. Y.; Park, H. W.; Jun, B. H.; Kim, C. J.

    2008-01-01

    We report refinement of crystalline boron by an attrition ball milling system and the superconducting properties of the MgB 2 pellets prepared from the refined boron. In this work, we have conducted the ball milling with only crystalline boron powder, in order to improve homogeneity and control the grain size of the MgB 2 that is formed from it. We observed that the crystalline responses in the ball-milled boron became broader and weaker when the ball-milling time was further increased. On the other hand, the B 2 O 3 peak became stronger in the powders, resulting in an increase in the amount of MgO within the MgB 2 volume. The main reason for this is a greater oxygen uptake. From the perspective of the superconducting properties, however, the sample prepared from boron that was ball milled for 5 hours showed an improvement of critical current density (J c ), even with increased MgO phase, under an external magnetic field at 5 and 20 K.

  12. Hydrogen storage performances of LaMg{sub 11}Ni + x wt% Ni (x = 100, 200) alloys prepared by mechanical milling

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yanghuan, E-mail: zhangyh59@sina.com [Key Laboratory of Integrated Exploitation of Baiyun Obo Multi-Metal Resources, Inner Mongolia University of Science and Technology, Baotou 014010 (China); Department of Functional Material Research, Central Iron and Steel Research Institute, Beijing 100081 (China); Wang, Haitao [Key Laboratory of Integrated Exploitation of Baiyun Obo Multi-Metal Resources, Inner Mongolia University of Science and Technology, Baotou 014010 (China); Department of Functional Material Research, Central Iron and Steel Research Institute, Beijing 100081 (China); Zhai, Tingting; Yang, Tai; Yuan, Zeming; Zhao, Dongliang [Department of Functional Material Research, Central Iron and Steel Research Institute, Beijing 100081 (China)

    2015-10-05

    Highlights: • Amorphous and nanostructured alloys were prepared by mechanical milling. • The maximum discharge capacity of ball milled alloys reaches to 1053.5 mA h/g. • The addition of Ni significantly increases the discharge capacity. • Increasing milling time reduces the kinetic performances of ball milled alloys. - Abstract: In order to improve the hydrogen storage performances of Mg-based materials, LaMg{sub 11}Ni alloy was prepared by vacuum induction melting. Then the nanocrystalline/amorphous LaMg{sub 11}Ni + x wt% Ni (x = 100, 200) hydrogen storage alloys were synthesized by ball milling technology. The structure characterizations of the alloys were carried out by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The electrochemical hydrogen storage characteristics were tested by using programmed control battery testing system. The electrochemical impedance spectra (EIS), potentiodynamic polarization curves and potential-step curves were also plotted by an electrochemical workstation (PARSTAT 2273). The results indicate that the as-milled alloys exhibit a nanocrystalline and amorphous structure, and the amorphization degree of the alloys visibly increases with extending milling time. Prolonging the milling duration markedly enhances the electrochemical discharge capacity and cyclic stability of the alloys. The electrochemical kinetics, including high rate discharge ability (HRD), charge transfer rate, limiting current density (I{sub L}), hydrogen diffusion coefficient (D), monotonously decrease with milling time prolonging.

  13. The crystallization of amorphous Fe2MnGe powder prepared by ball milling

    International Nuclear Information System (INIS)

    Zhang, L.; Brueck, E.; Tegus, O.; Buschow, K.H.J.; Boer, F.R. de

    2003-01-01

    We synthesized for the first time the intermetallic compound Fe 2 MnGe. To avoid preferential evaporation of volatile components we exploited mechanical alloying. Amorphous Fe 2 MnGe alloy powder was prepared by planetary ball milling elemental starting materials. The amorphous-to-crystalline transition was studied by means of differential scanning calorimetry (DSC) and X-ray diffraction (XRD). A cubic D0 3 phase is formed at low temperature and transforms to a high-temperature hexagonal D0 19 phase. The apparent activation energy was determined by means of the Kissinger method

  14. Mechanically Induced Graphite-Nanodiamonds-Phase Transformations During High-Energy Ball Milling

    Science.gov (United States)

    El-Eskandarany, M. Sherif

    2017-05-01

    Due to their unusual mechanical, chemical, physical, optical, and biological properties, nearly spherical-like nanodiamonds have received much attention as desirable advanced nanomaterials for use in a wide spectrum of applications. Although, nanodiamonds can be successfully synthesized by several approaches, applications of high temperature and/or high pressure may restrict the real applications of such strategic nanomaterials. Distinct from the current preparation approaches used for nanodiamonds preparation, here we show a new process for preparing ultrafine nanodiamonds (3-5 nm) embedded in a homogeneous amorphous-carbon matrix. Our process started from high-energy ball milling of commercial graphite powders at ambient temperature under normal atmospheric helium gas pressure. The results have demonstrated graphite-single wall carbon nanotubes-amorphous-carbon-nanodiamonds phase transformations carried out through three subsequent stages of ball milling. Based on XRD and RAMAN analyses, the percentage of nanodiamond phase + C60 (crystalline phase) produced by ball milling was approximately 81%, while the amorphous phase amount was 19%. The pressure generated on the powder together the with temperature increase upon the ball-powder-ball collision is responsible for the phase transformations occurring in graphite powders.

  15. Hydrogen storage in Mg-Ni-Fe compounds prepared by melt spinning and ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Palade, P. [Settore Materiali, Dipartimento di Ingegneria Meccanica, Universita di Padova, via Marzolo 9, 35131 Padova (Italy); National Institute for Physics of Materials, Atomistilor 105 bis, P.O. Box MG-7, 077125 Bucharest-Magurele (Romania); Sartori, S. [Settore Materiali, Dipartimento di Ingegneria Meccanica, Universita di Padova, via Marzolo 9, 35131 Padova (Italy); Maddalena, A. [Settore Materiali, Dipartimento di Ingegneria Meccanica, Universita di Padova, via Marzolo 9, 35131 Padova (Italy); Principi, G. [Settore Materiali, Dipartimento di Ingegneria Meccanica, Universita di Padova, via Marzolo 9, 35131 Padova (Italy)]. E-mail: giovanni.principi@unipd.it; Lo Russo, S. [Dipartimento di Fisica, Universita di Padova, Via Marzolo 8, 35131 Padova (Italy); Lazarescu, M. [National Institute for Physics of Materials, Atomistilor 105 bis, P.O. Box MG-7, 077125 Bucharest-Magurele (Romania); Schinteie, G. [National Institute for Physics of Materials, Atomistilor 105 bis, P.O. Box MG-7, 077125 Bucharest-Magurele (Romania); Kuncser, V. [National Institute for Physics of Materials, Atomistilor 105 bis, P.O. Box MG-7, 077125 Bucharest-Magurele (Romania); Filoti, G. [National Institute for Physics of Materials, Atomistilor 105 bis, P.O. Box MG-7, 077125 Bucharest-Magurele (Romania)

    2006-05-18

    Magnesium-rich Mg-Ni-Fe intermetallic compounds have been prepared by two different routes: (a) short time ball milling of ribbons obtained by melt spinning; (b) long time ball milling of a mixture of MgH{sub 2}, Ni and Fe powders. The first type of samples displays an hydrogen desorption kinetics better than the second one. Pressure composition isotherm measurements exhibit for both type of samples two plateaux, the lower and wider corresponding to the MgH{sub 2} phase and the upper and shorter corresponding to the Mg{sub 2}NiH{sub 4} phase. The presence of the two types of hydrides is confirmed by X-ray diffraction analysis. Moessbauer spectroscopy shows that in melt spun and subsequently milled samples iron is mainly in a disordered structure and segregates after hydrogenation, while in directly milled powders remains mainly unalloyed. After multiple hydrogen absorption/desorption cycles the main part of iron is in metallic state in samples of both types, those of first type preserving better hydrogen desorption kinetics.

  16. Reduced graphene oxide synthesis by high energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Mondal, O. [Department of Physics, M.U.C Women' s College, Burdwan 713104 (India); Mitra, S. [MLS Prof' s Unit, Indian Association for the Cultivation of Science, Kolkata 700032 (India); Pal, M. [CSIR-Central Glass and Ceramic Research Institute, Kolkata 700032 (India); Datta, A. [University School of Basic and Applied Science (USBAS), Guru Gobind Singh Indraprastha University, New Delhi 110075 (India); Dhara, S. [Surface and Nanoscience Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India); Chakravorty, D., E-mail: mlsdc@iacs.res.in [MLS Prof' s Unit, Indian Association for the Cultivation of Science, Kolkata 700032 (India)

    2015-07-01

    Graphene oxide is transformed to reduced graphene oxide by high energy ball milling in inert atmosphere. The process of ball milling introduces defects and removes oxygen functional groups, thereby creating the possibility of fine tuning the band gap of all intermediate stages of the structural evolution. A limit of the backbone sp{sup 2} network structure has been found which should be able to accommodate defects, before amorphization sets in. The amorphization of graphene oxide is achieved rather quickly in comparison to that of graphite. From thermogravimetric and differential scanning calorimetric analysis along with Fourier transform infrared (FTIR) and Raman spectroscopic studies, it is found that the number of oxygen-containing groups decreases at a faster rate than that of aromatic double bonds with increasing ball milling time with a maximum limit of 3 h. Several characterization techniques (FTIR, Raman, UV–Visible and X-ray photoelectron spectroscopy) have confirmed that the material synthesized is, indeed, reduced graphene oxide. - Highlights: • Graphene oxide is transformed to reduced graphene oxide by high energy ball milling in inert atmosphere. • Fine tuning the band gap by introducing defects and removing oxygen functional groups. • Introduction of excess defects leads to amorphization. • Photoluminescence has been observed in the UV-blue region.

  17. Comprehensive characterization of ball-milled powders simulating a tribofilm system

    Energy Technology Data Exchange (ETDEWEB)

    Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de; Dietrich, P.M., E-mail: Paul.dietrich@yahoo.de; Unger, W.E.S., E-mail: Wolfgang.Unger@bam.de; Österle, W., E-mail: Werner.Oesterle@bam.de

    2016-01-15

    A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ball milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.

  18. Reduction of hydrogen desorption temperature of ball-milled MgH2 by NbF5 addition

    International Nuclear Information System (INIS)

    Recham, N.; Bhat, V.V.; Kandavel, M.; Aymard, L.; Tarascon, J.-M.; Rougier, A.

    2008-01-01

    Enhanced sorption properties of ball-milled MgH 2 are reported by adding NbF 5 . Among various catalyst amounts, 2 mol% of NbF 5 reveals to be the optimum concentration leading to significant reduction of the desorption temperature as well as faster kinetics of ball-milled MgH 2 . At 200 deg. C, temperature at which MgH 2 does not show any activity, MgH 2NbF 5 /2mol% composite desorbs 3.2 wt.% of H 2 in 50 mins. Interestingly, the addition of NbF 5 is also associated with an increase in the desorption pressure. At 300 deg. C, MgH 2NbF 5 /2mol% composite starts to desorb hydrogen at 600 mbar in comparison with 1 mbar for MgH 2 . Further improvements were successfully achieved by pre-grinding NbF 5 prior to ball-milling the catalyst with MgH 2 . Such pre-ground NbF 5 catalyzed MgH 2 composite desorbs 3 wt.% of H 2 at 150 deg. C. Improved properties are associated with smaller activation energies down to values close to the enthalpy of formation of MgH 2 . Finally, the mechanism at the origin of the enhancement is discussed in terms of catalyst stability, MgF 2 formation and electronic density localization

  19. Effect of process variables on synthesis of MgB2 by a high energy ball mill

    Directory of Open Access Journals (Sweden)

    Kurama Haldun

    2016-01-01

    Full Text Available The discovery of superconductivity of MgB2 in 2001, with a critical temperature of 39 K, offered the promise of important large-scale applications at around 20 K. Except than the other featured synthesis methods, mechanical activation performed by high energy ball mills, as bulk form synthesis or as a first step of wire and thin film productions, has considered as an effective alternative production route in recent years. The process of mechanical activation (MA starts with mixing the powders in the right proportion and loading the powder mixture into the mill with the grinding media. The milled powder is then consolidated into a bulk shape and heat-treated to obtain desired microstructure and properties. Thus, the important components of the MA process are the raw materials, mill type and process variables. During the MA process, heavy deformation of particles occure. This is manifested by the presence of a variety of crystal defects such as dislocations, vacancies, stacking faults and increased number of particle boundaries. The presence of this defect structure enhances the diffusivity of solute hence the critical currents and magnetic flux pinning ability of MgB2 are improved. The aim of the present study is to determine the effects of process variables such as ball-to-powder mass ratio, size of balls, milling time, annealing temperature and contribution of process control agent (toluene on the product size, morphology and conversion level of precursor powders to MgB2 after subsequent heat treatment. The morphological analyses of the samples were performed by a high vacuum electron microscope ZEISS SUPRA VP 50. The phase compositions of the samples were performed with an Rigaku-Rint 2200 diffractometer, with nickel filtered Cu Kα radiation and conversion level. The MgB2 phase wt % was calculated by the Rietveld refinement method. The obtained results were discussed according to the process variables to find out their affect on the structure

  20. Synthesis of the Mg2Ni alloy prepared by mechanical alloying using a high energy ball mill

    International Nuclear Information System (INIS)

    Iturbe G, J. L.; Lopez M, B. E.; Garcia N, M. R.

    2010-01-01

    Mg 2 Ni was synthesized by a solid state reaction from the constituent elemental powder mixtures via mechanical alloying. The mixture was ball milled for 10 h at room temperature in an argon atmosphere. The high energy ball mill used here was fabricated at ININ. A hardened steel vial and three steel balls of 12.7 mm in diameter were used for milling. The ball to powder weight ratio was 10:1. A small amount of powder was removed at regular intervals to monitor the structural changes. All the steps were performed in a little lucite glove box under argon gas, this glove box was also constructed in our Institute. The structural evolution during milling was characterized by X-ray diffraction and scanning electron microscopy techniques. The hydrogen reaction was carried out in a micro-reactor under controlled conditions of pressure and temperature. The hydrogen storage properties of mechanically milled powders were evaluated by using a thermogravimetric analysis system. Although homogeneous refining and alloying take place efficiently by repeated forging, the process time can be reduced to one fiftieth of the time necessary for conventional mechanical milling and attrition. (Author)

  1. Synthesis of the Mg{sub 2}Ni alloy prepared by mechanical alloying using a high energy ball mill

    Energy Technology Data Exchange (ETDEWEB)

    Iturbe G, J. L.; Lopez M, B. E. [ININ, Departamento de Quimica, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Garcia N, M. R., E-mail: joseluis.iturbe@inin.gob.m [UNAM, Facultad de Estudios Superiores Zaragoza, Batalla 5 de Mayo s/n, Esq. Fuerte de Loreto, Col. Ejercito de Oriente, 09230 Mexico D. F. (Mexico)

    2010-07-01

    Mg{sub 2}Ni was synthesized by a solid state reaction from the constituent elemental powder mixtures via mechanical alloying. The mixture was ball milled for 10 h at room temperature in an argon atmosphere. The high energy ball mill used here was fabricated at ININ. A hardened steel vial and three steel balls of 12.7 mm in diameter were used for milling. The ball to powder weight ratio was 10:1. A small amount of powder was removed at regular intervals to monitor the structural changes. All the steps were performed in a little lucite glove box under argon gas, this glove box was also constructed in our Institute. The structural evolution during milling was characterized by X-ray diffraction and scanning electron microscopy techniques. The hydrogen reaction was carried out in a micro-reactor under controlled conditions of pressure and temperature. The hydrogen storage properties of mechanically milled powders were evaluated by using a thermogravimetric analysis system. Although homogeneous refining and alloying take place efficiently by repeated forging, the process time can be reduced to one fiftieth of the time necessary for conventional mechanical milling and attrition. (Author)

  2. Iron-based amorphous alloys and methods of synthesizing iron-based amorphous alloys

    Science.gov (United States)

    Saw, Cheng Kiong; Bauer, William A.; Choi, Jor-Shan; Day, Dan; Farmer, Joseph C.

    2016-05-03

    A method according to one embodiment includes combining an amorphous iron-based alloy and at least one metal selected from a group consisting of molybdenum, chromium, tungsten, boron, gadolinium, nickel phosphorous, yttrium, and alloys thereof to form a mixture, wherein the at least one metal is present in the mixture from about 5 atomic percent (at %) to about 55 at %; and ball milling the mixture at least until an amorphous alloy of the iron-based alloy and the at least one metal is formed. Several amorphous iron-based metal alloys are also presented, including corrosion-resistant amorphous iron-based metal alloys and radiation-shielding amorphous iron-based metal alloys.

  3. Suppressing Heavy Metal Leaching through Ball Milling of Fly Ash

    Directory of Open Access Journals (Sweden)

    Zhiliang Chen

    2016-07-01

    Full Text Available Ball milling is investigated as a method of reducing the leaching concentration (often termed stablilization of heavy metals in municipal solid waste incineration (MSWI fly ash. Three heavy metals (Cu, Cr, Pb loose much of their solubility in leachate by treating fly ash in a planetary ball mill, in which collisions between balls and fly ash drive various physical processes, as well as chemical reactions. The efficiency of stabilization is evaluated by analysing heavy metals in the leachable fraction from treated fly ash. Ball milling reduces the leaching concentration of Cu, Cr, and Pb, and water washing effectively promotes stabilization efficiency by removing soluble salts. Size distribution and morphology of particles were analysed by laser particle diameter analysis and scanning electron microscopy. X-ray diffraction analysis reveals significant reduction of the crystallinity of fly ash by milling. Fly ash particles can be activated through this ball milling, leading to a significant decrease in particle size, a rise in its BET-surface, and turning basic crystals therein into amorphous structures. The dissolution rate of acid buffering materials present in activated particles is enhanced, resulting in a rising pH value of the leachate, reducing the leaching out of some heavy metals.

  4. Microstructural Evolution, Thermodynamics, and Kinetics of Mo-Tm2O3 Powder Mixtures during Ball Milling

    Directory of Open Access Journals (Sweden)

    Yong Luo

    2016-10-01

    Full Text Available The microstructural evolution, thermodynamics, and kinetics of Mo (21 wt % Tm2O3 powder mixtures during ball milling were investigated using X-ray diffraction and transmission electron microscopy. Ball milling induced Tm2O3 to be decomposed and then dissolved into Mo crystal. After 96 h of ball milling, Tm2O3 was dissolved completely and the supersaturated nanocrystalline solid solution of Mo (Tm, O was obtained. The Mo lattice parameter increased with increasing ball-milling time, opposite for the Mo grain size. The size and lattice parameter of Mo grains was about 8 nm and 0.31564 nm after 96 h of ball milling, respectively. Ball milling induced the elements of Mo, Tm, and O to be distributed uniformly in the ball-milled particles. Based on the semi-experimental theory of Miedema, a thermodynamic model was developed to calculate the driving force of phase evolution. There was no chemical driving force to form a crystal solid solution of Tm atoms in Mo crystal or an amorphous phase because the Gibbs free energy for both processes was higher than zero. For Mo (21 wt % Tm2O3, it was mechanical work, not the negative heat of mixing, which provided the driving force to form a supersaturated nanocrystalline Mo (Tm, O solid solution.

  5. Investigation of the milling-induced thermal behavior of crystalline and amorphous griseofulvin.

    Science.gov (United States)

    Trasi, Niraj S; Boerrigter, Stephan X M; Byrn, Stephen Robert

    2010-07-01

    To gain a better understanding of the physical state and the unusual thermal behavior of milled griseofulvin. Griseofulvin crystals and amorphous melt quench samples were milled in a vibrating ball mill for different times and then analyzed using differential scanning calorimetry (DSC) and powder X-ray diffraction (PXRD). Modulated DSC (mDSC) and annealing studies were done for the milled amorphous samples to further probe the effects of milling. Milling of griseofulvin crystals results in decrease in crystallinity and amorphization of the compound. A double peak is seen for crystallization in the DSC, which is also seen for the milled melt quench sample. Both enthalpy and temperature of crystallization decrease for the milled melt quenched sample. Tg is visible under the first peak with the mDSC, and annealing shows that increasing milling time results in faster crystallization upon storage. Milling of griseofulvin results in the formation of an amorphous form and not a mesophase. It increases the amount of surface created and the overall energy of the amorphous griseofulvin, which leads to a decreased temperature of crystallization. The two exotherms in the DSC are due to some particles having nuclei on the surface.

  6. Process intensification effect of ball milling on the hydrothermal pretreatment for corn straw enzymolysis

    International Nuclear Information System (INIS)

    Yuan, Zhengqiu; Long, Jinxing; Wang, Tiejun; Shu, Riyang; Zhang, Qi; Ma, Longlong

    2015-01-01

    Highlights: • Novel pretreatment of ball milling combined with hydrothermal method was presented. • Intensification effect of ball milling was significant for corn straw enzymolysis. • Ball milling destroyed the physical structure of corn straw. • Chemical (liquid mixture) method removed lignin and hemicellulose. • Glucose yield increased from 0.41 to 13.86 mg mL −1 under the optimized condition. - Abstract: Enhancement of the cellulose accessibility is significant for biomass enzymatic hydrolysis. Here, we reported an efficient combined pretreatment for corn straw enzymolysis using ball milling and dilute acid hydrothermal method (a mixture solvent of H 2 O/ethanol/sulfuric acid/hydrogen peroxide liquid). The process intensification effect of ball milling on the pretreatment of the corn straw was studied through the comparative characterization of the physical–chemical properties of the raw and pretreated corn straw using FT-IR, BET, XRD, SEM, and HPLC analysis. The effect of the pretreatment temperature was also investigated. Furthermore, various pretreatment methods were compared as well. Moreover, the pretreatment performance was measured by enzymolysis. The results showed that ball milling had a significant process intensification effect on the corn straw enzymolysis. The glucose concentration was dramatically increased from 0.41 to 13.86 mg mL −1 after the combined treatment of ball milling and hydrothermal. The efficient removal of lignin and hemicellulose and the enlargement of the surface area were considered to be responsible for this significant increase based on the intensive analysis on the main components and the physical–chemical properties of the raw and pretreated corn straw

  7. Effect of metal ion and ball milling on the electrochemical properties of M0.5TiOPO4 (M = Ni, Cu, Mg)

    International Nuclear Information System (INIS)

    Godbole, Vikram A.; Villevieille, Claire; Novák, Petr

    2013-01-01

    Various metal titanium oxyphosphates, M 0.5 TiOPO 4 (M = Ni, Cu, Mg) were synthesized via modified solution route synthesis. The as synthesized M 0.5 TiOPO 4 (M = Ni, Cu, Mg) were electrochemically tested using galvanostatic cycling, cyclic voltammetry, and rate performance measurements in order to investigate the effect of metal ion (M) on the electrochemical performance of this family of materials. All the studied materials reacted with 3 Li + during the 1st lithiation showing reaction plateaus at different potentials versus Lithium. Similar studies were performed on M 0.5 TiOPO 4 (M = Ni, Cu, Mg) samples with smaller particle size, obtained via ball milling, in order to understand the effect of particle size on the electrochemistry of the materials. The ball milled samples delivered higher specific charge during the 1st cycle showing reaction plateaus at different potentials, poorer capacity retention, and poorer rate capability as compared to the as synthesized ones. This was attributed to a change in morphology and particle size of the samples upon ball milling. Amongst all the tested materials, the as synthesized Cu 0.5 TiOPO 4 showed the best electrochemistry. The ball milled Mg 0.5 TiOPO 4 reacted with ∼5.5 Li + during 1st lithiation (as compared to 3 Li + expected from this family of compounds) and 3.3 Li + during the 1st delithiation (rather than the expected 2 Li + ). This suggests a reaction mechanism where Mg 0.5 TiOPO 4 undergoes a phase transformation forming Mg 0 , which reversibly alloys with 2.5 extra Li + . Thus the electrochemical cycling of Mg 0.5 TiOPO 4 gives insights into the reaction mechanism in this family of materials

  8. The influence of ball-milling time on the dehydrogenation properties of the NaAlH4-MgH2 composite

    NARCIS (Netherlands)

    Bendyna, J.K.; Dyjak, S.M.; Notten, P.H.L.

    2015-01-01

    The recently developed NaAlH4eMgH2 composite shows improved hydrogen-storage properties compared to MgH2 and NaAlH4. However, the dehydrogenation reaction rates are still too limited, hampering practical applications. Mechanical ball milling is broadly used to improve the dehydrogenation reaction

  9. Simulation of ball motion and energy transfer in a planetary ball mill

    International Nuclear Information System (INIS)

    Lu Sheng-Yong; Mao Qiong-Jing; Li Xiao-Dong; Yan Jian-Hua; Peng Zheng

    2012-01-01

    A kinetic model is proposed for simulating the trajectory of a single milling ball in a planetary ball mill, and a model is also proposed for simulating the local energy transfer during the ball milling process under no-slip conditions. Based on the kinematics of ball motion, the collision frequency and power are described, and the normal impact forces and effective power are derived from analyses of collision geometry. The Hertzian impact theory is applied to formulate these models after having established some relationships among the geometric, dynamic, and thermophysical parameters. Simulation is carried out based on two models, and the effects of the rotation velocity of the planetary disk Ω and the vial-to-disk speed ratio ω/Ω on other kinetic parameters is investigated. As a result, the optimal ratio ω/Ω to obtain high impact energy in the standard operating condition at Ω = 800 rpm is estimated, and is equal to 1.15. (interdisciplinary physics and related areas of science and technology)

  10. Microstructures and Dehydrogenation Properties of Ball-milled MgH2-K2Ti6O13-Ni Composite Systems

    Directory of Open Access Journals (Sweden)

    ZHANG Jian

    2016-11-01

    Full Text Available The K2Ti6O13 whisker separate-doped and K2Ti6O13 whisker and Ni powder multi-doped MgH2 hydrogen storage composite systems were prepared by mechanical milling method. The microstructures and dehydrogenation properties of the prepared samples were characterized by some testing methods such as X-ray diffraction (XRD, scanning electron microscope (SEM and differential scanning calorimeter (DSC. The results show that the K2Ti6O13 whisker not only plays the roles in refining the MgH2 crystalline grain, but also inhibit the agglomeration of MgH2 particles in K2Ti6O13 whisker separate-doped system, which results in the decreased dehydrogenation temperature of MgH2 matrix. When the mass ratio of K2Ti6O13 to MgH2 is 3:7, the improvement effect on dehydrogenation properties of MgH2 is the most remarkable. As compared with pure ball-milled MgH2, the dehydrogenation temperature of MgH2 in K2Ti6O13 whisker separate-doped system is decreased by nearly 75℃. For K2Ti6O13 whisker and Ni powder multi-dopedsystem, the dehydrogenation temperature of MgH2 matrix is further decreased compared to K2Ti6O13 whisker separate-doped one due to the dual effects of refined MgH2 crystalline grain by K2Ti6O13 whisker and destabilized MgH2 lattice by Ni solution. As compared with pure ball-milled MgH2, the dehydrogenation temperature of MgH2 in K2Ti6O13 whisker and Ni powder multi-doped system is decreased by nearly 87℃.

  11. Effect of the milling time on thermal stability of mechanically alloyed Mg{sub 5}0 Ni{sub 5}0 amorphous alloy; Efecto del tiempo de molienda sobre la estabilidad termica del amorfo Mg{sub 5}0 Ni:50 producido mediante aleado mecanico

    Energy Technology Data Exchange (ETDEWEB)

    Guzman, D.; Ordonez, S.; Serafini, D.; Rojas, P.; Aguilar, C.; Santander, M.; Navea, L.

    2009-07-01

    In order to study the relationship between the milling time used in the production of Mg{sub 5}0Ni{sub 5}0 amorphous alloy and its thermal stability, seven amorphous alloys were produced by milling for 20, 25, 30, 35, 40, 50 and 60 h each sample. The obtained powders were morphological and structurally characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. The thermal stability of amorphous alloys was study by differential scanning calorimetry (DSC). Based on the obtained results, it can be concluded that the increase in the added energy when milling for longer time causes the homogenization of the microstructure with an increase in amorphous phase, which dissolves a large amount of nickel in its structure. Therefore, the simultaneous crystallization of the Mg{sub 2}Ni and MgNi{sub 2} intermetallic compounds at 345 degree centigrade can be explained. (Author) 19 refs.

  12. Reactive-inspired ball-milling synthesis of an ODS steel: study of the influence of ball-milling and annealing

    International Nuclear Information System (INIS)

    Brocq, M.

    2010-10-01

    In the context of the development of new ODS (Oxide Dispersion Strengthened) steels as core materials in future nuclear reactors, we investigated a new process inspired by reactive ball-milling which consists in using YFe 3 andFe 2 O 3 as starting reactants instead of Y 2 O 3 to produce a dispersion of nano-oxides in a steel matrix and the influence of synthesis conditions on the nano-oxide characteristics were studied. For that aim, ODS steels were prepared by ball-milling and then annealed. Multi-scale characterizations were performed after each synthesis step, using notably atom probe tomography and small angle neutron scattering. The process inspired by reactive ball-milling was shown to be efficient for ODS steel synthesis, but it does not modify the nano-oxide characteristics as compared to those of oxides directly incorporated in the matrix by ball-milling. Broadly speaking, the nature of the starting oxygen bearing reactants has no influence on nano-oxide formation. Moreover, we showed that the nucleation of nano-oxides nucleation can start during milling and continues during annealing with a very fast kinetic. The final characteristics of nano-oxides formed in this way can be monitored through ball-milling parameters (intensity, temperature and atmosphere) and annealing parameters (duration and temperature). (author)

  13. A study on a new algorithm to optimize ball mill system based on modeling and GA

    International Nuclear Information System (INIS)

    Wang Heng; Jia Minping; Huang Peng; Chen Zuoliang

    2010-01-01

    Aiming at the disadvantage of conventional optimization method for ball mill pulverizing system, a novel approach based on RBF neural network and genetic algorithm was proposed in the present paper. Firstly, the experiments and measurement for fill level based on vibration signals of mill shell was introduced. Then, main factors which affected the power consumption of ball mill pulverizing system were analyzed, and the input variables of RBF neural network were determined. RBF neural network was used to map the complex non-linear relationship between the electric consumption and process parameters and the non-linear model of power consumption was built. Finally, the model was optimized by genetic algorithm and the optimal work conditions of ball mill pulverizing system were determined. The results demonstrate that the method is reliable and practical, and can reduce the electric consumption obviously and effectively.

  14. Structure and thermal stability of biodegradable Mg-Zn-Ca based amorphous alloys synthesized by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Datta, Moni Kanchan; Chou, Da-Tren; Hong, Daeho; Saha, Partha [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Chung, Sung Jae [Mechanical Engineering and Materials Science, Swanson School of Engineering, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Lee, Bouen [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Sirinterlikci, Arif [Department of Engineering, Robert Morris University, Moon Township, Pittsburgh, PA 15108 (United States); Ramanathan, Madhumati; Roy, Abhijit [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Kumta, Prashant N., E-mail: matscib@gmail.com [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Mechanical Engineering and Materials Science, Swanson School of Engineering, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Chemical and Petroleum Engineering, Swanson School of Engineering, University of Pittsburgh, Pittsburgh, PA 15261 (United States); School of Dental Medicine, University of Pittsburgh, Pittsburgh, PA 15261 (United States); Center for Complex Engineered Multifunctional Materials, University of Pittsburgh, Pittsburgh, PA 15261 (United States)

    2011-12-15

    Room temperature solid state diffusion reaction induced by mechanical alloying (MA) of elemental blends of Mg, Zn and Ca of nominal composition 60 at.% Mg-35 at.% Zn-5 at.% Ca has been studied. Formation of fully amorphous structure has been identified after 5 h of MA performed in a SPEX 8000M shaker mill, with milling continued up to 8 h to confirm the formation of homogeneous amorphous phase. Thermal stability of the amorphous phase has been studied using differential scanning calorimetry (DSC) and isothermal heat treatment at different temperatures. The amorphous powder consolidated using cold isostatic pressing (CIP) showed an envelope density {approx}80% of absolute density, which increased to an envelope density {approx}84% of absolute density after sintering at an optimized temperature of {approx}523 K for 9 h. Electrochemical bio-corrosion testing of the CIP compacted amorphous pellet as well as the sintered pellet performed in Dulbecco's Modified Eagle Medium, showed improved corrosion resistance in comparison to the as-cast pure Mg. Cytotoxicity testing of the CIP compacted amorphous pellet, performed using the MTT assay with MC3T3 osteoblastic cells, showed low cytotoxicity in comparison to the as-cast pure Mg.

  15. Kinetic parameters of grinding media in ball mills with various liner design and mill speed based on DEM modeling

    Science.gov (United States)

    Khakhalev, P. A.; Bogdanov, VS; Kovshechenko, V. M.

    2018-03-01

    The article presents analysis of the experiments in the ball mill of 0.5x0.3 m with four different liner types based on DEM modeling. The numerical experiment always complements laboratory research and allow obtaining high accuracy output data. An important property of the numerical experiment is the possibility of visualization of the results. The EDEM software allows calculating trajectory of the grinding bodies and kinetic parameters of each ball for the relative mill speed and the different types of mill’s liners.

  16. Synthesis of carbon nanotubes from acetylene on the FeCoMgO catalytic system obtained by ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Biris, A R; Simon, S; Lupu, D; Misan, I [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania); Biris, A S; Dervishi, E; Li, Z; Watanabe, F [UALR Nanotechnology Center, University of Arkansas, 2801 S University Ave, Little Rock, AR 72204 (United States); Lucaci, M, E-mail: alexandru.biris@itim-cj.r [National Institute for Research and Development in Electrical Engineering ICPE-CA 313 Splaiul Unirii, 030138 Bucharest (Romania)

    2009-08-01

    Highly crystalline multi wall carbon nanotubes have been synthesized by RF-CVD from acetylene at 850{sup 0}C over a Fe:Co:MgO catalyst. The catalytic system was obtained by mixing for 100 h Fe, Co and MgO powders in a ball milling device under petroleum ether environment, followed by oxidation in air at 500{sup 0}C for 24 h. Most of the nanotubes had external diameters in order of dozens of nm and lengths of microns, resulting in an aspect ration of over 1000. Their external to internal diameter ratio varied between 2.5 and 3.

  17. Effect of amorphous Mg50Ni50 on hydriding and dehydriding behavior of Mg2Ni alloy

    International Nuclear Information System (INIS)

    Guzman, D.; Ordonez, S.; Fernandez, J.F.; Sanchez, C.; Serafini, D.; Rojas, P.A.; Aguilar, C.; Tapia, P.

    2011-01-01

    Composite Mg 2 Ni (25 wt.%) amorphous Mg 50 Ni 50 was prepared by mechanical milling starting with nanocrystalline Mg 2 Ni and amorphous Mg 50 Ni 50 powders, by using a SPEX 8000 D mill. The morphological and microstructural characterization of the powders was performed via scanning electron microscopy and X-ray diffraction. The hydriding characterization of the composite was performed via a solid gas reaction method in a Sievert's-type apparatus at 363 K under an initial hydrogen pressure of 2 MPa. The dehydriding behavior was studied by differential thermogravimetry. On the basis of the results, it is possible to conclude that amorphous Mg 50 Ni 50 improved the hydriding and dehydriding kinetics of Mg 2 Ni alloy upon cycling. A tentative rationalization of experimental observations is proposed. - Research Highlights: → First study of the hydriding behavior of composite Mg 2 Ni (25 wt.%) amorphous Mg 50 Ni 50 . → Microstructural characterization of composite material using XRD and SEM was obtained. → An improved effect of Mg 50 Ni 50 on the Mg 2 Ni hydriding behavior was verified. → The apparent activation energy for the hydrogen desorption of composite was obtained.

  18. Preparation of 50Ni-45Ti-5Zr powders by high-energy ball milling and hot pressing

    Energy Technology Data Exchange (ETDEWEB)

    Marinzeck de Alcantara Abdala, Julia, E-mail: juabdala@yahoo.com.b [Instituto de Pesquisa e Desenvolvimento, Universidade do Vale do Paraiba, Av. Shishima Hifumi, 2911, 12244-000 Sao Jose dos Campos (Brazil); Bacci Fernandes, Bruno, E-mail: brunobacci@yahoo.com.b [Divisao de Engenharia Mecanica, Instituto Tecnologico de Aeronautica, Praca Marechal-do-Ar Eduardo Gomes, 50, 12228-904 Sao Jose dos Campos (Brazil); Santos, Dalcy Roberto dos, E-mail: dalcy@iae.cta.b [Instituto de Aeronautica e Espaco, Centro Tecnologico Aeroespacial, Praca Marechal-do-Ar Eduardo Gomes, 50, 12228-904 Sao Jose dos Campos (Brazil); Rodrigues Henriques, Vinicius Andre, E-mail: vinicius@iae.cta.b [Instituto de Aeronautica e Espaco, Centro Tecnologico Aeroespacial, Praca Marechal-do-Ar Eduardo Gomes, 50, 12228-904 Sao Jose dos Campos (Brazil); Moura Neto, Carlos de, E-mail: mneto@ita.b [Divisao de Engenharia Mecanica, Instituto Tecnologico de Aeronautica, Praca Marechal-do-Ar Eduardo Gomes, 50, 12228-904 Sao Jose dos Campos (Brazil); Saraiva Ramos, Alfeu, E-mail: alfeu@univap.b [Instituto de Pesquisa e Desenvolvimento, Universidade do Vale do Paraiba, Av. Shishima Hifumi, 2911, 12244-000 Sao Jose dos Campos (Brazil)

    2010-04-16

    This study reports on the preparation of the 50Ni-45Ti-5Zr (at.%) alloy by high-energy ball milling and hot pressing. The elemental powder mixture was processed in silicon nitride and hardened steel vials, and samples were collected after different milling times. To recover the previous powders in addition wet milling isopropyl alcohol (for 20 min) was adopted. The mechanically alloyed powders were hot-pressed under vacuum at 900 {sup o}C for 1 h using pressure levels close to 200 MPa. The milled powders were characterized by means of scanning electron microscopy, X-ray diffraction, and energy dispersive spectrometry techniques. It was noted that the ductile starting powders were continuously cold-welded during ball milling. This fact was more pronounced during the processing of 50Ni-45Ti-5Zr powders in hardened steel vial. After milling for 5 h, the results suggested that amorphous and nanocrystalline structures were achieved. The complete consolidation was found after hot pressing of mechanically alloyed 50Ni-45Ti-5Zr powders, and a large amount of the B2-NiTi phase was formed mainly after processing in stainless steel balls and vial.

  19. Ball Milling Treatment of Black Dross for Selective Dissolution of Alumina in Sodium Hydroxide Leaching

    OpenAIRE

    Thi Thuy Nhi Nguyen; Man Seung Lee; Thi Hong Nguyen

    2018-01-01

    A process consisting of ball milling followed by NaOH leaching was developed to selectively dissolve alumina from black dross. From the ball milling treatment, it was found that milling speed greatly affected the leaching behavior of silica and the oxides of Ca, Fe, Mg, and Ti present in dross. The leaching behavior of the mechanically activated dross was investigated by varying NaOH concentration, leaching temperature and time, and pulp density. In most of the leaching conditions, only alumi...

  20. Structure and magnetism of SmCo5 nanoflakes prepared by surfactant-assisted ball milling with different ball sizes

    International Nuclear Information System (INIS)

    Nie, Junwu; Han, Xianghua; Du, Juan; Xia, Weixing; Zhang, Jian; Guo, Zhaohui; Yan, Aru; Li, Wei; Ping Liu, J.

    2013-01-01

    Anisotropic magnetic SmCo 5 nanoflakes have been fabricated by surfactant-assisted ball milling (SABM) using hardened steel balls of one of the following sizes: 4, 6.5, 9.5 and 12.7 mm in diameters. The magnetic properties of SmCo 5 particles prepared by SABM with different milling ball sizes in diameters were investigated systematically. It was showed that the nanoflakes milled by amount of small size balls had a higher coercivity and lower anisotropy, i.e., worse grain orientation although in a short milling time while the nanoflakes prepared with same weight of big balls tend to have a lower coercivity, better grain orientation. The coercivity mechanism of the nanoflake was studied and it was mainly dominated with the domain-wall pinning. The SEM analysis shows that the morphology of nanoflakes prepared with different ball sizes are almost the same when the balls to powder weight ratio is fixed. The different magnetic properties caused by different ball sizes are mainly due to the different microstructure changes, i.e, grain refinement and c-axis orientation, which are demonstrated by X-ray diffraction (XRD) analysis and transmission electron microscope (TEM). Based on the experiments above, a combined milling process was suggested and done to improve magnetic properties as your need. - Highlights: • We fabricated anisotropic magnetic SmCo 5 nanoflakes by surfactant-assisted ball milling (SABM). • We investigated the magnetic properties of SmCo 5 particles systematically. It was showed that the coercivity, high or low, and grain orientation, good or bad, were influenced strongly by balls size. The different magnetisms caused by different ball sizes is mainly due to the different microstructure changes. • The coercivity mechanism of the nanoflake was studied and it was mainly dominated with the domain-wall pinning

  1. Composition dependency of the glass forming ability (GFA) in Mg-Ni-Si system by mechanical alloying

    International Nuclear Information System (INIS)

    Xie Haowen; Lin Jianguo; Li Yuncang; Hodgson, Peter D.; Wen Cuie

    2007-01-01

    The pure elemental powder mixtures with the compositions of Mg 65 Ni x Si 35-x (x = 10, 20, 25, 33 at.%) were subject to high-energy ball mill, and the structures of the mixtures at different intervals of milling were characterised by X-ray diffraction (XRD). The compositional dependency of the glass forming ability (GFA) in Mg-Ni-Si system was evaluated based on the experimental results and the theoretical calculation. The compositional dependency of GFA in Mg-Ni-Si system can be understood well by comparing the enthalpies of the crystalline and amorphous phases based on the Miedema's theory for the formation enthalpy of alloys. Increasing the Ni/Mg ratio and/or decreasing Si content can improve the amorphous formability. The calculation results might be of great help in optimising the composition with high GFA in Mg-Ni-Si system

  2. Ball milled bauxite residue as a reinforcing filler in phosphate-based intumescent system

    Directory of Open Access Journals (Sweden)

    Adiat Ibironke Arogundade

    2018-01-01

    Full Text Available Bauxite residue (BR is an alumina refinery waste with a global disposal problem. Of the 120 MT generated annually, only 3 MT is disposed via utilization. One of the significant challenges to sustainable utilization has been found to be the cost of processing. In this work, using ball milling, we achieved material modification of bauxite residue. Spectrometric imaging with FESEM showed the transformation from an aggregate structure to nano, platy particulates, leading to particle size homogeneity. BET analysis showed surface area was increased by 23%, while pH was reduced from 10.8 to 9.1 due to collapsing of the hydroxyl surface by the fracturing action of the ball mill. Incorporation of this into a phosphate-based fire retardant, intumescent formulation led to improved material dispersion and the formation of reinforcing heat shielding char nodules. XRD revealed the formation of ceramic metal phosphates which acted as an additional heat sink to the intumescent system, thereby reducing char oxidation and heat transfer to the substrate. Steel substrate temperature from a Bunsen burner test reduced by 33%. Therefore, ball milling can serve as a simple, low-cost processing route for the reuse of bauxite residue in intumescent composites.

  3. Determination of the boundary conditions of the grinding load in ball mills

    Science.gov (United States)

    Sharapov, Rashid R.

    2018-02-01

    The prospects of application in ball mills for grinding cement clinker with inclined partitions are shown. It is noted that ball mills with inclined partitions are more effective. An algorithm is proposed for calculating the power consumed by a ball mill with inclined inter-chamber partitions in which an axial movement of the ball load takes place. The boundary conditions in which the ball load is located are determined. The equations of bounding the grinding load are determined. The behavior of a grinding load is considered in view of the characteristic cross sections. The coordinates of the centers of gravity of the grinding load with a definite step and the shape of the cross sections are determined. It is theoretically shown that grinding load in some parts of the ball mill not only consumes, but also helps to rotate the ball mill. Methods for calculating complex analytical expressions for determining the coordinates of the centers of gravity of the grinding load under the conditions of its longitudinal motion have developed. The carried out researches allow to approach from the general positions to research of behavior of a grinding load in the ball mills equipped with various in-mill devices.

  4. Micro structrual characterization and analysis of ball milled silicon carbide

    Science.gov (United States)

    Madhusudan, B. M.; Raju, H. P.; Ghanaraja., S.

    2018-04-01

    Mechanical alloying has been one of the prominent methods of powder synthesis technique in solid state involving cyclic deformation, cold welding and fracturing of powder particles. Powder particles in this method are subjected to greater mechanical deformation due to the impact of ball-powder-ball and ball-powder-container collisions that occurs during mechanical alloying. Strain hardening and fracture of particles decreases the size of the particles and creates new surfaces. The objective of this Present work is to use ball milling of SiC powder for different duration of 5, 10, 15 and 20 hours by High energy planetary ball milling machine and to evaluate the effect of ball milling on SiC powder. Micro structural Studies using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and EDAX has been investigated.

  5. Effect of amorphous Mg{sub 50}Ni{sub 50} on hydriding and dehydriding behavior of Mg{sub 2}Ni alloy

    Energy Technology Data Exchange (ETDEWEB)

    Guzman, D., E-mail: danny.guzman@uda.cl [Departamento de Ingenieria en Metalurgia, Facultad de Ingenieria, Universidad de Atacama y Centro Regional de Investigacion y Desarrollo Sustentable de Atacama (CRIDESAT), Av. Copayapu 485, Copiapo (Chile); Ordonez, S. [Departamento de Ingenieria Metalurgica, Facultad de Ingenieria, Universidad de Santiago de Chile, Av. Lib. Bernardo O' Higgins 3363, Santiago (Chile); Fernandez, J.F.; Sanchez, C. [Departamento de Fisica de Materiales, Facultad de Ciencias, Universidad Autonoma de Madrid, Cantoblanco 28049, Madrid (Spain); Serafini, D. [Departamento de Fisica, Facultad de Ciencias, Universidad de Santiago de Chile and Center for Interdisciplinary Research in Materials, CIMAT, Av. Lib. Bernardo O' Higgins 3363, Santiago (Chile); Rojas, P.A. [Escuela de Ingenieria Mecanica, Facultad de Ingenieria, Av. Los Carrera 01567, Quilpue, Pontificia Universidad Catolica de Valparaiso, PUCV (Chile); Aguilar, C. [Departamento de Ingenieria Metalurgica y Materiales, Universidad Tecnica Federico Santa Maria, Av. Espana 1680, Valparaiso (Chile); Tapia, P. [Departamento de Ingenieria en Metalurgia, Facultad de Ingenieria, Universidad de Atacama, Av. Copayapu 485, Copiapo (Chile)

    2011-04-15

    Composite Mg{sub 2}Ni (25 wt.%) amorphous Mg{sub 50}Ni{sub 50} was prepared by mechanical milling starting with nanocrystalline Mg{sub 2}Ni and amorphous Mg{sub 50}Ni{sub 50} powders, by using a SPEX 8000 D mill. The morphological and microstructural characterization of the powders was performed via scanning electron microscopy and X-ray diffraction. The hydriding characterization of the composite was performed via a solid gas reaction method in a Sievert's-type apparatus at 363 K under an initial hydrogen pressure of 2 MPa. The dehydriding behavior was studied by differential thermogravimetry. On the basis of the results, it is possible to conclude that amorphous Mg{sub 50}Ni{sub 50} improved the hydriding and dehydriding kinetics of Mg{sub 2}Ni alloy upon cycling. A tentative rationalization of experimental observations is proposed. - Research Highlights: {yields} First study of the hydriding behavior of composite Mg{sub 2}Ni (25 wt.%) amorphous Mg{sub 50}Ni{sub 50}. {yields} Microstructural characterization of composite material using XRD and SEM was obtained. {yields} An improved effect of Mg{sub 50}Ni{sub 50} on the Mg{sub 2}Ni hydriding behavior was verified. {yields} The apparent activation energy for the hydrogen desorption of composite was obtained.

  6. High-energy ball milling of powder B-C mixtures

    International Nuclear Information System (INIS)

    Ramos, Alfeu S.; Taguchi, Simone P.; Ramos, Erika C.T.; Arantes, Vera L.; Ribeiro, Sebastiao

    2006-01-01

    The present work reports on the preparation of B-10 at.% C and B-18 at.% C powders by high-energy ball milling and further heat treatment. The milling process was carried out in a planetary ball mill. Following the milling process, powder samples were heat-treated at 1200 deg. C for 4 h using inert atmosphere. The milled and heat-treated B-10C and B-18C powders were characterized by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. A reduction on the intensity of B and C peaks was noticed after milling for 2 h, probably due the fine powder particle sizes because the pronounced fracture mechanism during ball milling of brittle starting components. The XRD patterns of B-10C and B-18C powders milled for 6 h indicated the presence of other peaks, suggesting that a metastable structure could have been formed. After milling for 90 h, these unknown peaks were still present. A large amount of B 4 C was formed after heat treatment at 1200 deg. C for 4 h beside these unknown peaks

  7. Response to Thermal Exposure of Ball-Milled Aluminum-Borax Powder Blends

    Science.gov (United States)

    Birol, Yucel

    2013-04-01

    Aluminum-borax powder mixtures were ball milled and heated above 873 K (600 °C) to produce Al-B master alloys. Ball-milled powder blends reveal interpenetrating layers of deformed aluminum and borax grains that are increasingly refined with increasing milling time. Thermal exposure of the ball-milled powder blends facilitates a series of thermite reactions between these layers. Borax, dehydrated during heating, is reduced by Al, and B thus generated reacts with excess Al to produce AlB2 particles dispersed across the aluminum grains starting at 873 K (600 °C). AlB2 particles start to form along the interface of the aluminum and borax layers. Once nucleated, these particles grow readily to become hexagonal-shaped crystals that traverse the aluminum grains with increasing temperatures as evidenced by the increase in the size as well as in the number of the AlB2 particles. Ball milling for 1 hour suffices to achieve a thermite reaction between borax and aluminum. Ball milling further does not impact the response of the powder blend to thermal exposure. The nucleation-reaction sites are multiplied, however, with increasing milling time and thus insure a higher number of smaller AlB2 particles. The size of the AlB2 platelets may be adjusted with the ball milling time.

  8. Hydrogen storage thermodynamics and kinetics of LaMg11Ni + x wt.% Ni (x = 100, 200) alloys synthesized by mechanical milling

    International Nuclear Information System (INIS)

    Zhang, Yanghuan; Jia, Zhichao; Central Iron and Steel Research Institute, Beijing; Yuan, Zeming; Qi, Yan; Zhao, Dongliang; Hou, Zhonghui

    2016-01-01

    LaMg 11 Ni + x wt.% Ni (x = 100, 200) composite hydrogen storage alloys with a nanocrystalline/amorphous structure were synthesized using ball milling technology. The effects of Ni content and milling time on hydrogen storage thermodynamics and dynamics of the alloys were investigated systematically. The hydrogen desorption properties were assessed using a Sieverts apparatus and differential scanning calorimetry. The thermodynamic parameters for the hydrogen absorption and desorption were calculated using the Van't Hoff equation. The hydrogen desorption activation energies of the hydrogenated alloys were also estimated by Arrhenius and Kissinger methods. Results indicate that the amount of Ni added has no effect on the thermodynamics of the alloys, but it significantly improves their absorption and desorption kinetics. Furthermore, the milling time has a great influence on the hydrogen storage properties. To be specific, the hydrogen absorption capacities reach the maximum values with the variation of milling time, and the hydrogen desorption activation energy obviously decreases with increasing milling time.

  9. Multifractal properties of ball milling dynamics

    Energy Technology Data Exchange (ETDEWEB)

    Budroni, M. A., E-mail: mabudroni@uniss.it; Pilosu, V.; Rustici, M. [Dipartimento di Chimica e Farmacia, Università degli Studi di Sassari, Via Vienna 2, Sassari 07100 (Italy); Delogu, F. [Dipartimento di Ingegneria Meccanica, Chimica, e dei Materiali, Università degli Studi di Cagliari, via Marengo 2, Cagliari 09123 (Italy)

    2014-06-15

    This work focuses on the dynamics of a ball inside the reactor of a ball mill. We show that the distribution of collisions at the reactor walls exhibits multifractal properties in a wide region of the parameter space defining the geometrical characteristics of the reactor and the collision elasticity. This feature points to the presence of restricted self-organized zones of the reactor walls where the ball preferentially collides and the mechanical energy is mainly dissipated.

  10. Residual stresses analysis in ball end milling of nickel-based superalloy Inconel 718

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Junteng; Zhang, Dinghua; Wu, Baohai; Luo, Ming [Key Laboratory of Contemporary Design and Integrated Manufacturing Technology, Northwestern Polytechnical University (China)

    2017-11-15

    Inconel 718 is widely used in the aviation, space, automotive and biomedical industries because of its outstanding properties. Near-surface residual stresses that are induced by ball end milling in Inconel 718 can be crucial for the performance and service time of the machined parts. In this paper, the influences of cutting conditions, including the use of cutting parameters, cutting fluid and spindle angles, on the residual stresses in the ball end milling process of Inconel 718 alloy were investigated experimentally. X-ray diffraction measurements reveal that residual stress distributions are highly influenced by cutting parameters, especially the depth of cut and cutting speed. The milling operation with cooling induces more compressive stresses trend and the magnitude of the residual stresses increases in the tensile direction with the increase of spindle angles. These cutting induced effects were further discussed with respect to thermal- mechanical coupling theory and some observations made by optical microscopy. From this investigation, it is suggested that the machining process parameters are not the smaller the better for the control of residual stresses in the ball end milling process of Inconel 718. (author)

  11. Nano-oxide nucleation in a 14Cr-ODS steel elaborated by reactive-inspired ball-milling: Multiscale characterizations

    International Nuclear Information System (INIS)

    Brocq, M.; Legendre, F.; Sakasegawa, H.; Radiguet, B.; Cuvilly, F.; Pareige, P.; Mathon, M.H.

    2009-01-01

    Oxide dispersion strengthened (ODS) steels are promising structural materials for both fusion and fission Generation IV reactors. Indeed, they exhibit excellent mechanical and creep properties and radiation resistance thanks to a fine and dense dispersion of complex nanometric oxides. ODS steels are usually elaborated by ball-milling iron based and yttrium oxide powders and then by thermomechanical treatments. It is expected that ball-milling dissolves yttrium oxides in the metallic matrix and that annealing induces nano-oxide precipitation. However the formation mechanism remains unclear and as a consequence the process is still uncontrolled. In this context, we proposed a new approach based on reactive ball milling of iron oxide (Fe 2 O 3 ), yttria (YFe 3 ) and iron based alloy in a dedicated instrumented ball-milling device. Also, a fine scale characterization, after each step of the process including ball-milling, is performed. A Fe-14Cr-2W-1Ti-0.8Y-0.2O (%wt) ODS steel was synthesized by reactive ball-milling and was characterized at very fine scale in both as-milled and as-annealed state. Atom Probe Tomography (APT) and Small Angle Neutron Scattering (SANS) were combined. After ballmilling, most of Y and O were, as expected, in solution in the ferritic matrix but some complex Y-Ti nano-oxides were also observed, indicating that oxide nucleation can start during ball-milling. With annealing the number of nano-oxides increases. In this presentation, experimental results of APT and SANS will be detailed and compared with what is usually observed in ODS steels elaborated by conventional ball milling. Finally, a formation mechanism of nano-oxides deduced from these results will be proposed. (author)

  12. Atomic disorder and amorphization of B2-structure CoZr by ball milling

    International Nuclear Information System (INIS)

    Zhou, G.F.; Bakker, H.

    1996-01-01

    For a considerable number of intermetallic compounds it has been found that ball milling introduces atomic (chemical) disorder. Disorder due to milling was demonstrated by x-ray diffraction in AlRu, crystallizing in the B2 structure (ordered b.c.c.) by a decrease of the intensity of superlattice reflections relative to fundamental reflections. The same technique was used to investigate disordering by milling in Ni 3 Al, crystallizing in the L1 2 structure (ordered f.c.c.). In both cases the disorder is anti-site disorder of both components, i.e. both atomic species substitute on the wrong sublattices. Besides x-ray diffraction measurements of magnetic properties turned out to be useful in monitoring structural changes due to milling. The change in the superconducting transition temperature, measured by magnetic a.c. susceptibility, was used to demonstrate atomic disordering by milling in Nb 3 Sn and Nb 3 Au. The type of disorder turned out to be anti-site disorder. Such a type of disorder occurs in the same materials also at high temperatures or after irradiation by neutrons. The disordering was accompanied by an increase of the lattice parameter. An increase in high-field magnetization accompanied by a decrease of the lattice parameter during milling was found in B2 CoGa and B2 CoAl. In principle in the completely ordered state both compounds are non-magnetic, because the CO atoms are shielded from one another by Ga and Al atoms, respectively. However, when a Co atom is transferred to the wrong sublattice, it is surrounded by Co atoms as nearest neighbors and bears a magnetic moment. This explains the strong increase of the magnetization due to milling

  13. Ferromagnetic behavior of nanocrystalline Cu–Mn alloy prepared by ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Mondal, B.N., E-mail: bholanath_mondal@yahoo.co.in [Department of Central Scientific Services, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032 (India); Sardar, G. [Department of Zoology, Baruipur College, South 24 parganas 743 610 (India); Nath, D.N. [Department of Physical Chemistry, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032 (India); Chattopadhyay, P.P. [Department of Metallurgy and Materials Engineering, Bengal Engineering and Science University, Shibpur, Howrah 711 103 (India)

    2014-12-15

    50Cu–50Mn (wt%) alloy was produced by ball milling. The milling was continued up to 30 h followed by isothermal annealing over a four interval of temperature from 350 to 650 °C held for 1 h. Crystallite size, lattice strain, lattice parameter were determined by Rietveld refinement structure analysis of X-ray diffraction data. The amount of dissolved/precipitated Mn (wt%) after ball milling/milling followed by annealing was calculated by quantative phase analysis (QPA). The increase of coercivity could be attributed to the introduction of lattice strain and reduction of crystallite size as a function of milling time. Electron paramagnetic resonance and superconducting quantum interface device analysis indicate that soft ferromagnetic behavior has been achieved by ball milled and annealed Cu–Mn alloy. The maximum coercivity value of Cu–Mn alloy obtained after annealing at 350 °C for 1 h is 277 Oe. - Highlights: • A small amount of Mn has dissolved in Cu after ball milling for 30 h. • Coercivity of the Cu–Mn alloy has increased with an increase in milling time. • Substantial MnO has formed after annealing at 650 °C for 1 h. • The ball milled and annealed alloy have revealed soft ferromagnetic behavior. • The alloy annealed at 350 °C shows the maximum value of coercivity.

  14. Preparation of tungsten-iron carbide by ball milling

    International Nuclear Information System (INIS)

    Wang, G.M.; Campbell, S.J.; Calka, A.; Kaczmarek, W.A.

    1996-01-01

    Several sets of elemental powder mixtures of Fe-W-C (W 46 Fe 46 C 8 , W 60 Fe 20 C 20 and W 34 Fe 33 C 33 ) were ball milled using Uni-Ball mill for periods of up to 550 h in vacuum with a ball - to - powder ratio of about 35:1. Depending on the milling time, the main component of the as-milled materials was found to be solid solutions of Fe-W-C or Fe-C. Ternary phase W 3 Fe 3 C was obtained on annealing the as-milled materials at about 700 deg C. This product was then found to transfer to (FeW) 6 C on heat treatment at about 800 deg C. The resultant products of the annealing processes were found to depend not only on the annealing temperature, but also the starting composition, especially the initial carbon concentration. Detailed information on the structural and phase evolution during thermal treatment as measured using x-ray diffraction, Moessbauer spectroscopy and thermal analysis is presented. Special interest is focused on the competition for formation in this system between the Fe-C, W-Fe and W-C phases

  15. CVD carbon powders modified by ball milling

    Directory of Open Access Journals (Sweden)

    Kazmierczak Tomasz

    2015-09-01

    Full Text Available Carbon powders produced using a plasma assisted chemical vapor deposition (CVD methods are an interesting subject of research. One of the most interesting methods of synthesizing these powders is using radio frequency plasma. This method, originally used in deposition of carbon films containing different sp2/sp3 ratios, also makes possible to produce carbon structures in the form of powder. Results of research related to the mechanical modification of these powders have been presented. The powders were modified using a planetary ball mill with varying parameters, such as milling speed, time, ball/powder mass ratio and additional liquids. Changes in morphology and particle sizes were measured using scanning electron microscopy and dynamic light scattering. Phase composition was analyzed using Raman spectroscopy. The influence of individual parameters on the modification outcome was estimated using statistical method. The research proved that the size of obtained powders is mostly influenced by the milling speed and the amount of balls. Powders tend to form conglomerates sized up to hundreds of micrometers. Additionally, it is possible to obtain nanopowders with the size around 100 nm. Furthermore, application of additional liquid, i.e. water in the process reduces the graphitization of the powder, which takes place during dry milling.

  16. Attempted - to -Phase Conversion of Croconic Acid via Ball Milling

    Science.gov (United States)

    2017-05-18

    ARL-TN-0824 MAY 2017 US Army Research Laboratory Attempted α- to β-Phase Conversion of Croconic Acid via Ball Milling by...Laboratory Attempted α- to β-Phase Conversion of Croconic Acid via Ball Milling by Steven W Dean, Rose A Pesce-Rodriguez, and Jennifer A Ciezak...

  17. Effect of milling time on microstructure and properties of Nano-titanium polymer by high-energy ball milling

    Science.gov (United States)

    Wang, Bo; Wei, Shicheng; Wang, Yujiang; Liang, Yi; Guo, Lei; Xue, Junfeng; Pan, Fusheng; Tang, Aitao; Chen, Xianhua; Xu, Binshi

    2018-03-01

    Nano-titanium (Nano-Ti) was prepared by high-energy ball milling from pure Ti power and grinding agents (Epoxy resin) at room temperature. The effect of milling time on structure and properties of Nano-Ti polymer were investigated systematically. The results show that high-energy ball milling is an effective way to produce Nano-Ti polymer. The dispersion stability and compatibility between Ti power and grinding agents are improved by prolonging the milling time at a certain degree, that is to say, the optimization milling time is 240 min. The particle size of Ti powder and the diffraction peaks intensity of Ti decrease obviously as the milling time increases due to the compression stress, shear friction and other mechanical forces are formed during ball milling. FT-IR result displays that the wavenumber of all the bands move to lower wavenumber after ball milling, and the epoxy ring is open. The system internal energy rises owing to the broken epoxy group and much more Nano-Ti is formed to promote the grafting reaction between Nano-Ti and epoxy resin. The results from TEM and XPS also prove that. And the grafting ration is maximum as the milling time is 240 min, the mass loss ratio is 17.53%.

  18. A study on thermal and mechanical properties of mechanically milled HDPE and PP

    International Nuclear Information System (INIS)

    Can, S.; Tan, S.

    2003-01-01

    In this study, mechanical mixing of HDPE and PP was performed via ball milling. Prepared compositions were 75/25 , 50/50 , 25/75 w/w HDPE/PP. Milling time and ball to powder ratio (B/P) were kept constant and system was cooled by adding solid CO 2 to improve the milling efficiency. To compare these systems with traditional methods, mixtures were also melt mixed by Brabender Plasti-Corder. Both milled and melt mixed systems were examined with DSC for thermal properties and tensile testing for mechanical properties Results are discussed by comparing milled , melt mixed and as-received polymers. It is observed that, unlike ball milled systems' in melt mixed systems mechanical properties are composition dependent. In addition , ball milling results in amorphization of both polymers and very high amounts of PP (75wt %) creates very amorphous HDPE structure. (Original)

  19. Surface modification of titanium hydride with epoxy resin via microwave-assisted ball milling

    International Nuclear Information System (INIS)

    Ning, Rong; Chen, Ding; Zhang, Qianxia; Bian, Zhibing; Dai, Haixiong; Zhang, Chi

    2014-01-01

    Highlights: • TiH 2 was modified with epoxy resin by microwave-assisted ball milling. • The epoxy ring was opened under the coupling effect of microwave and ball milling. • Microwave-assisted ball milling improved the compatibility of TiH 2 with epoxy. - Abstract: Surface modification of titanium hydride with epoxy resin was carried out via microwave-assisted ball milling and the products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermo-gravimetry (TG) and Fourier transform infrared spectroscopy (FT-IR). A sedimentation test was performed to investigate the compatibility of the modified nano titanium hydride with the epoxy resin. The results show that the epoxy resin molecules were grafted on the surface of nano titanium hydride particles during the microwave-assisted ball milling process, which led to the improvement of compatibility between the nanoparticles and epoxy resin. According to the FT-IR, the grafting site was likely to be located around the epoxy group due to the fact that the epoxy ring was opened. However, compared with microwave-assisted ball milling, the conventional ball milling could not realize the surface modification, indicating that the coupling effect of mechanical force and microwave played a key role during the process

  20. High-efficient production of boron nitride nanosheets via an optimized ball milling process for lubrication in oil.

    Science.gov (United States)

    Deepika; Li, Lu Hua; Glushenkov, Alexey M; Hait, Samik K; Hodgson, Peter; Chen, Ying

    2014-12-03

    Although tailored wet ball milling can be an efficient method to produce a large quantity of two-dimensional nanomaterials, such as boron nitride (BN) nanosheets, milling parameters including milling speed, ball-to-powder ratio, milling ball size and milling agent, are important for optimization of exfoliation efficiency and production yield. In this report, we systematically investigate the effects of different milling parameters on the production of BN nanosheets with benzyl benzoate being used as the milling agent. It is found that small balls of 0.1-0.2 mm in diameter are much more effective in exfoliating BN particles to BN nanosheets. Under the optimum condition, the production yield can be as high as 13.8% and the BN nanosheets are 0.5-1.5 μm in diameter and a few nanometers thick and of relative high crystallinity and chemical purity. The lubrication properties of the BN nanosheets in base oil have also been studied. The tribological tests show that the BN nanosheets can greatly reduce the friction coefficient and wear scar diameter of the base oil.

  1. Phase transition of Ni-Mn-Ga alloy powders prepared by vibration ball milling

    International Nuclear Information System (INIS)

    Tian, B.; Chen, F.; Tong, Y.X.; Li, L.; Zheng, Y.F.; Liu, Y.; Li, Q.Z.

    2011-01-01

    Research highlights: → The vibration ball milling with a high milling energy introduces the atomic disorder and large lattice distortion in the alloy during milling and makes the formation of disordered fcc structure phase in the alloy. → The transition temperature and activation energy for disordered fcc → disordered bcc are ∼320 o C and 209 ± 8 kJ/mol, respectively. → The alloy powders annealed at 800 o C for 1 h show a one-stage martensitic transformation with quite lower latent heat compared to the bulk alloy. - Abstract: This study investigated the phase transformation of the flaky shaped Ni-Mn-Ga powder particles with thickness around 1 μm prepared by vibration ball milling and post-annealing. The SEM, XRD, DSC and ac magnetic susceptibility measurement techniques were used to characterize the Ni-Mn-Ga powders. The structural transition of Heusler → disordered fcc occurred in the powders prepared by vibration ball milling (high milling energy) for 4 h, which was different from the structural transition of Heusler → disordered fct of the powders fabricated by planetary ball milling (low milling energy) for 4 h. The two different structures after ball milling should be due to the larger lattice distortion occurred in the vibration ball milling process than in the planetary ball milling process. The structural transition of disordered fcc → disordered bcc took place at ∼320 o C during heating the as-milled Ni-Mn-Ga powders, which was attributed to the elimination of lattice distortion caused by ball milling. The activation energy for this transition was 209 ± 8 kJ/mol. The Ni-Mn-Ga powder annealed at 800 o C mainly contained Heusler austenite phase at room temperature and showed a low volume of martensitic transformation upon cooling. The inhibition of martensitic transformation might be attributed to the reduction of grain size in the annealed Ni-Mn-Ga particles.

  2. Physicochemical properties of direct compression tablets with spray dried and ball milled solid dispersions of tadalafil in PVP-VA.

    Science.gov (United States)

    Wlodarski, K; Tajber, L; Sawicki, W

    2016-12-01

    The aim of this research was to develop immediate release tablets comprising solid dispersion (IRSDTs) of tadalafil (Td) in a vinylpyrrolidone and vinyl acetate block copolymer (PVP-VA), characterized by improved dissolution profiles. The solid dispersion of Td in PVP-VA (Td/PVP-VA) in a weight ratio of 1:1 (w/w) was prepared using two different processes i.e. spray drying and ball milling. While the former process has been well established in the formulation of IRSDTs the latter has not been exploited in these systems yet. Regardless of the preparation method, both Td/PVP-VA solid dispersions were amorphous as confirmed by PXRD, DSC and FTIR. However, different morphology of particles (SEM) resulted in differences in water apparent solubility and disk intrinsic dissolution rate (DIDR). Both solid dispersions and crystalline Td were successfully made into directly compressible tablets at three doses of Td, i.e. 2.5mg, 10mgand20mg, yielding nine different formulations (D 1 -D 9 ). Each of the lots met the requirements set by Ph.Eur. and was evaluated with respect to appearance, diameter, thickness, mass, hardness, friability, disintegration time and content of Td. IRSDTs performed as supersaturable formulations and had significantly improved water dissolution profiles in comparison with equivalent tablets containing crystalline Td and the marketed formulations. Tablets with both spray dried and ball milled Td/PVP-VA revealed the greatest improvement in dissolution depending on the investigated doses, i.e. 2.5mgand20mg, respectively. Also, dissolution of Td from Td/PVP-VA delivered in different forms occurred in the following order: powders>tablets>capsules. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Ball-milling and AlB2 addition effects on the hydrogen sorption properties of the CaH2 + MgB2 system

    International Nuclear Information System (INIS)

    Schiavo, B.; Girella, A.; Agresti, F.; Capurso, G.; Milanese, C.

    2011-01-01

    Research highlights: → Calcium hydride + magnesium-aluminum borides as candidates for hydrogen storage. → Long time ball milling improves hydrogen sorption kinetics of the CaH 2 +MgB 2 system. → Coexistence of MgB 2 and AlB 2 does not improve hydrogen sorption performances. → Total substitution of MgB 2 with AlB 2 improves the system kinetics and reversibility. → Below 400 deg. C almost the full hydrogen capacity of the CaH 2 + AlB 2 system is reached. - Abstract: Among the borohydrides proposed for solid state hydrogen storage, Ca(BH 4 ) 2 is particularly interesting because of its favourable thermodynamics and relatively cheap price. Composite systems, where other species are present in addition to the borohydride, show some advantages in hydrogen sorption properties with respect to the borohydrides alone, despite a reduction of the theoretical storage capacity. We have investigated the milling time influence on the sorption properties of the CaH 2 + MgB 2 system from which Ca(BH 4 ) 2 and MgH 2 can be synthesized by hydrogen absorption process. Manometric and calorimetric measurements showed better kinetics for long time milled samples. We found that the total substitution of MgB 2 with AlB 2 in the starting material can improve the sorption properties significantly, while the co-existence of both magnesium and aluminum borides in the starting mixture did not cause any improvement. Rietveld refinements of the X-ray powder diffraction spectra were used to confirm the hypothesized reactions.

  4. Processing of magnetically anisotropic MnBi particles by surfactant assisted ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Kanari, K. [Department of Physics, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece); Sarafidis, C., E-mail: hsara@physics.auth.gr [Department of Physics, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece); Gjoka, M.; Niarchos, D. [INN, NCSR Demokritos, Athens 15310 (Greece); Kalogirou, O. [Department of Physics, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece)

    2017-03-15

    MnBi particles are obtained from bulk MnBi using mechanochemical processing. The structure and magnetic properties of the MnBi particles are investigated by means of X-ray diffraction analysis, scanning electron microscopy and magnetometry. Surfactant assisted high energy ball milling results to the samples’ degradation even after one hour of milling. In the case of surfactant assisted low energy ball milling the increase of ball milling duration decreases the average particle size while the particles seem to be more separated. The saturation magnetization (M{sub s}) was found to decrease for large milling times beginning from 61 Am{sup 2}/kg, while the coercivity (μ{sub 0}H{sub c}) increases with the increase of ball milling duration up to 35 min where it reaches 1.62 T and thereafter it decreases. - Highlights: • Effect of surfactants in processing of MnBi. • Magnetization degradation due to air storage and due to processing. • Coercivity of 1.6 T in epoxy resin oriented material.

  5. Encaging palladium(0 in layered double hydroxide: A sustainable catalyst for solvent-free and ligand-free Heck reaction in a ball mill

    Directory of Open Access Journals (Sweden)

    Wei Shi

    2017-08-01

    Full Text Available In this paper, the synthesis of a cheap, reusable and ligand-free Pd catalyst supported on MgAl layered double hydroxides (Pd/MgAl-LDHs by co-precipitation and reduction methods is described. The catalyst was used in Heck reactions under high-speed ball milling (HSBM conditions at room temperature. The effects of milling-ball size, milling-ball filling degree, reaction time, rotation speed and grinding auxiliary category, which would influence the yields of mechanochemical Heck reactions, were investigated in detail. The characterization results of XRD, ICP–MS and XPS suggest that Pd/MgAl-LDHs have excellent textural properties with zero-valence Pd on its layers. The reaction results indicate that the catalyst could be utilized in HSBM systems to afford a wide range of Heck coupling products in satisfactory yields. Furthermore, this catalyst could be easily recovered and reused for at least five times without significant loss of catalytic activity.

  6. Structural study of ball-milled sodium alanate under high pressure

    International Nuclear Information System (INIS)

    Selva Vennila, R.; Drozd, Vadym; George, Lyci; Saxena, Surendra K.; Liermann, Hanns-Peter; Liu, H.Z.; Stowe, Ashley C.; Berseth, Polly; Anton, Donald; Zidan, Ragaiy

    2009-01-01

    Ball-milled NaAlH 4 was studied up to 15 GPa in a diamond anvil cell (DAC) by X-ray diffraction using a synchrotron radiation source. Lattice parameters were determined from the X-ray diffraction data at various pressures up to 6.5 GPa. Intensity of the powder diffraction patterns decreased with increasing pressure. Amorphisation started at a pressure of ∼6.5 GPa and completed at 13.5 GPa. Reversible phase transformation from amorphous phase to the tetragonal phase was observed. A fit to the pressure-volume data equation of state was obtained using the Birch-Murnaghan equation of state and the bulk modulus was found to be 52.16 ± 0.9 GPa which is twice higher than the unmilled NaAlH 4

  7. The effect of intermediate stop and ball size in fabrication of recycled steel powder using ball milling from machining steel chips

    International Nuclear Information System (INIS)

    Fitri, M.W.M.; Shun, C.H.; Rizam, S.S.; Shamsul, J.B.

    2007-01-01

    A feasibility study for producing recycled steel powder from steel scrap by ball milling was carried out. Steel scrap from machining was used as a raw material and was milled using planetary ball milling. Three samples were prepared in order to study the effect of intermediate stop and ball size. Sample with intermediate stop during milling process showed finer particle size compared to the sample with continuous milling. Decrease in the temperature of the vial during the intermediate stop milling gives less ductile behaviour to the steel powder, which is then easily work-hardened and fragmented to fine powder. Mixed small and big size ball give the best production of recycled steel powder where it gives higher impact force to the scrap and accelerate the fragmentation of the steel scrap into powder. (author)

  8. Ball Milling Assisted Solvent and Catalyst Free Synthesis of Benzimidazoles and Their Derivatives.

    Science.gov (United States)

    El-Sayed, Taghreed H; Aboelnaga, Asmaa; Hagar, Mohamed

    2016-08-24

    Benzoic acid and o-phenylenediamine efficiently reacted under the green solvent-free Ball Milling method. Several reaction parameters were investigated such as rotation frequency; milling balls weight and milling time. The optimum reaction condition was milling with 56.6 g weight of balls at 20 Hz frequency for one hour milling time. The study was extended for synthesis of a series of benzimidazol-2-one or benzimidazol-2-thione using different aldehydes; carboxylic acids; urea; thiourea or ammonium thiocyanate with o-phenylenediamine. Moreover; the alkylation of benzimidazolone or benzimidazolthione using ethyl chloroacetate was also studied.

  9. Influence of Solvent Composition on the Performance of Spray-Dried Co-Amorphous Formulations

    DEFF Research Database (Denmark)

    Mishra, Jaya; Rades, Thomas; Löbmann, Korbinian

    2018-01-01

    Ball-milling is usually used to prepare co-amorphous drug–amino acid (AA) mixtures. In this study, co-amorphous drug–AA mixtures were produced using spray-drying, a scalable industrially preferred preparation method. The influence of the solvent type and solvent composition was investigated....... Mixtures of indomethacin (IND) and each of the three AAs arginine, histidine, and lysine were ball-milled and spray-dried at a 1:1 molar ratio, respectively. Spray-drying was performed at different solvent ratios in (a) ethanol and water mixtures and (b) acetone and water mixtures. Different ratios...... that using spray-drying as a preparation method, all IND–AA mixtures could be successfully converted into the respective co-amorphous forms, irrespective of the type of solvent used, but depending on the solvent mixture ratios. Both ball-milled and spray-dried co-amorphous samples showed an enhanced...

  10. Ball milling of chalcopyrite: Moessbauer spectroscopy and XRD studies

    International Nuclear Information System (INIS)

    Pollak, H.; Fernandes, M.; Levendis, D.; Schonig, L.

    1999-01-01

    The aim of this project is to study the behavior of chalcopyrite under ball milling for extended periods in order to determine how it's decompose or transform. Tests were done with chalcopyrite mixed with iron and zinc with and without surfactant. The use of surfactants has various effects such as avoiding oxidation and clustering of the fine particles. In all case magnetic chalcopyrite is transformed into a paramagnetic component showing a disordered structure, thus revealing that Cu atoms have replaced Fe atoms. In the case of ball milling in air, chalcopyrite is decomposed with the lost of iron, while in milling under surfactants, iron enters into the chalcopyrite structure. (author)

  11. High-Energy Ball-Milling of Alloys and Compounds

    International Nuclear Information System (INIS)

    Le Caer, G.; Delcroix, P.; Begin-Colin, S.; Ziller, T.

    2002-01-01

    After outlining some characteristics of high-energy ball-milling, we discuss selected examples of phase transformation and of alloy synthesis which focus on deviations from archetypal behaviours and throw light on the milling mechanisms. Some contributions of Moessbauer spectrometry to the characterization of ground materials are described.

  12. Structural study of ball-milled sodium alanate under high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Selva Vennila, R. [Center for Study of Matter at Extreme Conditions, Florida International University, Miami, FL 33199 (United States)], E-mail: selva.raju@fiu.edu; Drozd, Vadym; George, Lyci; Saxena, Surendra K. [Center for Study of Matter at Extreme Conditions, Florida International University, Miami, FL 33199 (United States); Liermann, Hanns-Peter [High Pressure Collaboration Access Team (HPCAT) and Geophysical Laboratory, Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States); Liu, H.Z. [HPCAT, Geophysical Laboratory, Carnegie Institution of Washington, Building 434E, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Stowe, Ashley C.; Berseth, Polly; Anton, Donald; Zidan, Ragaiy [Savannah River National Laboratory, Energy Security Department, Aiken, SC 29808 (United States)

    2009-04-03

    Ball-milled NaAlH{sub 4} was studied up to 15 GPa in a diamond anvil cell (DAC) by X-ray diffraction using a synchrotron radiation source. Lattice parameters were determined from the X-ray diffraction data at various pressures up to 6.5 GPa. Intensity of the powder diffraction patterns decreased with increasing pressure. Amorphisation started at a pressure of {approx}6.5 GPa and completed at 13.5 GPa. Reversible phase transformation from amorphous phase to the tetragonal phase was observed. A fit to the pressure-volume data equation of state was obtained using the Birch-Murnaghan equation of state and the bulk modulus was found to be 52.16 {+-} 0.9 GPa which is twice higher than the unmilled NaAlH{sub 4}.

  13. FePt magnetic particles prepared by surfactant-assisted ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Velasco, V., E-mail: vvjimeno@fis.ucm.es [Instituto de Magnetismo Aplicado, UCM-ADIF-CSIC, P.O. Box 155, Las Rozas 28230 (Spain); Departamento de Física de Materiales, Universidad Complutense de Madrid, Madrid 28040 (Spain); Hernando, A.; Crespo, P. [Instituto de Magnetismo Aplicado, UCM-ADIF-CSIC, P.O. Box 155, Las Rozas 28230 (Spain); Departamento de Física de Materiales, Universidad Complutense de Madrid, Madrid 28040 (Spain)

    2013-10-15

    High-energy ball milling of Fe and Pt elemental powders has been carried out under dry and wet (in presence of solvent and surfactants) conditions. Dry milling leads to the formation of the disordered FCC-FePt alloy whereas by the wet milling procedure the main process is the decrease of Fe and Pt particle size, although some dissolution of Pt into Fe grains cannot be ruled out, and no hint of the formation of the FCC-FePt phase is observed even to milling times up to 20 h, as X-ray diffraction, electron microscopy and Mössbauer spectroscopy indicates. The as-milled particles were annealed at 600 °C for 2 h under Ar atmosphere. It is noticed that the disordered fcc-FePt phase observed in particles milled under dry conditions transform to ordered fct phase characterized by a hard magnetic behavior with a coercive field up to 10,000 Oe. However, those particles milled in the surfactant/solvent medium exhibit a soft magnetic behavior with a coercive field of 600 Oe. These results indicate that wet high-energy ball milling is not an adequate technique for obtaining single-phase FePt particles. - Highlights: • FePt particles have been obtained by high-energy ball milling. • In the presence of surfactants and solvents, almost no alloying process takes place. • After annealing, the coercive field of the FePt alloy particles increases from 150 Oe to 10,000 Oe.

  14. Reverse martensitic transformation in alumina-15 vol% zirconia nanostructured powder synthesized by high energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Maneshian, M.H. [Department of Materials Science and Engineering, Sharif University of Technology, Azadi Avenue, P.O. Box 11365-9466, Tehran (Iran, Islamic Republic of)], E-mail: mh_maneshian@yahoo.com; Banerjee, M.K. [National Institute of Foundry and Forge Technology, Hatia, Ranchi 834003 (India)

    2008-07-14

    In the present work, three alumina-15 vol% zirconia composites with Y{sub 2}O{sub 3}, MgO as dopants and without oxide as dopant have been investigated. High energy ball milling (HEBM) provides the positive thermodynamic driving force for monoclinic to tetragonal transformation and it reduces starting temperature for the reverse martensitic transformation, meanwhile mobility of zirconium cations and oxygen anions are enhanced in zirconia by HEBM. The general, albeit heuristic, reasoning is corroborated by nanocrystallity, particle size and also the retained monoclinic seem to play an important role. After 10 h HEBM, approximately 28% zirconia tetragonal phase is achieved. Non-stoichiometric tetragonal zirconia phase; Zr{sub 0.95}O{sub 2} is seen to have been achieved by high energy ball milling (HEBM). The structural and compositional evolutions during HEBM have been investigated using X-ray diffraction method (XRD) and scanning electron microscopy (SEM). High resolution transmission electron microscope (TEM) is also used for further understanding about the phenomenological changes taking place during high energy ball milling.

  15. Structural and magnetic properties of ball milled copper ferrite

    DEFF Research Database (Denmark)

    Goya, G.F.; Rechenberg, H.R.; Jiang, Jianzhong

    1998-01-01

    The structural and magnetic evolution in copper ferrite (CuFe2O4) caused by high-energy ball milling are investigated by x-ray diffraction, Mössbauer spectroscopy, and magnetization measurements. Initially, the milling process reduces the average grain size of CuFe2O4 to about 6 nm and induces....... The canted spin configuration is also suggested by the observed reduction in magnetization of particles in the blocked state. Upon increasing the milling time, nanometer-sized CuFe2O4 particles decompose, forming alpha-Fe2O3 and other phases, causing a further decrease of magnetization. After a milling time...... of 98 h, alpha-Fe2O3 is reduced to Fe3O4, and magnetization increases accordingly to the higher saturation magnetization value of magnetite. Three sequential processes during high-energy ball milling are established: (a) the synthesis of partially inverted CuFe2O4 particles with a noncollinear spin...

  16. High surface area niobium oxides as catalysts for improved hydrogen sorption properties of ball milled MgH2

    International Nuclear Information System (INIS)

    Bhat, V.V.; Rougier, A.; Aymard, L.; Nazri, G.A.; Tarascon, J.-M.

    2008-01-01

    We report, high surface area (up to 200 m 2 /g) nanocrystalline niobium oxide (so called p-Nb 2 O 5 ) synthesized by 'chimie douce' route and its importance in enhancing the hydrogen sorption properties of MgH 2 . p-Nb 2 O 5 induces faster kinetics than commonly used commercial Nb 2 O 5 (c-Nb 2 O 5 ) when ball milled with MgH 2 (named (MgH 2 ) catalyst ) by reducing the time of desorption from 35 min in (MgH 2 ) c-Nb 2 O 5 to 12 min in (MgH 2 ) p-Nb 2 O 5 at 300 deg. C. The BET surface area of as-prepared Nb 2 O 5 was tuned by heat treatment and its effect on sorption properties was studied. Among them, both p-Nb 2 O 5 and Nb 2 O 5 :350 (p-Nb 2 O 5 heated to 350 deg. C with a BET specific surface area of 46 m 2 /g) desorb 5 wt.% within 12 min, exhibiting the best catalytic activity. Furthermore, thanks to the addition of high surface area Nb 2 O 5 , the desorption temperature was successfully lowered down to 200 deg. C, with a significant amount of desorbed hydrogen (4.5 wt.%). In contrast, the composite (MgH 2 ) c-Nb 2 O 5 shows no desorption at this 'low' temperature

  17. Raman spectroscopy fingerprint of stainless steel-MWCNTs nanocomposite processed by ball-milling

    Directory of Open Access Journals (Sweden)

    Marcos Allan Leite dos Reis

    2018-01-01

    Full Text Available Stainless steel 304L alloy powder and multiwalled carbon nanotubes were mixed by ball-milling under ambient atmosphere and in a broad range of milling times, which spans from 0 to 120 min. Here, we provided spectroscopic signatures for several distinct composites produced, to show that the Raman spectra present interesting splittings of the D-band feature into two main sub-bands, D-left and D-right, together with several other secondary features. The G-band feature also presents multiple splittings that are related to the outer and inner diameter distributions intrinsic to the multiwalled carbon nanotube samples. A discussion about the second order 2D-band (also known as G′-band is also provided. The results reveal that the multiple spectral features observed in the D-band are related to an increased chemical functionalization. A lower content of amorphous carbon at 60 and 90 min of milling time is verified and the G-band frequencies associated to the tubes in the outer diameters distribution is upshifted, which suggests that doping induced by strain is taking place in the milled samples. The results indicate that Raman spectroscopy can be a powerful tool for a fast and non-destructive characterization of carbon nanocomposites used in powder metallurgy manufacturing processes.

  18. Raman spectroscopy fingerprint of stainless steel-MWCNTs nanocomposite processed by ball-milling

    Science.gov (United States)

    dos Reis, Marcos Allan Leite; Barbosa Neto, Newton Martins; de Sousa, Mário Edson Santos; Araujo, Paulo T.; Simões, Sónia; Vieira, Manuel F.; Viana, Filomena; Loayza, Cristhian R. L.; Borges, Diego J. A.; Cardoso, Danyella C. S.; Assunção, Paulo D. C.; Braga, Eduardo M.

    2018-01-01

    Stainless steel 304L alloy powder and multiwalled carbon nanotubes were mixed by ball-milling under ambient atmosphere and in a broad range of milling times, which spans from 0 to 120 min. Here, we provided spectroscopic signatures for several distinct composites produced, to show that the Raman spectra present interesting splittings of the D-band feature into two main sub-bands, D-left and D-right, together with several other secondary features. The G-band feature also presents multiple splittings that are related to the outer and inner diameter distributions intrinsic to the multiwalled carbon nanotube samples. A discussion about the second order 2D-band (also known as G'-band) is also provided. The results reveal that the multiple spectral features observed in the D-band are related to an increased chemical functionalization. A lower content of amorphous carbon at 60 and 90 min of milling time is verified and the G-band frequencies associated to the tubes in the outer diameters distribution is upshifted, which suggests that doping induced by strain is taking place in the milled samples. The results indicate that Raman spectroscopy can be a powerful tool for a fast and non-destructive characterization of carbon nanocomposites used in powder metallurgy manufacturing processes.

  19. Mechanochemical synthesis of nanostructured chemical hydrides in hydrogen alloying mills

    International Nuclear Information System (INIS)

    Wronski, Z.; Varin, R.A.; Chiu, C.; Czujko, T.; Calka, A.

    2007-01-01

    Mechanical alloying of magnesium metal powders with hydrogen in specialized hydrogen ball mills can be used as a direct route for mechanochemical synthesis of emerging chemical hydrides and hydride mixtures for advanced solid-state hydrogen storage. In the 2Mg-Fe system, we have successfully synthesized the ternary complex hydride Mg 2 FeH 6 in a mixture with nanometric Fe particles. The mixture of complex magnesium-iron hydride and nano-iron released 3-4 wt.%H 2 in a thermally programmed desorption experiment at the range 285-295 o C. Milling of the Mg-2Al powder mixture revealed a strong competition between formation of the Al(Mg) solid solution and the β-MgH 2 hydride. The former decomposes upon longer milling as the Mg atoms react with hydrogen to form the hydride phase, and drive the Al out of the solid solution. The mixture of magnesium dihydride and nano-aluminum released 2.1 wt.%H 2 in the temperature range 329-340 o C in the differential scanning calorimetry experiment. The formation of MgH 2 was suppressed in the Mg-B system; instead, a hydrogenated amorphous phase (Mg,B)H x , was formed in a mixture with nanometric MgB 2 . Annealing of the hydrogen-stabilized amorphous mixture produced crystalline MgB 2

  20. MgO-based adsorbents for CO2 adsorption: Influence of structural and textural properties on the CO2 adsorption performance.

    Science.gov (United States)

    Elvira, Gutiérrez-Bonilla; Francisco, Granados-Correa; Víctor, Sánchez-Mendieta; Alberto, Morales-Luckie Raúl

    2017-07-01

    A series of MgO-based adsorbents were prepared through solution-combustion synthesis and ball-milling process. The prepared MgO-based powders were characterized using X-ray diffraction, scanning electron microscopy, N 2 physisorption measurements, and employed as potential adsorbents for CO 2 adsorption. The influence of structural and textural properties of these adsorbents over the CO 2 adsorption behaviour was also investigated. The results showed that MgO-based products prepared by solution-combustion and ball-milling processes, were highly porous, fluffy, nanocrystalline structures in nature, which are unique physico-chemical properties that significantly contribute to enhance their CO 2 adsorption. It was found that the MgO synthesized by solution combustion process, using a molar ratio of urea to magnesium nitrate (2:1), and treated by ball-milling during 2.5hr (MgO-BM2.5h), exhibited the maximum CO 2 adsorption capacity of 1.611mmol/g at 25°C and 1atm, mainly via chemisorption. The CO 2 adsorption behaviour on the MgO-based adsorbents was correlated to their improved specific surface area, total pore volume, pore size distribution and crystallinity. The reusability of synthesized MgO-BM2.5h was confirmed by five consecutive CO 2 adsorption-desorption times, without any significant loss of performance, that supports the potential of MgO-based adsorbent. The results confirmed that the special features of MgO prepared by solution-combustion and treated by ball-milling during 2.5hr are favorable to be used as effective MgO-based adsorbent in post-combustion CO 2 capture technologies. Copyright © 2016. Published by Elsevier B.V.

  1. Nanocrystalline TiAl powders synthesized by high-energy ball milling: effects of milling parameters on yield and contamination

    International Nuclear Information System (INIS)

    Bhattacharya, Prajina; Bellon, Pascal; Averback, Robert S.; Hales, Stephen J.

    2004-01-01

    High-energy ball milling was employed to produce nanocrystalline Ti-Al powders. As sticking of the powders can be sufficiently severe to result in a near zero yield, emphasis was placed on varying milling conditions so as to increase the yield, while avoiding contamination of the powders. The effects of milling parameters such as milling tools, initial state of the powders and addition of process control agents (PCA's) were investigated. Cyclohexane, stearic acid and titanium hydride were used as PCA's. Milling was conducted either in a Cr-steel vial with C-steel balls, or in a tungsten carbide (WC) vial with WC balls, using either elemental or pre-alloyed powders. Powder samples were characterized using X-ray diffraction, scanning and transmission electron microscopy. In the absence of PCA's mechanical alloying in a WC vial and attrition milling in a Cr-steel vial were shown to lead to satisfactory yields, about 65-80%, without inducing any significant contamination of the powders. The results suggest that sticking of the powders on to the milling tools is correlated with the phase evolution occurring in these powders during milling

  2. Soft magnetic properties of bulk amorphous Co-based samples

    International Nuclear Information System (INIS)

    Fuezer, J.; Bednarcik, J.; Kollar, P.

    2006-01-01

    Ball milling of melt-spun ribbons and subsequent compaction of the resulting powders in the supercooled liquid region were used to prepare disc shaped bulk amorphous Co-based samples. The several bulk samples have been prepared by hot compaction with subsequent heat treatment (500 deg C - 575 deg C). The influence of the consolidation temperature and follow-up heat treatment on the magnetic properties of bulk samples was investigated. The final heat treatment leads to decrease of the coercivity to the value between the 7.5 to 9 A/m (Authors)

  3. Low-temperature synthesis of MgB{sub 2} via powder metallurgy processing

    Energy Technology Data Exchange (ETDEWEB)

    Birol, Yucel [Dokuz Eylul University, Department of Metallurgical and Materials Engineering, Faculty of Engineering, Buca, Izmir (Turkey)

    2016-12-15

    Ball-milled Mg/B{sub 2}O{sub 3} powder blends reveal interpenetrating layers of deformed magnesium and boron oxide grains that are increasingly refined with increasing milling time. Boron oxide is reduced by Mg and MgO thus formed reacts with the remaining B{sub 2}O{sub 3} to produce Mg{sub 3}(BO{sub 3}){sub 2} during ball milling for 30 min. Both B{sub 2}O{sub 3} and Mg{sub 3}(BO{sub 3}){sub 2} react with Mg to produce MgB{sub 2} upon further ball milling. An annealing treatment can be employed when ball milling is performed for less than 1 h as thermal exposure of the ball-milled Mg/B{sub 2}O{sub 3} powder blends also leads to the formation of MgB{sub 2}. The above reactions take place between 500 and 700 C when the Mg/B{sub 2}O{sub 3} powder blend is ball milled for 30 min, and between 450 and 550 C, after ball milling for 1 h. This is a very attractive route owing to processing temperatures where the volatility of Mg is no longer a problem. (orig.)

  4. Non-isothermal synergetic catalytic effect of TiF{sub 3} and Nb{sub 2}O{sub 5} on dehydrogenation high-energy ball milled MgH{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Tiebang, E-mail: tiebangzhang@nwpu.edu.cn; Hou, Xiaojiang; Hu, Rui; Kou, Hongchao; Li, Jinshan

    2016-11-01

    MgH{sub 2}-M (M = TiF{sub 3} or Nb{sub 2}O{sub 5} or both of them) composites prepared by high-energy ball milling are used in this work to illustrate the dehydrogenation behavior of MgH{sub 2} with the addition of catalysts. The phase compositions, microstructures, particle morphologies and distributions of MgH{sub 2} with catalysts have been evaluated. The non-isothermal synergetic catalytic-dehydrogenation effect of TiF{sub 3} and Nb{sub 2}O{sub 5} evaluated by differential scanning calorimetry gives the evidences that the addition of catalysts is an effective strategy to destabilize MgH{sub 2} and reduce hydrogen desorption temperatures and activation energies. Depending on additives, the desorption peak temperatures of catalyzed MgH{sub 2} reduce from 417 °C to 341 °C for TiF{sub 3} and from 417 °C to 336 °C for Nb{sub 2}O{sub 5}, respectively. The desorption peak temperature reaches as low as 310 °C for MgH{sub 2} catalyzed by TiF{sub 3} coupling with Nb{sub 2}O{sub 5}. The non-isothermal synergetic catalytic effect of TiF{sub 3} and Nb{sub 2}O{sub 5} is mainly attributed to electronic exchange reactions with hydrogen molecules, which improve the recombination of hydrogen atoms during dehydrogenation process of MgH{sub 2}. - Highlights: • Catalytic surface for MgH{sub 2} is achieved by high-energy ball milling. • Non-isothermal dehydrogenation behavior of MgH{sub 2} with TiF{sub 3} and/or Nb{sub 2}O{sub 5} is illustrated. • Dehydrogenation activation energies of synergetic catalyzed MgH{sub 2} are obtained. • Synergetic catalytic-dehydrogenation mechanism of TiF{sub 3} and Nb{sub 2}O{sub 5} is proposed.

  5. The Tool Life of Ball Nose end Mill Depending on the Different Types of Ramping

    Science.gov (United States)

    Vopát, Tomáš; Peterka, Jozef; Kováč, Martin

    2014-12-01

    The article deals with the cutting tool wear measurement process and tool life of ball nose end mill depending on upward ramping and downward ramping. The aim was to determine and compare the wear (tool life) of ball nose end mill for different types of copy milling operations, as well as to specify particular steps of the measurement process. In addition, we examined and observed cutter contact areas of ball nose end mill with machined material. For tool life test, DMG DMU 85 monoBLOCK 5-axis CNC milling machine was used. In the experiment, cutting speed, feed rate, axial depth of cut and radial depth of cut were not changed. The cutting tool wear was measured on Zoller Genius 3s universal measuring machine. The results show different tool life of ball nose end mills depending on the copy milling strategy.

  6. The Tool Life of Ball Nose end Mill Depending on the Different Types of Ramping

    Directory of Open Access Journals (Sweden)

    Vopát Tomáš

    2014-12-01

    Full Text Available The article deals with the cutting tool wear measurement process and tool life of ball nose end mill depending on upward ramping and downward ramping. The aim was to determine and compare the wear (tool life of ball nose end mill for different types of copy milling operations, as well as to specify particular steps of the measurement process. In addition, we examined and observed cutter contact areas of ball nose end mill with machined material. For tool life test, DMG DMU 85 monoBLOCK 5-axis CNC milling machine was used. In the experiment, cutting speed, feed rate, axial depth of cut and radial depth of cut were not changed. The cutting tool wear was measured on Zoller Genius 3s universal measuring machine. The results show different tool life of ball nose end mills depending on the copy milling strategy.

  7. A software tool for simulation of surfaces generated by ball nose end milling

    DEFF Research Database (Denmark)

    Bissacco, Giuliano

    2004-01-01

    , for prediction of surface topography of ball nose end milled surfaces, was developed. Such software tool is based on a simplified model of the ideal tool motion and neglects the effects due to run-out, static and dynamic deflections and error motions, but has the merit of generating in output a file in a format...... readable by a surface processor software (SPIP [2]), for calculation of a number of surface roughness parameters. In the next paragraph a description of the basic features of ball nose end milled surfaces is given, while in paragraph 3 the model is described....

  8. Amorphization of Fe-Nb by mechanical alloying

    International Nuclear Information System (INIS)

    Yang, J.Y.; Zhang, T.J.; Cui, K.; Li, X.G.; Zhang, J.

    1996-01-01

    Elemental powder mixtures of Fe x Nb 1-x were mechanically alloyed in a planetary ball mill. Powders milled for different times were characterized by X-ray diffraction, transmission and scanning electron microscopy, differential thermal analysis and microhardness measurement. The results show that powders with 0.30≤x≤0.70 could be amorphized after 30 h milling; the maximum hardness (Hv) of milled Fe 50 Nb 50 powders attained was 1490. Based on a thermodynamical analysis, the glass forming range of the Fe-Nb system was calculated, and found to agree with the experimental result very well. (orig.)

  9. Discrete element method based scale-up model for material synthesis using ball milling

    Science.gov (United States)

    Santhanam, Priya Radhi

    depending on hardness of brittle component relative to milling media. To improve the DEM model of the attritor mill, it is desired to avoid the removal of unrealistic, high-force events using an approach that would not predict such events in the first place. It is observed that during experiments in attritor, balls may jam causing an increased resistance to the impeller's rotation. The impeller may instantaneously slow down, quickly returning to its pre-set rotation rate. Previous DEM models did not account for such rapid changes in the impeller's rotation. In this work, this relationship between impeller's torque and rotation rate is obtained experimentally and introduced in DEM. As a result, predicted Ed, are shown to correlate well with the experimental data. Finally, a methodology is proposed combining an experiment and its DEM description enabling one to identify the appropriate interaction parameters for powder systems. The experiment uses a miniature vibrating hopper and can be applied to characterize the powder flow for variety of materials. The hopper is designed to hold up to 20,000 particles of 50-mum diameter, which can be directly described in DEM. Based on comparison of discharge rate from experiments and model, all 6 interaction parameters were analyzed and the ideal conditions identified for Zirconia beads. The values of these parameters for powders are generally not the same as those established for macroscopic bodies. In addition, effects of some other experimental parameters such as particle size distribution and amplitude of vibration are also investigated.

  10. Ammonia synthesis over multi-promoted iron catalysts obtained by high-energy ball-milling

    DEFF Research Database (Denmark)

    Jacobsen, C.J.H.; Jiang, Jianzhong; Mørup, Steen

    1999-01-01

    The feasibility of producing ammonia synthesis catalysts from high-energy ball-milling of a simple mixture of the constituent oxides has been investigated. The effect of ball-milling the fused oxidic precursor of the industrial KM1 ammonia synthesis catalyst has also been studied. The results show...

  11. Crystallite sizes of LiH before and after ball milling and thermal exposure

    International Nuclear Information System (INIS)

    Ortiz, Angel L.; Osborn, William; Markmaitree, Tippawan; Shaw, Leon L.

    2008-01-01

    The powder characteristics of lithium hydride (LiH) as a function of high-energy ball milling condition are systematically investigated via quantitative X-ray diffraction (XRD) analysis. The results obtained from the XRD analysis are compared with those attained from scanning electron microscopy (SEM), transmission electron microscopy (TEM), and specific surface area (SSA) analyses. The thermal stability of the ball-milled LiH is also investigated in order to provide physical insights into its cyclic stability in hydrogen sorption and desorption cycles. The results indicate that ball milling is effective in obtaining nano-crystalline LiH powder which is relatively stable with retention of nano-crystals after thermal exposure at 285 deg. C (equivalent to 0.58T m ) for 1 h. The good thermal stability observed is attributed to the presence of many pores in the agglomerates at the ball-milled condition. These pores effectively prevent crystal growth during the thermal exposure

  12. Crystallite sizes of LiH before and after ball milling and thermal exposure

    Energy Technology Data Exchange (ETDEWEB)

    Ortiz, Angel L. [Departamento de Electronica e Ingenieria Electromecanica, Universidad de Extremadura, Badajoz (Spain); Osborn, William; Markmaitree, Tippawan [Department of Chemical, Materials and Biomolecular Engineering, University of Connecticut, 97 North Eagleville Road, U-3136 Storrs, CT 06269-3136 (United States); Shaw, Leon L. [Department of Chemical, Materials and Biomolecular Engineering, University of Connecticut, 97 North Eagleville Road, U-3136 Storrs, CT 06269-3136 (United States)], E-mail: leon.shaw@uconn.edu

    2008-04-24

    The powder characteristics of lithium hydride (LiH) as a function of high-energy ball milling condition are systematically investigated via quantitative X-ray diffraction (XRD) analysis. The results obtained from the XRD analysis are compared with those attained from scanning electron microscopy (SEM), transmission electron microscopy (TEM), and specific surface area (SSA) analyses. The thermal stability of the ball-milled LiH is also investigated in order to provide physical insights into its cyclic stability in hydrogen sorption and desorption cycles. The results indicate that ball milling is effective in obtaining nano-crystalline LiH powder which is relatively stable with retention of nano-crystals after thermal exposure at 285 deg. C (equivalent to 0.58T{sub m}) for 1 h. The good thermal stability observed is attributed to the presence of many pores in the agglomerates at the ball-milled condition. These pores effectively prevent crystal growth during the thermal exposure.

  13. Influence of Solvent Composition on the Performance of Spray-Dried Co-Amorphous Formulations

    Directory of Open Access Journals (Sweden)

    Jaya Mishra

    2018-04-01

    Full Text Available Ball-milling is usually used to prepare co-amorphous drug–amino acid (AA mixtures. In this study, co-amorphous drug–AA mixtures were produced using spray-drying, a scalable industrially preferred preparation method. The influence of the solvent type and solvent composition was investigated. Mixtures of indomethacin (IND and each of the three AAs arginine, histidine, and lysine were ball-milled and spray-dried at a 1:1 molar ratio, respectively. Spray-drying was performed at different solvent ratios in (a ethanol and water mixtures and (b acetone and water mixtures. Different ratios of these solvents were chosen to study the effect of solvent mixtures on co-amorphous formulation. Residual crystallinity, thermal properties, salt/partial salt formation, and powder dissolution profiles of the IND–AA mixtures were investigated and compared to pure crystalline and amorphous IND. It was found that using spray-drying as a preparation method, all IND–AA mixtures could be successfully converted into the respective co-amorphous forms, irrespective of the type of solvent used, but depending on the solvent mixture ratios. Both ball-milled and spray-dried co-amorphous samples showed an enhanced dissolution rate and maintained supersaturation compared to the crystalline and amorphous IND itself. The spray-dried samples resulting in co-amorphous samples were stable for at least seven months of storage.

  14. Effect of high-energy ball milling in the structural and textural properties of kaolinite

    Directory of Open Access Journals (Sweden)

    E. C. Leonel

    2014-06-01

    Full Text Available Through the process of high-energy ball milling it is possible to obtain solid materials with higher surface area and different particle sizes. These characteristics are very important for some application such as adsorption. Besides, applications of some clays depend on the functionalization which, for kaolinite, takes place in the aluminol groups. Modification in the structural and textural properties of kaolinite by high-energy milling can improve functionalization of kaolinite due to the exposure of aluminol groups. In this work studies were done on the influence of high-energy ball milling on the morphological properties of kaolinite, taking into account parameters such as filling of the miller, number of balls and amount of mass to be milled. Moreover, studies involving milling kinetics of purified kaolinite were carried out to verify modification in the morphology of kaolinite with milling time.

  15. Ball mill tool for crushing coffee and cocoa beans base on fraction size sieving results

    Science.gov (United States)

    Haryanto, B.; Sirait, M.; Azalea, M.; Alvin; Cahyani, S. E.

    2018-02-01

    Crushing is one of the operation units that aimed to convert the size of solid material to be smoother particle’s size. The operation unit that can be used in this crushing is ball mill. The purpose of this study is to foresee the effect of raw material mass, grinding time, and the number of balls that are used in the ball mill tool related to the amount of raw material of coffee and cocoa beans. Solid material that has become smooth is then sieved with sieve mesh with size number: 50, 70, 100, and 140. It is in order to obtain the mass fraction that escaped from each sieve mesh. From the experiment, it can be concluded that mass percentage fraction of coffee powder is bigger than cocoa powder that escaped from the mesh. Hardness and humidity of coffee beans and cocoa beans have been the important factors that made coffee beans is easier to be crushed than cocoa beans.

  16. Matrix model of the grinding process of cement clinker in the ball mill

    Science.gov (United States)

    Sharapov, Rashid R.

    2018-02-01

    In the article attention is paid to improving the efficiency of production of fine powders, in particular Portland cement clinker. The questions of Portland cement clinker grinding in closed circuit ball mills. Noted that the main task of modeling the grinding process is predicting the granulometric composition of the finished product taking into account constructive and technological parameters used ball mill and separator. It is shown that the most complete and informative characterization of the grinding process in a ball mill is a grinding matrix taking into account the transformation of grain composition inside the mill drum. Shows how the relative mass fraction of the particles of crushed material, get to corresponding fraction. Noted, that the actual task of reconstruction of the matrix of grinding on the experimental data obtained in the real operating installations. On the basis of experimental data obtained on industrial installations, using matrix method to determine the kinetics of the grinding process in closed circuit ball mills. The calculation method of the conversion of the grain composition of the crushed material along the mill drum developed. Taking into account the proposed approach can be optimized processing methods to improve the manufacturing process of Portland cement clinker.

  17. Tungsten-nanodiamond composite powders produced by ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Nunes, D., E-mail: daniela.nunes@ist.utl.pt [Associacao Euratom/IST, Instituto de Plasmas e Fusao Nuclear, Instituto Superior Tecnico, Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); LNEG, Estrada do Paco do Lumiar, 1649-038 Lisboa (Portugal); ICEMS, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Livramento, V. [Associacao Euratom/IST, Instituto de Plasmas e Fusao Nuclear, Instituto Superior Tecnico, Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); LNEG, Estrada do Paco do Lumiar, 1649-038 Lisboa (Portugal); Mardolcar, U.V. [Departamento de Fisica, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Centro de Ciencias Moleculares e Materiais, Faculdade de Ciencias da Universidade de Lisboa, Campo Grande, 1749-016 Lisboa (Portugal); Correia, J.B. [LNEG, Estrada do Paco do Lumiar, 1649-038 Lisboa (Portugal); Carvalho, P.A. [ICEMS, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Departamento de Bioengenharia, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal)

    2012-07-15

    The major challenge in producing tungsten-nanodiamond composites by ball milling lies in successfully dispersing carbon nanoparticles in the metallic matrix while keeping carbide formation at a minimum. Processing windows for carbide minimization have been established through systematic variation of the nanodiamond fraction, milling energy and milling time. Materials characterization has been carried out by X-ray diffraction, scanning and transmission electron microscopy and microhardness testing. Nanostructured matrices with homogeneously dispersed particles that preserved the diamond structure have been produced. Differential thermal analysis has been used to evaluate the composites thermal stability.

  18. Preparation of iron sulphides by high energy ball milling

    DEFF Research Database (Denmark)

    Lin, R.; Jiang, Jianzhong; Larsen, R.K.

    1998-01-01

    The reaction of a powder mixture consisting of 50 a.% Fe and 50 a.% S during high energy ball milling has been studied by x-ray diffraction and Mossbauer spectroscopy. After around 19 h of milling FeS2 and FeS havebeen formed. By further milling the FeS compound becomes dominating and only Fe......S with an average crystallite size of about 10 nm was observed after milling times longer than 67 h. Mossbauer spectra obtained with applied fields show that the particles are antiferromagnetic or have a strongly canted spin structure....

  19. Low-temperature magnetic behavior of ball-milled copper ferrite

    DEFF Research Database (Denmark)

    Goya, G.F.; Rechenberg, H.R.; Jiang, Jianzhong

    1999-01-01

    We present a study on magnetic properties of CuFe2O4 nanoparticles, produced by high-energy ball milling. The series of samples obtained, with average particle sizes LFAN alpha d RTAN ranging from 61 nm to 9 nm, display increasing relaxation effects at room temperature. Irreversibility of the mag......We present a study on magnetic properties of CuFe2O4 nanoparticles, produced by high-energy ball milling. The series of samples obtained, with average particle sizes LFAN alpha d RTAN ranging from 61 nm to 9 nm, display increasing relaxation effects at room temperature. Irreversibility...... of the magnetization and shifts to negative fields in the hysteresis loops are observed below T-f APEQ 55 K, indicating unidirectional magnetic anisotropy in milled samples. These features could be explained by assuming the formation of a spin-disordered surface layer, which is exchange-coupled to the ferrimagnetic...

  20. Dry grinding of talc in a stirred ball mill

    Directory of Open Access Journals (Sweden)

    Cayirli Serkan

    2016-01-01

    Full Text Available The aim of this work was to investigate micro fine size dry grindability of talc in a stirred ball mill. The effects of various parameters such as grinding time, stirrer speed, powder filling ratio and ball filling ratio were investigated. Alumina balls were used as grinding media. Experiments were carried out using the 24 full factorial design. The main and interaction effects were evaluated using the Yates method. Test results were evaluated on the basis of product size and surface area.

  1. Reversible a-Fe2O3 to Fe3O4 transformation during ball milling

    DEFF Research Database (Denmark)

    Linderoth, Søren; Jiang, Jianzhong; Mørup, Steen

    1997-01-01

    The transformation of hematite to magnetite by high-energy ball milling in a sealed container has been studied by Mossbauer spectroscopy and x-ray diffraction. Mechanisms for this transformation are critically discussed. The dominant mechanism is concluded to be due to bond breaking during the high...... energy ball milling followed by release of the oxygen from the vial. The reverse transformation, magnetite to hematite, is demonstrated to occur by ball milling in air. Mechanisms for this reverse transformation are also put forward....

  2. Phase evolution during early stages of mechanical alloying of Cu–13 wt.% Al powder mixtures in a high-energy ball mill

    International Nuclear Information System (INIS)

    Dudina, Dina V.; Lomovsky, Oleg I.; Valeev, Konstantin R.; Tikhov, Serguey F.; Boldyreva, Natalya N.; Salanov, Aleksey N.; Cherepanova, Svetlana V.; Zaikovskii, Vladimir I.; Andreev, Andrey S.; Lapina, Olga B.; Sadykov, Vladislav A.

    2015-01-01

    Highlights: • Phase formation during early stages of Cu–Al mechanical alloying was studied. • The products of mechanical alloying are of highly non-equilibrium character. • X-ray amorphous phases are present in the products of mechanical alloying. • An Al-rich X-ray amorphous phase is distributed between the crystallites. - Abstract: We report the phase and microstructure evolution of the Cu–13 wt.% Al mixture during treatment in a high-energy planetary ball mill with a particular focus on the early stages of mechanical alloying. Several characterization techniques, including X-ray diffraction phase analysis, nuclear magnetic resonance spectroscopy, differential dissolution, thermal analysis, and electron microscopy/elemental analysis, have been combined to study the evolution of the phase composition of the mechanically alloyed powders and describe the microstructure of the multi-phase products of mechanical alloying at different length scales. The following reaction sequence has been confirmed: Cu + Al → CuAl 2 (+Cu) → Cu 9 Al 4 + (Cu) → Cu(Al). The phase evolution was accompanied by the microstructure changes, the layered structure of the powder agglomerates disappearing with milling time. This scheme is further complicated by the processes of copper oxidation, reduction of copper oxides by metallic aluminum, and by variation of the stoichiometry of Cu(Al) solid solutions with milling time. Substantial amounts of X-ray amorphous phases were detected as well. Differential dissolution technique has revealed that a high content of aluminum in the Cu(Al) solid solution-based powders is due to the presence of Al-rich phases distributed between the Cu(Al) crystallites

  3. Defect induced electronic states and magnetism in ball-milled graphite.

    Science.gov (United States)

    Milev, Adriyan; Dissanayake, D M A S; Kannangara, G S K; Kumarasinghe, A R

    2013-10-14

    The electronic structure and magnetism of nanocrystalline graphite prepared by ball milling of graphite in an inert atmosphere have been investigated using valence band spectroscopy (VB), core level near-edge X-ray absorption fine structure (NEXAFS) spectroscopy and magnetic measurements as a function of the milling time. The NEXAFS spectroscopy of graphite milled for 30 hours shows simultaneous evolution of new states at ~284.0 eV and at ~290.5 eV superimposed upon the characteristic transitions at 285.4 eV and 291.6 eV, respectively. The modulation of the density of states is explained by evolution of discontinuities within the sheets and along the fracture lines in the milled graphite. The magnetic measurements in the temperature interval 2-300-2 K at constant magnetic field strength show a correlation between magnetic properties and evolution of the new electronic states. With the reduction of the crystallite sizes of the graphite fragments, the milled material progressively changes its magnetic properties from diamagnetic to paramagnetic with contributions from both Pauli and Curie paramagnetism due to the evolution of new states at ~284 and ~290.5 eV, respectively. These results indicate that the magnetic behaviour of ball-milled graphite can be manipulated by changing the milling conditions.

  4. Transforming from paramagnetism to room temperature ferromagnetism in CuO by ball milling

    Directory of Open Access Journals (Sweden)

    Daqiang Gao

    2011-12-01

    Full Text Available In this work, we experimentally demonstrate that it is possible to induce ferromagnetism in CuO by ball milling without any ferromagnetic dopant. The magnetic measurements indicate that paramagnetic CuO is driven to the ferromagnetic state at room temperature by ball milling gradually. The saturation magnetization of the milled powders is found to increase with expanding the milling time and then decrease by annealing under atmosphere. The fitted X-ray photoelectron spectroscopy results indicate that the observed induction and weaken of the ferromagnetism shows close relationship with the valence charged oxygen vacancies (Cu1+-VO in CuO.

  5. Effect of additional nickel on crystallization degree evolution of expanded graphite during ball-milling and annealing

    International Nuclear Information System (INIS)

    Wang Liqin; Yue Xueqing; Zhang Fucheng; Zhang Ruijun

    2010-01-01

    Expanded graphite (EG) and a mixture of EG and nickel (EG-Ni system) were ball-milled and subsequently annealed, respectively. The products were characterized by X-ray diffraction (XRD), Raman spectra and transmission electron microscopy (TEM). After 100 h milling, the average crystallite thickness (L c ) of EG and EG-Ni system deceases from 14.5 to 8.0 and 9.6 nm, respectively, while the interlayer spacing (d 002 ) increases from 0.3341 to 0.3371 and 0.3348 nm, respectively. It can be concluded that ball-milling decreases the crystallization degree of EG, while the additional nickel restrains this process. For the samples ball-milled for 80 h, the disorder parameter I D /(I D + I G ) ratio of EG and EG-Ni system is in the range of 20.7-55.8% and 31.7-45.8%, respectively, implying that the presence of nickel is beneficial to more homogeneous ball-milling of EG. When the samples after ball-milling for 80 h were annealed for 4 h, the average crystallite thickness of EG and EG-Ni system increases from 8.5 to 9.0 nm and from 11.8 to 15.5 nm, respectively. It is deduced that annealing improves the crystallization degree of ball-milled EG, and the additional nickel is helpful for this process.

  6. Fabrication of Ti-Ni-Cu shape memory alloy powders by ball milling method

    International Nuclear Information System (INIS)

    Kang, S.; Nam, T.

    2001-01-01

    Ti-Ni and Ti-Ni-Cu shape memory alloy powders have been fabricated by ball milling method, and then alloying behavior and transformation behavior were investigated by means of optical microscopy, electron microscopy, X-ray diffraction and differential scanning calorimetry. As milled Ti-Ni powders fabricated with milling time less than 20 hrs was a mixture of pure elemental Ti and Ni, and therefore it was unable to obtain alloy powders because the combustion reaction between Ti and Ni occurred during heat treatment. Since those fabricated with milling time more than 20 hrs was a mixture of Ti-rich and Ni-rich Ti-Ni solid solution, however, it was possible to obtain alloy powders without the combustion reaction during heat treatment. Clear exothermic and endothermic peaks appeared in the cooling and heating curves, respectively in DSC curves of 20 hrs and 30 hrs milled Ti-Ni powders. On the other hand, in DSC curves of 1 hr, 10 hrs, 50 hrs and 100 hrs, the thermal peaks were almost discernible. The most optimum ball milling time for fabricating Ti-Ni alloy powders was 30 hrs. Ti-40Ni-10Cu(at%) alloy powders were fabricated successfully by ball milling conditions with rotating speed of 100 rpm and milling time of 30 hrs. (author)

  7. Effect of ball-milling to the surface morphology of CaCO3

    Science.gov (United States)

    Sulimai, N. H.; Rani, Rozina Abdul; Khusaimi, Z.; Abdullah, S.; Salifairus, M. J.; Alrokayan, Salman; Khan, Haseeb; Rusop, M.

    2018-05-01

    Calcium Carbonate can be synthesized in many approaches. This work studied on the physical changes to Calcium Carbonate (CaCO3) by ball-milling activity in different parameters; number of ball; collision duration; revolution per minute (RPM). Zirconia balls were used in the work because it has the best durability to withstand ball-milling conditions set. Industrial grade CaCO3 particles that were run in aforementioned parameters were characterized by Field Emission Scanning Electron Microscope (FE-SEM) to study the physical changes on the size and surface of the CaCO3. They were also characterized with Fourier Transform Infra-red Spectroscopy (FTIR) were fingerprint of CaCO3 regions were identified and any changes in the band position and intensity were discussed. Number of Zirconia balls and collision duration is directly proportional to the absorbance intensity whereas it is inversely proportional for the rpm. The best number of parameters producing the highest Absorbance is 100 Zirconia balls in duration of 1 hour and 100rpm.

  8. Comparative Study by MS and XRD of Fe50Al50 Alloys Produced by Mechanical Alloying, Using Different Ball Mills

    International Nuclear Information System (INIS)

    Rojas Martinez, Y.; Perez Alcazar, G. A.; Bustos Rodriguez, H.; Oyola Lozano, D.

    2005-01-01

    In this work we report a comparative study of the magnetic and structural properties of Fe 50 Al 50 alloys produced by mechanical alloying using two different planetary ball mills with the same ball mass to powder mass relation. The Fe 50 Al 50 sample milled during 48 h using the Fritsch planetary ball mill pulverisette 5 and balls of 20 mm, presents only a bcc alloy phase with a majority of paramagnetic sites, whereas that sample milled during the same time using the Fritsch planetary ball mill pulverisette 7 with balls of 15 mm, presents a bcc alloy phase with paramagnetic site (doublet) and a majority of ferromagnetic sites which include pure Fe. However for 72 h of milling this sample presents a bcc paramagnetic phase, very similar to that prepared with the first system during 48 h. These results show that the conditions used in the first ball mill equipment make more efficient the milling process.

  9. Preparation of natural pyrite nanoparticles by high energy planetary ball milling as a nanocatalyst for heterogeneous Fenton process

    Energy Technology Data Exchange (ETDEWEB)

    Fathinia, Siavash [Department of Mining Engineering, Faculty of Engineering and Technology, Imam Khomeini International University, Qazvin (Iran, Islamic Republic of); Research Laboratory of Advanced Water and Wastewater Treatment Processes, Department of Applied Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of); Fathinia, Mehrangiz [Research Laboratory of Advanced Water and Wastewater Treatment Processes, Department of Applied Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of); Rahmani, Ali Akbar [Department of Mining Engineering, Faculty of Engineering and Technology, Imam Khomeini International University, Qazvin (Iran, Islamic Republic of); Khataee, Alireza, E-mail: a_khataee@tabrizu.ac.ir [Research Laboratory of Advanced Water and Wastewater Treatment Processes, Department of Applied Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)

    2015-02-01

    Graphical abstract: - Highlights: • Pyrite nanoparticles were successfully produced by planetary ball milling process. • The physical and chemical properties of pyrite nanoparticles were fully examined. • The degradation of AO7 was notably enhanced by pyrite nanoparticles Fenton system. • The influences of basic operational parameters were investigated using CCD. - Abstract: In the present study pyrite nanoparticles were prepared by high energy mechanical ball milling utilizing a planetary ball mill. Various pyrite samples were produced by changing the milling time from 2 h to 6 h, in the constant milling speed of 320 rpm. X-ray diffraction (XRD), scanning electron microscopy (SEM) linked with energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy (FT-IR) analysis and Brunauer–Emmett–Teller (BET) were performed to explain the characteristics of primary (unmilled) and milled pyrite samples. The average particle size distribution of the produced pyrite during 6 h milling was found to be between 20 nm and 100 nm. The catalytic performance of the different pyrite samples was examined in the heterogeneous Fenton process for degradation of C.I. Acid Orange 7 (AO7) solution. Results showed that the decolorization efficiency of AO7 in the presence of 6 h-milled pyrite sample was the highest. The impact of key parameters on the degradation efficiency of AO7 by pyrite nanoparticles catalyzed Fenton process was modeled using central composite design (CCD). Accordingly, the maximum removal efficiency of 96.30% was achieved at initial AO7 concentration of 16 mg/L, H{sub 2}O{sub 2} concentration of 5 mmol/L, catalyst amount of 0.5 g/L and reaction time of 25 min.

  10. Magnetoresistivity and microstructure of YBa2Cu3Oy prepared using planetary ball milling

    International Nuclear Information System (INIS)

    Hamrita, A.; Ben Azzouz, F.; Madani, A.; Ben Salem, M.

    2012-01-01

    Superconducting properties of YBa 2 Cu 3 O y prepared using planetary ball milling were studied. Y-deficient YBa 2 Cu 3 O y nanoparticles are embedded in the superconducting matrix. Ball milled sample exhibits a large magnetoresistivity in weak magnetic fields at 77 K. We have studied the microstructure and the magnetoresistivity of polycrystalline YBa 2 Cu 3 O y (YBCO or Y-123 for brevity) embedded with nanoparticles of Y-deficient YBCO, generated by the planetary ball milling technique. Bulk samples were synthesized from a precursor YBCO powder, which was prepared from commercial high purity Y 2 O 3 , Ba 2 CO 3 and CuO via a one-step annealing process in air at 950 °C. After planetary ball milling of the precursor, the powder was uniaxially pressed and subsequently annealed at 950 °C in air. Phase analysis by X-ray diffraction (XRD), granular structure examination by scanning electron microscopy (SEM), microstructure investigation by transmission electron microscopy (TEM) coupled with energy dispersive X-ray spectroscopy (EDXS) were carried out. TEM analyses show that nanoparticles of Y-deficient YBCO, generated by ball milling, are embedded in the superconducting matrix. Electrical resistance as a function of temperature, ρ(T), revealed that the zero resistance temperature, T co , is 84.5 and 90 K for the milled and unmilled samples respectively. The milled ceramics exhibit a large magnetoresistance in weak magnetic fields at liquid nitrogen temperature. This attractive effect is of high significance as it makes these materials promising candidates for practical application in magnetic field sensor devices.

  11. Thermogravimetric and Differential Scanning Calorimetric Behavior of Ball-Milled Nuclear Graphite

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Eung Seon; Kim, Min Hwan; Kim, Yong Wan [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of); Park, Yi Hyun; Cho, Seung Yon [National Fusion Research Institute, Daejeon (Korea, Republic of)

    2013-10-15

    An examination was made to characterize the oxidation behavior of ball-milled nuclear graphite powder through a TG-DSC analysis. With the ball milling time, the BET surface area increased with the reduction of particle size, but decreased with the chemisorptions of O{sub 2} on the activated surface. The enhancement of the oxidation after the ball milling is attributed to both increases in the specific surface area and atomic scale defects in the graphite structure. In a high temperature gas-cooled reactor, nuclear graphite has been widely used as fuel elements, moderator or reflector blocks, and core support structures owing to its excellent moderating power, mechanical properties and machinability. For the same reason, it will be used in a helium cooled ceramic reflector test blanket module for the ITER. Each submodule has a seven-layer breeding zone, including three neutron multiplier layers packed with beryllium pebbles, three lithium ceramic pebbles packed tritium breeder layers, and a reflector layer packed with 1 mm diameter graphite pebbles to reduce the volume of beryllium. The abrasion of graphite structures owing to relative motion or thermal cycle during operation may produce graphite dust. It is expected that graphite dust will be more oxidative than bulk graphite, and thus the oxidation behavior of graphite dust must be examined to analyze the safety of the reactors during an air ingress accident. In this study, the thermal stability of ball-milled graphite powder was investigated using a simultaneous thermogravimeter-differential scanning calorimeter.

  12. Effect of ball milling time on thermoelectric properties of bismuth telluride nanomaterials

    Science.gov (United States)

    Khade, Poonam; Bagwaiya, Toshi; Bhattacharaya, Shovit; Singh, Ajay; Jha, Purushottam; Shelke, Vilas

    2018-04-01

    The effect of different milling time on thermoelectric properties of bismuth telluride (Bi2Te3) was investigated. The nanomaterial was prepared by varying the ball milling time and followed by hot press sintering. The crystal structure and phase formation were verified by X-ray diffraction and Raman Spectroscopy. The experimental results show that electrical conductivity increases whereas thermal conductivity decreases with increasing milling time. The negative sign of seebeck coefficient indicate the n-type nature with majority charge carriers of electrons. A maximum figure of merit about 0.55 is achieved for l5hr ball milled Bi2Te3 sample. The present study demonstrates the simple and cost-effective method for synthesis of Bi2Te3 thermoelectric material at large scale thermoelectric applications.

  13. An analytical model for force prediction in ball nose micro milling of inclined surfaces

    DEFF Research Database (Denmark)

    Bissacco, Giuliano; Hansen, Hans Nørgaard; De Chiffre, Leonardo

    2010-01-01

    Ball nose micro milling is a key process for the generation of free form surfaces and inclined surfaces often present in mould inserts for micro replication. This paper presents a new cutting force model for ball nose micro milling that is capable of taking into account the effect of the edge...

  14. Cryogenic milling for the fabrication of high J{sub c} MgB{sub 2} bulk superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Kim, D. N.; Kang, M. O.; Park, H. W. [Korea University of Technology and Education, Cheonan (Korea, Republic of); Jun, B. H.; Kim, C. J. [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2017-06-15

    Cryogenic milling which is a combined process of low-temperature treatment and mechanical milling was applied to fabricate high critical current density (J{sub c}) MgB{sub 2} bulk superconductors. Liquid nitrogen was used as a coolant, and no solvent or lubricant was used. Spherical Mg (6-12 μm, 99.9 % purity) and plate-like B powder (⁓ 1 μm, 97 % purity) were milled simultaneously for various time periods (0, 2, 4, 6 h) at a rotating speed of 500 rpm using ZrO{sub 2} balls. The (Mg{sup +2B}) powders milled were pressed into pellets and heat-treated at 700°C for 1 h in flowing argon. The use of cryomilled powders as raw materials promoted the formation reaction of superconducting MgB{sub 2}, reduced the grain size of MgB{sub 2}, and suppressed the formation of impurity MgO. The superconducting critical temperature (T{sub c}) of MgB{sub 2} was not influenced as the milling time (t) increased up to 6 h. Meanwhile, the critical current density (J{sub c}) of MgB{sub 2} increased significantly when t increased to 4 h. When t increased further to 6 h, however, Jc decreased. The J{sub c} enhancement of MgB{sub 2} by cryogenic milling is attributed to the formation of the fine grain MgB{sub 2} and a suppression of the MgO formation.

  15. Study on the bonding state for carbon-boron nitrogen with different ball milling time

    International Nuclear Information System (INIS)

    Xiong, Y.H.; Xiong, C.S.; Wei, S.Q.; Yang, H.W.; Mai, Y.T.; Xu, W.; Yang, S.; Dai, G.H.; Song, S.J.; Xiong, J.; Ren, Z.M.; Zhang, J.; Pi, H.L.; Xia, Z.C.; Yuan, S.L.

    2006-01-01

    The varied bonding state and microstructure characterization were discussed for carbon-boron nitrogen (CBN) with abundant phase structure and nanostructure, which were synthesized directly by mechanical alloying technique at room temperature. According to the results of SEM and X-ray photoelectron spectroscopy (XPS) of CBN with different ball milling time, it is substantiated that the bonding state and microstructure for CBN were closely related to the ball milling time. With the increase of the ball milling time, some new chemical bonding states of CBN were observed, which implies that some new bonding state and microstructures have been formed. The results of XPS are accordance with that of X-ray diffraction of CBN

  16. Reliable Mechanochemistry: Protocols for Reproducible Outcomes of Neat and Liquid Assisted Ball-mill Grinding Experiments.

    Science.gov (United States)

    Belenguer, Ana M; Lampronti, Giulio I; Sanders, Jeremy K M

    2018-01-23

    The equilibrium outcomes of ball mill grinding can dramatically change as a function of even tiny variations in the experimental conditions such as the presence of very small amounts of added solvent. To reproducibly and accurately capture this sensitivity, the experimentalist needs to carefully consider every single factor that can affect the ball mill grinding reaction under investigation, from ensuring the grinding jars are clean and dry before use, to accurately adding the stoichiometry of the starting materials, to validating that the delivery of solvent volume is accurate, to ensuring that the interaction between the solvent and the powder is well understood and, if necessary, a specific soaking time is added to the procedure. Preliminary kinetic studies are essential to determine the necessary milling time to achieve equilibrium. Only then can exquisite phase composition curves be obtained as a function of the solvent concentration under ball mill liquid assisted grinding (LAG). By using strict and careful procedures analogous to the ones here presented, such milling equilibrium curves can be obtained for virtually all milling systems. The system we use to demonstrate these procedures is a disulfide exchange reaction starting from the equimolar mixture of two homodimers to obtain at equilibrium quantitative heterodimer. The latter is formed by ball mill grinding as two different polymorphs, Form A and Form B. The ratio R = [Form B] / ([Form A] + [Form B]) at milling equilibrium depends on the nature and concentration of the solvent in the milling jar.

  17. Scale-up of organic reactions in ball mills: process intensification with regard to energy efficiency and economy of scale.

    Science.gov (United States)

    Stolle, Achim; Schmidt, Robert; Jacob, Katharina

    2014-01-01

    The scale-up of the Knoevenagel-condensation between vanillin and barbituric acid carried out in planetary ball mills is investigated from an engineering perspective. Generally, the reaction proceeded in the solid state without intermediate melting and afforded selectively only one product. The reaction has been used as a model to analyze the influence and relationship of different parameters related to operation in planetary ball mills. From the viewpoint of technological parameters the milling ball diameter, dMB, the filling degree with respect to the milling balls' packing, ΦMB,packing, and the filling degree of the substrates with respect to the void volume of the milling balls' packing, ΦGS, have been investigated at different reaction scales. It was found that milling balls with small dMB lead to higher yields within shorter reaction time, treaction, or lower rotation frequency, rpm. Thus, the lower limit is set considering the technology which is available for the separation of the milling balls from the product after the reaction. Regarding ΦMB,packing, results indicate that the optimal value is roughly 50% of the total milling beakers' volume, VB,total, independent of the reaction scale or reaction conditions. Thus, 30% of VB,total are taken by the milling balls. Increase of the initial batch sizes changes ΦGS significantly. However, within the investigated parameter range no negative influence on the yield was observed. Up to 50% of VB,total can be taken over by the substrates in addition to 30% for the total milling ball volume. Scale-up factors of 15 and 11 were realized considering the amount of substrates and the reactor volume, respectively. Beside technological parameters, variables which influence the process itself, treaction and rpm, were investigated also. Variation of those allowed to fine-tune the reaction conditions in order to maximize the yield and minimize the energy intensity.

  18. Performance Study of Graphite Anode Slurry in Lithium-ion Flow Battery by Ball Milling

    Directory of Open Access Journals (Sweden)

    FENG Cai-mei

    2018-02-01

    Full Text Available Graphite anode slurry of lithium-ion flow battery was prepared by the method of ball milling. The morphology, conductivity, specific capacity and cycle performance of graphite anode slurry were studied. Results show that the addition of conductive carbon material can improve the suspension stability of the electrode slurry; the ball milling process can not only improve the suspension stability but also reduce the resistivity of the mixed powders of graphite and conductive carbon materials, the ball milling effect is satisfactory when the mass ratio of the balls and the solid particles is 5:1, but too high ratio of the milling ball and the solid materials can destroy the layer structure of the graphite and affect the stability of the slurry. Increasing the fraction of the graphite and conductive carbon materials can form stable electrical network structure in the slurry and improve the reversible capacity; at the premise of keeping the flowability of the electrode slurry, the reversible specific capacity can be more than 40mAh/g. The capacity loss of graphite anode slurry mainly occurs in the first charging-discharging process, as the increase of the cycles, the capacity loss rate decreases, the capacity goes stable after 5 cycles.

  19. Effects of high energy ball milling on synthesis and characteristics of Ti-Mg alloys

    CSIR Research Space (South Africa)

    Chikwanda, HK

    2008-01-01

    Full Text Available The synthesis of Ti-Mg alloys using mechanical alloying method has been investigated. Effects of the mechanical alloying parameters on the resultant microstructural features have been studied. This work presents the effects of milling speed...

  20. Colloidal Precursors from 'Ball-Milling in Liquid Medium' Process for CuInSe2 Thin Film

    International Nuclear Information System (INIS)

    Chung, Jae Hoon; Kim, Seung Joo

    2010-01-01

    CIS thin film can be fabricated by using the precursor obtained through ball-milling the elemental reagents in liquid media. The amorphous colloidal precursor with good dispersity was prepared in the medium that contains strong base and polar solvent (2 M ethylenediamine in DMF solution as used in this study). The 'ball-milling in liquid medium' method requires only elemental sources as starting materials and a proper solution so that it can be employed without additional processes for separation and purification. As a simple and less-toxic preparative route, this method would be practically available to prepare CIS-related solar cells. CuInSe 2 (CIS) and related chalcopyrite compounds are very promising materials for thin film solar cells due to their favorable band gap, high optical absorption coefficient and long-term stability. CIS-based solar cells have shown the highest conversion efficiency reaching a value of 20%. However, the vacuum-based processes that are used to fabricate CIS thin-films have some drawbacks such as the complexity in process, high production cost and difficulty in scaling up. Recently, several research groups have proposed different non-vacuum deposition processes for CIS solar cell. For example, H. W. Hillhouse et al. prepared the CIS absorber layer by using 'nanocrystal ink method' in which a colloidal nanocrystal ink was obtained from reaction of CuCl, InCl 3 and Se in oleylamine. D. B. Mitzi et al. used a solution-based precursor that was prepared by dissolution of Cu 2 Se, In 2 Se 3 , Ga 2 Se 3 and Se in hydrazine to fabricate the Ga-containing absorber layer, Cu(In,Ga)Se 2

  1. Fabrication of lanthanum-doped thorium dioxide by high-energy ball milling and spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Scott, Spencer M.; Yao, Tiankai [Department of Mechanical, Aerospace, and Nuclear Engineering, Rensselaer Polytechnic Institute, 110 8th Street, Troy, NY 12180 (United States); Lu, Fengyuan [Department of Mechanical & Industrial Engineering, Louisiana State University, Baton Rouge, LA 70803 (United States); Xin, Guoqing; Zhu, Weiguang [Department of Mechanical, Aerospace, and Nuclear Engineering, Rensselaer Polytechnic Institute, 110 8th Street, Troy, NY 12180 (United States); Lian, Jie, E-mail: lianj@rpi.edu [Department of Mechanical, Aerospace, and Nuclear Engineering, Rensselaer Polytechnic Institute, 110 8th Street, Troy, NY 12180 (United States)

    2017-03-15

    Abstract: High-energy ball milling was used to synthesize Th{sub 1-x}La{sub x}O{sub 2-0.5x} (x = 0.09, 0.23) solid solutions, as well as improve the sinterability of ThO{sub 2} powders. Dense La-doped ThO{sub 2} pellets with theoretical density above 94% were consolidated by spark plasma sintering at temperatures above 1400 °C for 20 min, and the densification behavior and the non-equilibrium effects on phase and structure were investigated. A lattice contraction of the SPS-densified pellets occurred with increasing ball milling duration, and a secondary phase with increased La-content was observed in La-doped pellets. A dependence on the La-content and sintering duration for the onset of localized phase segregation has been proposed. The effects of high-energy ball milling, La-content, and phase formation on the thermal diffusivity were also studied for La-doped ThO{sub 2} pellets by laser flash measurement. Increasing La-content and high energy ball milling time decreases thermal diffusivity; while the sintering peak temperature and holding time beyond 1600 °C dramatically altered the temperature dependence of the thermal diffusivity beyond 600 °C. - Highlights: • Lanthanum incorporation into ThO{sub 2} by high energy ball milling and rapid consolidation by spark plasma sintering. • Elucidation of phase behavior of the La-doped ThO{sub 2} and the contributions of La incorporation and SPS sintering conditions. • Investigation of the effects of La incorporation and high energy ball milling on the thermal behavior of La-doped ThO{sub 2}.

  2. Synthesis of the hydride mixtures (1 - x)AlH3/xMgH2 (0 ≤ x ≤ 0.3) by ball milling and their hydrogen storage properties

    International Nuclear Information System (INIS)

    Iosub, V.; Matsunaga, T.; Tange, K.; Ishikiriyama, M.; Miwa, K.

    2009-01-01

    In an effort to thermodynamically stabilize the alane (i.e., to increase the desorption enthalpy), partial substitution of Mg for Al was investigated by ball milling the mixtures (1 - x)AlH 3 /xMgH 2 (x = 0.1, 0.2 and 0.3). Rietveld analysis of the XRD profiles showed that the cell volume of α-AlH 3 increased with the Mg substitution rate, and thereby formation of solid solutions was assumed (x ≤ 0.05). In agreement with the experimental results, theoretical calculations indicated that a hypothetical supercell structure (MgAl 15 )H 47 (x = 0.0625), which contained a hydrogen vacancy, was at least metastable. However, the effect of alane stabilization by Mg substitution for Al was not observed, either by experiment or by simulation, and only an increase in the activation energy was measured.

  3. Hydrogen storage materials discovery via high throughput ball milling and gas sorption.

    Science.gov (United States)

    Li, Bin; Kaye, Steven S; Riley, Conor; Greenberg, Doron; Galang, Daniel; Bailey, Mark S

    2012-06-11

    The lack of a high capacity hydrogen storage material is a major barrier to the implementation of the hydrogen economy. To accelerate discovery of such materials, we have developed a high-throughput workflow for screening of hydrogen storage materials in which candidate materials are synthesized and characterized via highly parallel ball mills and volumetric gas sorption instruments, respectively. The workflow was used to identify mixed imides with significantly enhanced absorption rates relative to Li2Mg(NH)2. The most promising material, 2LiNH2:MgH2 + 5 atom % LiBH4 + 0.5 atom % La, exhibits the best balance of absorption rate, capacity, and cycle-life, absorbing >4 wt % H2 in 1 h at 120 °C after 11 absorption-desorption cycles.

  4. Effect of milling time on the structure, particle size, and morphology of montmorillonite

    International Nuclear Information System (INIS)

    Abareshi, M.

    2017-01-01

    In the current research, effect of milling on the structure, particle size and morphology of montmorillonite was investigated. For this purpose, the montmorillonite was analyzed by X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. Then the montmorillonite was milled using high energy planetary ball mill at different milling times (1-60 hours). After that, the structure, particle size and morphology of all samples were investigated by XRD, FTIR, SEM, and transmission electron microscopy. Results showed that the ball milling causes the particle size reduction of clay and separation of the clay layers. Moreover, ball milling increases the overall structural disorder and transforms the crystalline structure into an amorphous phase. Also, the morphology of clay particle changes from layered to aggregates of almost rounded particles after 60 hours of milling.

  5. Colloidal Precursors from 'Ball-Milling in Liquid Medium' Process for CuInSe{sub 2} Thin Film

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Jae Hoon; Kim, Seung Joo [Ajou University, Suwon (Korea, Republic of)

    2010-09-15

    CIS thin film can be fabricated by using the precursor obtained through ball-milling the elemental reagents in liquid media. The amorphous colloidal precursor with good dispersity was prepared in the medium that contains strong base and polar solvent (2 M ethylenediamine in DMF solution as used in this study). The 'ball-milling in liquid medium' method requires only elemental sources as starting materials and a proper solution so that it can be employed without additional processes for separation and purification. As a simple and less-toxic preparative route, this method would be practically available to prepare CIS-related solar cells. CuInSe{sub 2} (CIS) and related chalcopyrite compounds are very promising materials for thin film solar cells due to their favorable band gap, high optical absorption coefficient and long-term stability. CIS-based solar cells have shown the highest conversion efficiency reaching a value of 20%. However, the vacuum-based processes that are used to fabricate CIS thin-films have some drawbacks such as the complexity in process, high production cost and difficulty in scaling up. Recently, several research groups have proposed different non-vacuum deposition processes for CIS solar cell. For example, H. W. Hillhouse et al. prepared the CIS absorber layer by using 'nanocrystal ink method' in which a colloidal nanocrystal ink was obtained from reaction of CuCl, InCl{sub 3} and Se in oleylamine. D. B. Mitzi et al. used a solution-based precursor that was prepared by dissolution of Cu{sub 2}Se, In{sub 2}Se{sub 3}, Ga{sub 2}Se{sub 3} and Se in hydrazine to fabricate the Ga-containing absorber layer, Cu(In,Ga)Se{sub 2}.

  6. Comparative Study by MS and XRD of Fe{sub 50}Al{sub 50} Alloys Produced by Mechanical Alloying, Using Different Ball Mills

    Energy Technology Data Exchange (ETDEWEB)

    Rojas Martinez, Y., E-mail: yarojas@ut.edu.co [University of Tolima, Department of Physics (Colombia); Perez Alcazar, G. A. [University of Valle, Department of Physics (Colombia); Bustos Rodriguez, H.; Oyola Lozano, D., E-mail: doyolalozano@yahoo.com.mx [University of Tolima, Department of Physics (Colombia)

    2005-02-15

    In this work we report a comparative study of the magnetic and structural properties of Fe{sub 50}Al{sub 50} alloys produced by mechanical alloying using two different planetary ball mills with the same ball mass to powder mass relation. The Fe{sub 50}Al{sub 50} sample milled during 48 h using the Fritsch planetary ball mill pulverisette 5 and balls of 20 mm, presents only a bcc alloy phase with a majority of paramagnetic sites, whereas that sample milled during the same time using the Fritsch planetary ball mill pulverisette 7 with balls of 15 mm, presents a bcc alloy phase with paramagnetic site (doublet) and a majority of ferromagnetic sites which include pure Fe. However for 72 h of milling this sample presents a bcc paramagnetic phase, very similar to that prepared with the first system during 48 h. These results show that the conditions used in the first ball mill equipment make more efficient the milling process.

  7. Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al₂O₃ Nanocomposite Synthesized by Ball Milling and Powder Metallurgy.

    Science.gov (United States)

    Toozandehjani, Meysam; Matori, Khamirul Amin; Ostovan, Farhad; Abdul Aziz, Sidek; Mamat, Md Shuhazlly

    2017-10-26

    The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al₂O₃ (Al-5Al₂O₃) has been investigated. Al-5Al₂O₃ nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al₂O₃ nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD) analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness ( HV ), nano-hardness ( HN ), and Young's modulus ( E ) of Al-5Al₂O₃ nanocomposites. HV , HN , and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively.

  8. Nanograin formation in milled MoO3 powders

    International Nuclear Information System (INIS)

    Guerrero-Paz, J; Dorantes-Rosales, H; Aguilar-Martínez, J A; Garibay-Febles, V

    2013-01-01

    Powder of Molybdenum trioxide was milled for different times in horizontal ball mills. Such powder was characterized by TEM and XRD. Powder was rapidly de-agglomerated and fragmented up to attain nanoplates of two types, amorphous and crystalline. Finally, cold-welding of nanoplates occurred permitting some relaxation process to obtain a more stable energized structure consisting of equiaxial crystalline nanograins after 16 hours of milling.

  9. Investigation of physical properties and stability of indomethacin-cimetidine and naproxen-cimetidine co-amorphous systems prepared by quench cooling, coprecipitation and ball milling

    DEFF Research Database (Denmark)

    Lim, Ai Wei; Löbmann, Korbinian; Grohganz, Holger

    2016-01-01

    the samples. Structural relaxation (i.e. molecular mobility) behaviour was obtained from the Kohlrausch-Williams-Watts (KWW) relationship. KEY FINDINGS: A glass transition temperature (Tg ), on average 20 °C higher than the predicted Tg (calculated from the Fox equation), was observed in all samples....... The structural relaxation was dependent on the preparative methods. At a storage temperature of 40 °C, a comparatively higher molecular mobility was observed in indomethacin-cimetidine samples prepared by ball milling (ln τ(β) = 0.8), while similar molecular mobility was found for the same sample prepared...... by quench cooling (ln τ(β) = 2.4) and co-evaporation (ln τ(β) = 2.5). In contrast, molecular mobility of the naproxen-cimetidine samples followed the order co-evaporation (ln τ(β) = 0.8), quench cooling (ln τ(β) = 1.6) and ball milling (ln τ(β) = 1.8). CONCLUSION: The estimated relaxation times by the DSC...

  10. Pengaruh Lama Miling Terhadap Sifat Absorpsi Material Penyimpan Hidrogen MgH2 yang Dikatalisasi Dengan Fe (The Role of Milling Time on the Absorption Behaviour of MgH2 Catalyzed by Fe

    Directory of Open Access Journals (Sweden)

    Mustanir Mustanir

    2009-12-01

    Full Text Available Hidrida logam berbasis MgH2 dengan sisipan 1 wt% katalis Fe telah berhasil disintesis dengan teknik ball milling. Hasil proses miling selama 80 jam menunjukkan bahwa ukuran butir material telah membentuk struktur nanokristal. Hal ini ditunjukkan oleh profil difraksi sinar-X dimana terjadi pelebaran puncakpuncak difraksinya dengan meningkatnya waktu miling. Hasil uji absorpsi secara gravimetrik diketahui bahwa MgH2 berkatalis 1 wt% Fe mampu menyerap hydrogen sebesar 5,5 wt% dalam waktu ~20 menit pada temperatur 300 oC. Hasil ini sekaligus memperlihatkan bahwa sejumlah kecil katalis Fe bekerja secara baik dalam memperbaiki sifat absorpsi material penyimpan hydrogen berbasis Mg.(Metal hydrides are of great interest as hydrogen storage media especially for automotive application. Hydrides of magnesium and magnesium alloys are particularly attractive as they combine potentially high hydrogen storage capacities, 7.6 wt%. But, unfortunately, the sorption properties are poor. For example, conventional hydrogenation of magnesium requires prolonged treatment at temperatures of 300 oC and above. Here, we report the absorption properties of MgH2 catalyzed with a small amount of Fe element (1wt% under argon atmosphere prepared by ball milling in 80 hours. As the results, it showed the influence of milling time on the absortion kinetics of material which could absorp hydrogen in amount 5.5 within 20 minutes at 300 oC. It is obvious that longer milling time and small amount of catalyst could improve the sorption properties of Mg-based hydrides. © 2009 BCREC UNDIP. All rights reserved[Received: 13rd November 2009, Revised: 25th December 2009, Accepted: 31st December 2009][How to Cite: M. Mustanir, Z. Jalil. (2009. Pengaruh Lama Miling Terhadap Sifat Absorpsi Material Penyimpan Hidrogen MgH2 yang Dikatalisasi Dengan Fe (The Role of Milling Time on the Absorption Behaviour of MgH2 Catalyzed by Fe. Bulletin of Chemical Reaction Engineering and Catalysis, 4(2: 69

  11. Synthesis of Randomly Substituted Anionic Cyclodextrins in Ball Milling

    Directory of Open Access Journals (Sweden)

    László Jicsinszky

    2017-03-01

    Full Text Available A number of influencing factors mean that the random substitution of cyclodextrins (CD in solution is difficult to reproduce. Reaction assembly in mechanochemistry reduces the number of these factors. However, lack of water can improve the reaction outcomes by minimizing the reagent’s hydrolysis. High-energy ball milling is an efficient, green and simple method for one-step reactions and usually reduces degradation and byproduct formation. Anionic CD derivatives have successfully been synthesized in the solid state, using a planetary ball mill. Comparison with solution reactions, the solvent-free conditions strongly reduced the reagent hydrolysis and resulted in products of higher degree of substitution (DS with more homogeneous DS distribution. The synthesis of anionic CD derivatives can be effectively performed under mechanochemical activation without significant changes to the substitution pattern but the DS distributions were considerably different from the products of solution syntheses.

  12. Catalytically Enhanced Hydrogen Sorption in Mg-MgH2 by Coupling Vanadium-Based Catalyst and Carbon Nanotubes

    Directory of Open Access Journals (Sweden)

    Atikah Kadri

    2015-06-01

    Full Text Available Mg (MgH2-based composites, using carbon nanotubes (CNTs and pre-synthesized vanadium-based complex (VCat as the catalysts, were prepared by high-energy ball milling technique. The synergistic effect of coupling CNTs and VCat in MgH2 was observed for an ultra-fast absorption rate of 6.50 wt. % of hydrogen per minute and 6.50 wt. % of hydrogen release in 10 min at 200 °C and 300 °C, respectively. The temperature programmed desorption (TPD results reveal that coupling VCat and CNTs reduces both peak and onset temperatures by more than 60 °C and 114 °C, respectively. In addition, the presence of both VCat and CNTs reduces the enthalpy and entropy of desorption of about 7 kJ/mol H2 and 11 J/mol H2·K, respectively, as compared to those of the commercial MgH2, which ascribe to the decrease of desorption temperature. From the study of the effect of CNTs milling time, it is shown that partially destroyed CNTs (shorter milling time are better to enhance the hydrogen sorption performance.

  13. Synthesis of Ni3Ta, Ni2Ta and NiTa by high-energy ball milling and subsequent heat treatment

    International Nuclear Information System (INIS)

    Benites, H.S.N.; Silva, B.P da; Ramos, A.S.; Silva, A.A.A.P.; Coelho, G.C.; Lima, B.B. de

    2014-01-01

    The tantalum has relevance for the development of multicomponent Ni-based superalloys which are hardened by solid solution and precipitation mechanisms. Master alloys are normally used in the production step in order to produce refractory metals and alloys. The present work reports on the synthesis of Ni_3Ta, Ni_2Ta and NiTa by high-energy ball milling and subsequent heat treatment. The elemental Ni-25Ta, Ni-33Ta and Ni-50Ta (at.-%) powder mixtures were ball milled under Ar atmosphere using stainless steel balls and vials, 300 rpm and a ball-to-powder weight ratio of 10:1. Following, the as-milled samples were uniaxially compacted and heat-treated at 1100 deg C for 4h under Ar atmosphere. The characterization of as-milled and heat-treated samples was conducted by means of X-ray diffraction, scanning electron microscopy, and energy dispersive spectrometry. A large amount of Ni_3Ta, Ni_2Ta and NiTa was formed in the mechanically alloyed heat-treated Ni-25Ta, Ni-33Ta and Ni-50Ta alloys. (author)

  14. Removal of fluoride from drinking water using modified ultrafine tea powder processed using a ball-mill

    Energy Technology Data Exchange (ETDEWEB)

    Cai, Huimei; Xu, Lingyun; Chen, Guijie; Peng, Chuanyi [School of Tea & Food Science and Technology, Anhui Agricultural University/State Key Laboratory of Tea Plant Biology and Utilization, Anhui Agricultural University, Hefei 230036, Anhui (China); Ke, Fei [School of Tea & Food Science and Technology, Anhui Agricultural University/State Key Laboratory of Tea Plant Biology and Utilization, Anhui Agricultural University, Hefei 230036, Anhui (China); School of Science, Anhui Agricultural University, Hefei 230036 (China); Liu, Zhengquan; Li, Daxiang; Zhang, Zhengzhu [School of Tea & Food Science and Technology, Anhui Agricultural University/State Key Laboratory of Tea Plant Biology and Utilization, Anhui Agricultural University, Hefei 230036, Anhui (China); Wan, Xiaochun, E-mail: xcwan@ahau.edu.cn [School of Tea & Food Science and Technology, Anhui Agricultural University/State Key Laboratory of Tea Plant Biology and Utilization, Anhui Agricultural University, Hefei 230036, Anhui (China)

    2016-07-01

    Highlights: • Ultrafine tea powder (UTP) was prepared by ball-milling. • A novel and high efficient biosorbent from ultrafine tea powder (UTP) for the removal of fluoride from drinking water was prepared. • Loaded ultrafine tea powder adsorbed more fluoride adsorption than loaded tea waste. • UTP-Zr performed well over a considerably wide pH range, from 3.0 to 10.0. • UTP-Zr retains Zr metal ion during defluoridation, limiting secondary pollution. - Abstract: A low-cost and highly efficient biosorbent was prepared by loading zirconium(IV) onto ball-milled, ultrafine tea powder (UTP-Zr) for removal of fluoride from drinking water. To evaluate the fluoride adsorption capacity of UTP-Zr over a wide range of conditions, the biosorbent dosage, contact time, initial pH, initial fluoride concentration and presence of other ions were varied. UTP-Zr performed well over the considerably wide pH range of 3–10. The residual concentration of Zr in the treated water was below the limit of detection (0.01 mg/L). Fluoride adsorption by the UTP-Zr biosorbent followed the Langmuir model, with a maximum adsorption capacity of 12.43 mgF/g at room temperature. The fluoride adsorption kinetics fit the pseudo-second-order kinetic model. The synthesized biosorbent was characterized by BET, SEM, EDS, XRD and XPS to reveal how UTP-Zr interacts with fluoride. Results from this study demonstrated that UTP-based biosorbents will be useful and safe for the removal of fluoride from drinking water.

  15. Removal of fluoride from drinking water using modified ultrafine tea powder processed using a ball-mill

    International Nuclear Information System (INIS)

    Cai, Huimei; Xu, Lingyun; Chen, Guijie; Peng, Chuanyi; Ke, Fei; Liu, Zhengquan; Li, Daxiang; Zhang, Zhengzhu; Wan, Xiaochun

    2016-01-01

    Highlights: • Ultrafine tea powder (UTP) was prepared by ball-milling. • A novel and high efficient biosorbent from ultrafine tea powder (UTP) for the removal of fluoride from drinking water was prepared. • Loaded ultrafine tea powder adsorbed more fluoride adsorption than loaded tea waste. • UTP-Zr performed well over a considerably wide pH range, from 3.0 to 10.0. • UTP-Zr retains Zr metal ion during defluoridation, limiting secondary pollution. - Abstract: A low-cost and highly efficient biosorbent was prepared by loading zirconium(IV) onto ball-milled, ultrafine tea powder (UTP-Zr) for removal of fluoride from drinking water. To evaluate the fluoride adsorption capacity of UTP-Zr over a wide range of conditions, the biosorbent dosage, contact time, initial pH, initial fluoride concentration and presence of other ions were varied. UTP-Zr performed well over the considerably wide pH range of 3–10. The residual concentration of Zr in the treated water was below the limit of detection (0.01 mg/L). Fluoride adsorption by the UTP-Zr biosorbent followed the Langmuir model, with a maximum adsorption capacity of 12.43 mgF/g at room temperature. The fluoride adsorption kinetics fit the pseudo-second-order kinetic model. The synthesized biosorbent was characterized by BET, SEM, EDS, XRD and XPS to reveal how UTP-Zr interacts with fluoride. Results from this study demonstrated that UTP-based biosorbents will be useful and safe for the removal of fluoride from drinking water.

  16. THEORETICAL AND EXPERIMENTAL STUDIES OF ENERGY-EFFICIENT GRINDING PROCESS OF CEMENT CLINKER IN A BALL MILL

    Directory of Open Access Journals (Sweden)

    Kuznetsova M.M.

    2014-08-01

    Full Text Available The article presents results of theoretical and experimental research of grinding process of bulk materials in a ball mill. The new method of determination of energy efficiently mode of operation of ball mills in a process of a cement clinker grinding is proposed and experimentally tested.

  17. A study of the mechanism of microwave-assisted ball milling preparing ZnFe{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yingzhe; Wu, Yujiao [College of materials and metallurgical engineering, Guizhou Institute of Technology, Guiyang 550003 (China); 2011 Collaborative Innovation Center of Guizhou Province, Guiyang 550003 (China); Qin, Qingdong [College of materials and metallurgical engineering, Guizhou Institute of Technology, Guiyang 550003 (China); Wang, Fuchun [College of materials and metallurgical engineering, Guizhou Institute of Technology, Guiyang 550003 (China); 2011 Collaborative Innovation Center of Guizhou Province, Guiyang 550003 (China); Chen, Ding [College of Materials Science and Engineering, Hunan University, Changsha, Hunan 410082 (China)

    2016-07-01

    In this paper, well dispersed ZnFe{sub 2}O{sub 4} nano-particles with high magnetization saturation of 82.23 emu/g were first synthesized by microwave assisted ball milling and then the influences of pre-treatments and microwave powers to the progress were studied. It was found that under the both function of crack effect induced by ball milling and rotary motion induced by microwave the synthesized ferrtie nano-particles were well dispersed that is much different from the powders synthesized by normal high energy ball milling. The pre-treatment of ball milling can only enhance the reaction rate in the first several hours but the pre-irradiation of microwave can enhance the hole reaction rate. Further more, it was also been found that with increasing the microwave power, the more raw materials will converted into zinc ferrite in the first 5 h. 5 h latter the microwave power of 720 W is high enough for the coupling effect of microwave and ball milling with stirrer rotation speed of 256 rpm. - Highlights: • ZnFe{sub 2}O{sub 4} with 82.23 emu/g were synthesized without heat treatment. • The produced powder dispersed very well without any dispersant. • The pre-treatment of microwave enhanced the reaction rate much. • The pre-treatment of ball milling enhance chemical rate at beginning.

  18. Moessbauer effect study on mechanically alloyed amorphous Fe1-xTix alloys

    International Nuclear Information System (INIS)

    Chen Hong; Xu Zuxiong; Ma Ruzhang; Zhao Zhongtao; Ping Jueyun

    1994-01-01

    Amorphous Fe 1-x Ti x (x = 0.50, 0.60) powders were produced by mechanical alloying from pure elemental powders in a vibratory ball-mill. X-ray diffraction (XRD) and Moessbauer effect (ME) were used to study the progress of amorphization and the property of hydrogen absorption in Fe-Ti alloys. The amorphization process and the properties of the amorphous phase are discussed. (orig.)

  19. Effects of ball milling on microstructures and thermoelectric properties of higher manganese silicides

    International Nuclear Information System (INIS)

    Chen, Xi; Shi, Li; Zhou, Jianshi; Goodenough, John B.

    2015-01-01

    Highlights: • The already low κ L of HMS can be suppressed further by decreasing the grain size. • The ball milling process can lead to the formation of secondary MnSi and W/C-rich phases. • The formation of the MnSi ad W/C rich phases is found to suppress the thermoelectric power factor. - Abstract: Bulk nanostructured higher manganese silicide (HMS) samples with different grain size are prepared by melting, subsequent ball milling (BM), and followed by spark plasma sintering (SPS). The effects of BM time on the microstructures and thermoelectric properties of these samples are investigated. It is found that BM effectively reduces the grain size to about 90 nm in the sample after SPS, which leads to a decrease in both the thermal conductivity and electrical conductivity. By prolonging the BM time, MnSi and tungsten/carbon-rich impurity phases are formed due to the impact-induced decomposition of HMS and contamination from the tungsten carbide jar and balls during the BM, respectively. These impurities result in a reduced Seebeck coefficient and increased thermal conductivity above room temperature. The measured size-dependent lattice thermal conductivities agree qualitatively with the reported calculation results based on a combined phonon and diffuson model. The size effects are found to be increasingly significant as temperature decreases. Because of the formation of the impurity phases and a relatively large grain size, the ZT values are not improved in the ball-milled HMS samples. These findings suggest the need of alternative approaches for the synthesis of pure HMS with further reduced grain size and controlled impurity doping in order to enhance the thermoelectric figure-of-merit of HMS via nanostructuring

  20. Effects of milling method and calcination condition on phase and morphology characteristics of Mg4Nb2O9 powders

    International Nuclear Information System (INIS)

    Wongmaneerung, R.; Sarakonsri, T.; Yimnirun, R.; Ananta, S.

    2006-01-01

    Magnesium niobate, Mg 4 Nb 2 O 9 , powders has been synthesized by a solid-state reaction. Both conventional ball- and rapid vibro-milling have been investigated as milling methods, with the formation of the Mg 4 Nb 2 O 9 phase investigated as a function of calcination conditions by DTA and XRD. The particle size distribution of the calcined powders was determined by laser diffraction technique, while morphology, crystal structure and phase composition were determined via a combination of SEM, TEM and EDX techniques. The type of milling method together with the designed calcination condition was found to show a considerable effect on the phase and morphology evolution of the calcined Mg 4 Nb 2 O 9 powders. It is seen that optimization of calcination conditions can lead to a single-phase Mg 4 Nb 2 O 9 in both milling methods. However, the formation temperature and dwell time for single-phase Mg 4 Nb 2 O 9 powders were lower with the rapid vibro-milling technique

  1. One step conversion of wheat straw to sugars by simultaneous ball milling, mild acid, and fungus Penicillium simplicissimum treatment.

    Science.gov (United States)

    Yuan, Li; Chen, Zhenhua; Zhu, Yonghua; Liu, Xuanming; Liao, Hongdong; Chen, Ding

    2012-05-01

    Wheat straw is one of the major lignocellulosic plant residues in many countries including China. An attractive alternative is the utilization of wheat straw for bioethanol production. This article mainly studies a simple one-step wet milling with Penicillium simplicissimum and weak acid to hydrolysis of wheat straw. The optimal condition for hydrolysis was ball milling 48 h in citrate solvent (pH = 4) with P. simplicissimum H5 at the speed of 500 rpm and the yield of sugar increased with increased milling time. Corresponding structure transformations before and after milling analyzed by X-ray diffraction, transmission Fourier transform infrared spectroscopy, and environmental scanning electron microscopy clearly indicated that this combined treatment could be attributed to the crystalline and chemical structure changes of cellulose in wheat straw during ball milling. This combined treatment of ball milling, mild acid, and fungus hydrolysis enabled the conversion of the wheat straw. Compared with traditional method of ball milling, this work showed a more simple, novel, and environmentally friendly way in mechanochemical treatment of wheat straw.

  2. Sintered Fe-Ni-Cu-Sn-C Alloys Made of Ball-Milled Powders

    Directory of Open Access Journals (Sweden)

    Romański A.

    2014-10-01

    Full Text Available The main objective of this paper was to perform sinterability studies of ball-milled Fe-12%Ni-6.4%Cu-1.6%Sn-0.6%C powders. A mixture of precisely weighed amounts of elemental iron, nickel and graphite, and pre-alloyed 80/20 bronze powders was ball-milled for 8, 30 and 120 hours. After cold-pressing at 400 MPa the specimens were sintered at 900oC for 30 minutes in a reducing atmosphere and subsequently tested for density and hardness as well as subjected to structural studies using scanning electron microscopy (SEM and X-ray diffraction (XRD analysis.

  3. Fe-Al2O3 nanocomposites prepared by high-energy ball milling

    DEFF Research Database (Denmark)

    Linderoth, Søren; Pedersen, M.S.

    1994-01-01

    Nanocomposites of alpha-Fe and alpha-Al2O3, prepared by high-energy ball milling, exhibit coercivities which are enhanced by about two orders of magnitude with respect to the bulk value. The degree of enhancement depends on the volume fraction (x(upsilon)) of Fe, with a maximum for x(upsilon) alm......Nanocomposites of alpha-Fe and alpha-Al2O3, prepared by high-energy ball milling, exhibit coercivities which are enhanced by about two orders of magnitude with respect to the bulk value. The degree of enhancement depends on the volume fraction (x(upsilon)) of Fe, with a maximum for x...

  4. Preparation of high crystalline nanoparticles of rare-earth based complex pervoskites and comparison of their structural and magnetic properties with bulk counterparts

    DEFF Research Database (Denmark)

    Basith, M. A.; Islam, M. A.; Ahmmad, Bashir

    2017-01-01

    of crystalline and amorphous phases. FESEM images demonstrate the formation of nanoparticles with average particle size in the range of 50–100 nm for both ultrasonication and 4 h (h) of ball milling. The bulk materials and nanoparticles synthesized by both ultrasonication and 4 h ball milling exhibit...... of the nanoparticles due to ball milling particularly for milling time exceeding 8 h. This investigation demonstrates the potential of ultrasonication as a simple route to prepare high crystalline rare-earth based manganite nanoparticles with improved control compared to the traditional ball milling technique....

  5. Synthesis of Ni-YSZ cermet for an electrode of high temperature electrolysis by high energy ball milling

    International Nuclear Information System (INIS)

    Hong, H.S.; Chae, U.S.; Park, K.M.; Choo, S.T.

    2005-01-01

    Ni/YSZ composites for a cathode that can be used in high temperature electrolysis were prepared by ball milling of Ni and YSZ powder. Ball milling was performed in a dry process and in ethanol. The microstructure and electrical conductivity of the composites were examined by XRD, SEM, TEM and a 4-point probe. XRD patterns for both the dry and wet ball-milled powders showed that the composites were composed of crystalline Ni and YSZ particles. The patterns did not change with increases in the milling time up to 48 h. Dry-milling slightly increased the average particle size compared to starting Ni particles, but little change in the particle size was observed with the increase in milling time. On the other hand, the wet-milling reduced the average size and the increasing milling time induced a further decrease in the particle size. After cold-pressing and annealing at 900 C for 2 h, the dry-milled powder exhibited high stability against Ni sintering so that the particle size changed little, but the particle size increased in the wet-milled powder. The electrical conductivity increased after sintering at 900 C. Particles from the dry and wet process became denser and contacted closer after sintering, providing better electron migration paths. (orig.)

  6. A combination method of the theory and experiment in determination of cutting force coefficients in ball-end mill processes

    Directory of Open Access Journals (Sweden)

    Yung-Chou Kao

    2015-10-01

    Full Text Available In this paper, the cutting force calculation of ball-end mill processing was modeled mathematically. All derivations of cutting forces were directly based on the tangential, radial, and axial cutting force components. In the developed mathematical model of cutting forces, the relationship of average cutting force and the feed per flute was characterized as a linear function. The cutting force coefficient model was formulated by a function of average cutting force and other parameters such as cutter geometry, cutting conditions, and so on. An experimental method was proposed based on the stable milling condition to estimate the cutting force coefficients for ball-end mill. This method could be applied for each pair of tool and workpiece. The developed cutting force model has been successfully verified experimentally with very promising results.

  7. Optimum condition determination of Rirang uranium ores grinding using ball mill

    International Nuclear Information System (INIS)

    Affandi, Kosim; Waluyo, Sugeng; Sarono, Budi; Sujono; Muhammad

    2002-01-01

    The grinding experiment on Rirang Uranium ore has been carried out with the aim is to find out the optimum condition of wet grinding using ball mill to produce particle size -325, -200 and -100 mesh. This will be used for decomposition feed the test was done by examine the parameters comparison of ore's weight against ball's weight and time of grinding. The test shown that the product of particle size -325 meshes was achieved optimum condition at the comparison ore's weight: ball = 1:3, grinding time 150 minutes, % solid 60, speed rotation of ball mill 60 rpm and recovery of grinding was 93.51 % of -325 mesh. The product of particle size -200 mesh was achieved optimum condition at comparison ore's weight: ball = 1:2, time of grinding 60 minutes, the fraction of + 200 mesh was regrind, the recovery of grinding 6.82% at particle size of (-200 + 250) mesh, 5.75 % at (-250 + 325)m mesh and, 47.93 % -325 mesh. The product of particle size -100 mesh was achieved the optimum condition at comparison ore's weight: ball = 1:2, time of grinding at 30 minutes particle size +100 mesh regrinding using mortar grinder, recovery of grinding 30.10% at particle size (-100 + 150) m, 12.28 % at (-150 + 200) mesh, 15.92 % at (-200 + 250) mesh, 12.44 % at (-250 + 325) mesh and 29.26 % -325 mesh. The determination of specific gravity of Rirang uranium ore was between 4.15 - 4.55 g/cm 3

  8. Effects of ball milling on microstructures and thermoelectric properties of higher manganese silicides

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xi [Materials Science and Engineering Program, Texas Materials Institute, The University of Texas at Austin, Austin, TX 78712 (United States); Shi, Li, E-mail: lishi@mail.utexas.edu [Materials Science and Engineering Program, Texas Materials Institute, The University of Texas at Austin, Austin, TX 78712 (United States); Department of Mechanical Engineering, The University of Texas at Austin, Austin, TX 78712 (United States); Zhou, Jianshi; Goodenough, John B. [Materials Science and Engineering Program, Texas Materials Institute, The University of Texas at Austin, Austin, TX 78712 (United States); Department of Mechanical Engineering, The University of Texas at Austin, Austin, TX 78712 (United States)

    2015-08-25

    Highlights: • The already low κ{sub L} of HMS can be suppressed further by decreasing the grain size. • The ball milling process can lead to the formation of secondary MnSi and W/C-rich phases. • The formation of the MnSi ad W/C rich phases is found to suppress the thermoelectric power factor. - Abstract: Bulk nanostructured higher manganese silicide (HMS) samples with different grain size are prepared by melting, subsequent ball milling (BM), and followed by spark plasma sintering (SPS). The effects of BM time on the microstructures and thermoelectric properties of these samples are investigated. It is found that BM effectively reduces the grain size to about 90 nm in the sample after SPS, which leads to a decrease in both the thermal conductivity and electrical conductivity. By prolonging the BM time, MnSi and tungsten/carbon-rich impurity phases are formed due to the impact-induced decomposition of HMS and contamination from the tungsten carbide jar and balls during the BM, respectively. These impurities result in a reduced Seebeck coefficient and increased thermal conductivity above room temperature. The measured size-dependent lattice thermal conductivities agree qualitatively with the reported calculation results based on a combined phonon and diffuson model. The size effects are found to be increasingly significant as temperature decreases. Because of the formation of the impurity phases and a relatively large grain size, the ZT values are not improved in the ball-milled HMS samples. These findings suggest the need of alternative approaches for the synthesis of pure HMS with further reduced grain size and controlled impurity doping in order to enhance the thermoelectric figure-of-merit of HMS via nanostructuring.

  9. Microstructural evolution of nanostructured Ti0.9Al0.1N prepared by reactive ball-milling

    International Nuclear Information System (INIS)

    Bhaskar, U.K.; Bid, S.; Pradhan, S.K.

    2011-01-01

    Research highlights: → Nanocrystalline stoichiometric Ti 0.9 Al 0.1 N powder has been prepared by ball-milling the 0.9 mol fraction of α-Ti (hcp) and 0.1 mol fraction of aluminum (fcc) powders under N 2 at room temperature. Initially, α-Ti phase partially transformed to the transient β-Ti phase and Ti 0.9 Al 0.1 N (fcc) phase is noticed to form after 3 h of milling. Nanocrystalline stoichiometric Ti 0.9 Al 0.1 N phase is formed after 7 h of milling. The main features which are observed in the present study are stated below: 1.During ball-milling of α-Ti, the α-Ti phase partially converted to transient cubic β-Ti phase within 1 h of milling. 2.Ti 0.9 Al 0.1 N (fcc) phase is noticed to form after 3 h of milling. Complete formation of Ti 0.9 Al 0.1 N (fcc) is obtained at 7 h of milling which is lesser than complete formation time (9 h) of TiN. Doping Al atoms accelerates the formation of (TiAl)N phase. 3.The particle size of Ti 0.9 Al 0.1 N decrease rapidly up to 3 h and then increase slightly due to agglomeration effect. 4.The particle size of Ti 0.9 Al 0.1 N estimated from X-ray is in good agreement with that measured from HRTEM. - Abstract: Nanocrystalline stoichiometric Ti 0.9 Al 0.1 N powder has been prepared by ball-milling the α-Ti (hcp) and aluminum (fcc) powders under N 2 at room temperature. Initially, α-Ti phase partially transformed to the transient cubic β-Ti phase and Ti 0.9 Al 0.1 N (fcc) phase is noticed to form after 3 h of milling. Nanocrystalline stoichiometric Ti 0.9 Al 0.1 N phase is formed after 7 h of milling. After 1 h of milling, all Al atoms are diffused into the α-Ti matrix. The transient β-Ti phase is noticed to form after 1 h of milling and disappears completely after 7 h of milling. Microstructure characterization of unmilled and ball-milled powders by analyzing XRD patterns employing the Rietveld structure refinement reveals the inclusion of Al and nitrogen atoms into the Ti lattice on the way to formation of Ti 0.9 Al 0.1 N

  10. Effect of amorphous lamella on the crack propagation behavior of crystalline Mg/amorphous Mg-Al nanocomposites

    Science.gov (United States)

    Hai-Yang, Song; Yu-Long, Li

    2016-02-01

    The effects of amorphous lamella on the crack propagation behavior in crystalline/amorphous (C/A) Mg/Mg-Al nanocomposites under tensile loading are investigated using the molecular dynamics simulation method. The sample with an initial crack of orientation [0001] is considered here. For the nano-monocrystal Mg, the crack growth exhibits brittle cleavage. However, for the C/A Mg/Mg-Al nanocomposites, the ‘double hump’ behavior can be observed in all the stress-strain curves regardless of the amorphous lamella thickness. The results indicate that the amorphous lamella plays a critical role in the crack deformation, and it can effectively resist the crack propagation. The above mentioned crack deformation behaviors are also disclosed and analyzed in the present work. The results here provide a strategy for designing the high-performance hexagonal-close-packed metal and alloy materials. Project supported by the National Natural Science Foundation of China (Grant Nos. 11372256 and 11572259), the 111 Project (Grant No. B07050), the Program for New Century Excellent Talents in University of Ministry of Education of China (Grant No. NCET-12-1046), and the Program for New Scientific and Technological Star of Shaanxi Province, China (Grant No. 2012KJXX-39).

  11. Design and Testing of UMM Vertical Ball Mill (UVBM) for producing Aluminium Powder

    Science.gov (United States)

    Aisyah, I. S.; Caesarendra, Wahyu; Suprihanto, Agus

    2018-04-01

    UMM Vertical Ball Mill (UVBM) was intended to be the apparatus to produce metal powder with superior characteristic in production rate while retaining good quality of metal powder. The concept of design was adopting design theory of Phal and Beitz with emphasis on increasing of probability of success in engineering and economy aspects.Since it was designed as vertical ball mill, a new way to produce powder, then it need to be tested for the performance after manufactured. The test on UVBM was carried out by milling of aluminium chip for 5 (five) different milling time of 0.5 hours, 1 hour, 3 hours, 5 hours and 7 hours, and the powder product then be characterized for it morphology and size using Scanning Electron Microscope (SEM) and Sieve.The results of the study were the longer of the milling time, the finer of the powder. From the test results of SEM, the morphology of the powder with 5 variations of milling time were most of the powder in form of flake (flat), small round and angular (irregular). The distribution of powder size was best obtained on the variation of milling time 3 hours, 5 hours, and 7 hours with percentage of 200 mesh in size of 22.14 %, 64 % and 91.25 % respectively.

  12. Contamination risk of stable isotope samples during milling.

    Science.gov (United States)

    Isaac-Renton, M; Schneider, L; Treydte, K

    2016-07-15

    Isotope analysis of wood is an important tool in dendrochronology and ecophysiology. Prior to mass spectrometry analysis, wood must be homogenized, and a convenient method involves a ball mill capable of milling samples directly in sample tubes. However, sample-tube plastic can contaminate wood during milling, which could lead to biological misinterpretations. We tested possible contamination of whole wood and cellulose samples during ball-mill homogenization for carbon and oxygen isotope measurements. We used a multi-factorial design with two/three steel milling balls, two sample amounts (10 mg, 40 mg), and two milling times (5 min, 10 min). We further analyzed abrasion by milling empty tubes, and measured the isotope ratios of pure contaminants. A strong risk exists for carbon isotope bias through plastic contamination: the δ(13) C value of polypropylene deviated from the control by -6.77‰. Small fibers from PTFE filter bags used during cellulose extraction also present a risk as the δ(13) C value of this plastic deviated by -5.02‰. Low sample amounts (10 mg) showed highest contamination due to increased abrasion during milling (-1.34‰), which is further concentrated by cellulose extraction (-3.38‰). Oxygen isotope measurements were unaffected. A ball mill can be used to homogenize samples within test tubes prior to oxygen isotope analysis, but not prior to carbon or radiocarbon isotope analysis. There is still a need for a fast, simple and contamination-free sample preparation procedure. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  13. Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al2O3 Nanocomposite Synthesized by Ball Milling and Powder Metallurgy

    Science.gov (United States)

    Matori, Khamirul Amin; Ostovan, Farhad; Abdul Aziz, Sidek; Mamat, Md Shuhazlly

    2017-01-01

    The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al2O3 (Al-5Al2O3) has been investigated. Al-5Al2O3 nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al2O3 nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD) analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness (HV), nano-hardness (HN), and Young’s modulus (E) of Al-5Al2O3 nanocomposites. HV, HN, and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively. PMID:29072632

  14. Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al2O3 Nanocomposite Synthesized by Ball Milling and Powder Metallurgy

    Directory of Open Access Journals (Sweden)

    Meysam Toozandehjani

    2017-10-01

    Full Text Available The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al2O3 (Al-5Al2O3 has been investigated. Al-5Al2O3 nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al2O3 nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness (HV, nano-hardness (HN, and Young’s modulus (E of Al-5Al2O3 nanocomposites. HV, HN, and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively.

  15. Synthesis of free standing nanocrystalline Cu by ball milling at cryogenic temperature

    Energy Technology Data Exchange (ETDEWEB)

    Barai, K. [Department of Metallurgy and Materials Engineering, Bengal Engineering College, Shibpur, Howrah 711103 (India); Tiwary, C.S. [Department of Materials Engineering, Indian Institute of Science, Bangalore 560012 (India); Chattopadhyay, P.P. [Department of Metallurgy and Materials Engineering, Bengal Engineering College, Shibpur, Howrah 711103 (India); Chattopadhyay, K., E-mail: kamanio@materials.iisc.ernet.in [Department of Materials Engineering, Indian Institute of Science, Bangalore 560012 (India)

    2012-12-15

    This paper reports for the first time synthesis of free standing nano-crystalline copper crystals of a {approx}30-40 nm by ball milling of copper powder at 150 K under Argon atmosphere in a specially designed cryomill. The detailed characterization of these particles using multiple techniques that includes transmission electron microscopy confirms our conclusion. Careful analysis of the chemistry of these particles indicates that these particles are essentially contamination free. Through the analysis of existing models of grain size refinements during ball milling and low temperature deformation, we argue that the suppression of thermal processes and low temperature leads to formation of free nanoparticles as the process of fracture dominates over possible cold welding at low temperatures.

  16. Production of pyrite nanoparticles using high energy planetary ball milling for sonocatalytic degradation of sulfasalazine.

    Science.gov (United States)

    Khataee, Alireza; Fathinia, Siavash; Fathinia, Mehrangiz

    2017-01-01

    Sonocatalytic performance of pyrite nanoparticles was evaluated by the degradation of sulfasalazine (SSZ). Pyrite nanoparticles were produced via a high energy mechanical ball milling (MBM) in different processing time from 2h to 6h, in the constant milling speed of 320rpm. X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy (FT-IR) analysis and Brunauer-Emmett-Teller (BET) confirmed the production of pyrite nanoparticles during 6h of ball milling with the average size distribution of 20-80nm. The effects of various operational parameters including pH value, catalyst amount (mg/L), SSZ concentration (mg/L), ultrasonic frequency (kHz) and reaction time on the SSZ removal efficiency were examined. The obtained results showed that the maximum removal efficiency of 97.00% was obtained at pH value of 4, catalyst dosage of 0.5g/L, SSZ concentration of 10mg/L and reaction time of 30min. Experimental results demonstrated that the kinetic of the degradation process can be demonstrated using Langmuir-Hinshelwood (L-H) kinetic model. The effect of different inorganic ions such as Cl - , CO 3 2- and SO 4 2- was investigated on the L-H reaction rate (k r ) and adsorption (K s ) constants. Results showed that the presence of the mentioned ions significantly influenced the L-H constants. The impact of ethanol as a OH radical scavenger and some enhancers including H 2 O 2 and K 2 S 2 O 8 was investigated on the SSZ removal efficiency. Accordingly, the presence of ethanol suppressed SSZ degradation due to the quenching of OH radicals and the addition of K 2 S 2 O 8 and H 2 O 2 increased the SSZ removal efficiency, due to the formation of SO 4 - and additional OH radicals, respectively. Under the identical conditions of operating parameters, pyrite nanoparticles maintained their catalytic activity during four consecutive runs. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Effect of expansion temperature of expandable graphite on microstructure evolution of expanded graphite during high-energy ball-milling

    International Nuclear Information System (INIS)

    Yue Xueqing; Li Liang; Zhang Ruijun; Zhang Fucheng

    2009-01-01

    Two expanded graphites (EG), marked as EG-1 and EG-2, were prepared by rapid heating of expandable graphite to 600 and 1000 deg. C, respectively, and ball milled in a high-energy mill (planetary-type) under air atmosphere. The microstructure evolution of the ball-milled samples was characterized by X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). XRD analysis shows that the evolution degree of the average crystallite thickness along the c-axis (L c ) of EG-2 is lower than that of EG-1 during the milling process. From the HRTEM images of the samples after 100 h ball-milling, slightly curved graphene planes can be frequently observed both in the two EGs, however, EG-1 and EG-2 exhibit sharply curved graphene planes and smoothly curved graphene planes with high bending angles, respectively.

  18. Heterogeneous sono-Fenton-like process using martite nanocatalyst prepared by high energy planetary ball milling for treatment of a textile dye.

    Science.gov (United States)

    Dindarsafa, Mahsa; Khataee, Alireza; Kaymak, Baris; Vahid, Behrouz; Karimi, Atefeh; Rahmani, Amir

    2017-01-01

    High energy planetary ball milling was applied to prepare sono-Fenton nanocatalyst from natural martite (NM). The NM samples were milled for 2-6h at the speed of 320rpm for production of various ball milled martite (BMM) samples. The catalytic performance of the BMMs was greater than the NM for treatment of Acid Blue 92 (AB92) in heterogeneous sono-Fenton-like process. The NM and the BMM samples were characterized by XRD, FT-IR, SEM, EDX and BET analyses. The particle size distribution of the 6h-milled martite (BMM 3 ) was in the range of 10-90nm, which had the highest surface area compared to the other samples. Then, the impact of main operational parameters was investigated on the process. Complete removal of the dye was obtained at the desired conditions including initial pH 7, 2.5g/L BMM 3 dosage, 10mg/L AB92 concentration, and 150W ultrasonic power after 30min of treatment. The treatment process followed pseudo-first order kinetic. Environmentally-friendly modification of the NM, low leached iron amount and repeated application at milder pH were the significant benefits of the BMM 3 . The GC-MS was successfully used to identify the generated intermediates. Eventually, an artificial neural network (ANN) was applied to predict the AB92 removal efficiency based upon the experimental data with a proper correlation coefficient (R 2 =0.9836). Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Magnetic properties of nanocrystalline Fe–10%Ni alloy obtained by planetary ball mills

    International Nuclear Information System (INIS)

    Hamzaoui, Rabah; Elkedim, Omar

    2013-01-01

    Highlights: •Solid solution formation accompanied by a grain refinement for nanocrystalline Fe-Ni. •The shock mode process (SMP) prevails when Ω > >ω. •The friction mode process (FMP) is stronger when Ω < <ω. •The FMP leads to the formation of alloys exhibiting a soft magnetic behavior. -- Abstract: Planetary ball mill PM 400 from Retsch (with different milling times for Ω = 400 rpm, ω = 800 rpm) and P4 vario ball mill from Fritsch (with different milling conditions (Ω/ω), Ω and ω being the disc and the vial rotation speeds, respectively) are used for obtaining nanocrystalline Fe–10wt% Ni. The structure and magnetic properties are studied by using X-ray diffraction, SEM and hysteresis measurements, respectively. The bcc-Fe(Ni) phase formation is identified by X-ray diffraction. The higher the shock power and the higher milling time are, the larger the bcc lattice parameter and the lower the grain size. The highest value of the coercivity is 1600 A/m for Fe–10 wt.%Ni (with shock mode (424 rpm/100 rpm) after 36 h of milling), while the lowest value is 189 A/m for (400 rpm/800 rpm) after 72 h of milling. The milling performed in the friction mode has been found to lead the formation of alloys exhibiting a soft magnetic behavior for nanocrystalline Fe–10%Ni

  20. Long-Term Effects on Graphene Supercapacitors of Using a Zirconia Bowl and Zirconia Balls for Ball-Mill mixing of Active Materials

    Science.gov (United States)

    Song, Dae-Hoon; Kim, Jin-Young; Kahng, Yung Ho; Cho, Hoonsung; Kim, Eung-Sam

    2018-04-01

    Improving the energy storage performance of supercapacitor electrodes based on reduced graphene oxide (RGO) is one of the main subjects in this research field. However, when a zirconia bowl and zirconia balls were used for ball-mill mixing of the active materials for RGO supercapacitors, the energy storage performance deteriorated over time. Our study revealed that the source of the problem was the inclusion of zirconia bits from abrasion of the bowl and the balls during the ballmill mixing, which increased during a period of 1 year. We probed two solutions to this problem: 1) hydrofluoric (HF) acid treatment of the RGO supercapacitors and 2) use of a tempered steel bowl and tempered steel balls for the mixing. For both cases, the energy storage performance was restored to near the initial level, showing a specific capacitance ( C sp ) of 200 F/g. Our results should lead to progress in research on RGO supercapacitors.

  1. Synthesis and characterization of Mg-based amorphous alloys and their use for decolorization of Azo dyes

    International Nuclear Information System (INIS)

    Iqbal, M; Wang, W H

    2014-01-01

    Mg-based alloys are light weight and have wide range of applications in the automotive industry. These alloys are widely used because of their very attractive physical and mechanical properties and corrosion resistance. The properties and applications can be further improved by changing the nature of materials from crystalline to amorphous. In this study, melt spun ribbons (MSRs) of Mg 70 Zn 25 Ca 5 Mg 68 Zn 27 Ca 5 alloys were prepared by melt spinning technique by using 3-4N pure metals. Characterization of the samples was done by X-ray diffraction (XRD), differential scanning calorimetry (DSC) and energy dispersive x-ray analyzer (EDAX). Microstructural investigations were conducted by using scanning electron microscopy (SEM), atomic force microscopy (AFM) as well as optical and stereo scan microscopy techniques. DSC results showed multistage crystallization. Activation energy was found to be 225 kJ/mol by Kissinger method indicating good thermal stability against crystallization. XRD, DSC, SEM and EDS (energy dispersive spectroscopy) results are agreed very well. In order to study decolorization, the MSRs of Mg 70 Zn 25 Ca 5 Mg 68 Zn 27 Ca 5 alloys were treated repeatedly with various azo dyes at room temperature. In order to compare the results, MSRs of amorphous Zr- and Ni-based metallic glasses were also treated. Reaction of MSRs with azo dyes results in their decolorization in a few hours. Decolorization of azo dyes takes place by introducing amorphous MSRs which results in breaking the -N=N- bonds that exist in dye contents. It is concluded that Mg-based alloys are useful for paint and dye industries and will be beneficial to control water pollution. Comparison of results showed that Mg-based alloys are more efficient than Zr- and Ni-based amorphous alloys for decolorization of azo dyes

  2. Crystalline-to-amorphous phase transformation in mechanically alloyed Fe50W50 powders

    International Nuclear Information System (INIS)

    Sherif El-Eskandarany, M.S.; Sumiyama, K.; Suzuki, K.

    1997-01-01

    A mechanical alloying process via a ball milling technique has been applied for preparing amorphous Fe 50 W 50 alloy powders. The results have shown that during the first and second stages of milling (0 to 360 ks) W atoms emigrate to Fe lattices to form nanocrystalline b.c.c. Fe-W solid solution, with a grain size of about 7 nm in diameter. After 720 ks of the milling time, this solid solution was transformed to an amorphous Fe-W alloy coexisting with the residual fraction of the unprocessed W powders. During the last stage of milling (720 to 1,440 ks) all of this residual W powder reacts with the amorphous phase to form a homogeneous Fe 50 W 50 amorphous alloy. The crystallization temperature and the enthalpy change of crystallization of amorphous Fe 50 W 50 powders milled for 1,440 ks were measured to be 860 K and -9kJ/mol, respectively. The amorphous Fe 50 W 50 powder produced is almost paramagnetic at room temperature. The powder comprises homogeneous and smooth spheres with an average size of about 0.5 microm in diameter

  3. Excess lithium storage in LiFePO4-Carbon interface by ball-milling

    Science.gov (United States)

    Guo, Hua; Song, Xiaohe; Zheng, Jiaxin; Pan, Feng

    2016-07-01

    As one of the most popular cathode materials for high power lithium ion batteries (LIBs) of the electrical-vehicle (EV), lithium iron phosphate (LiFePO4 (LFP)) is limited to its relatively lower theoretical specific capacity of 170mAh g-1. To break the limits and further improve the capacity of LFP is promising but challenging. In this study, the ball-milling method is applied to the mixture of LFP and carbon, and the effective capacity larger than the theoretical one by 30mAh g-1 is achieved. It is demonstrated that ball-milling leads to the LFP-Carbon interface to store the excess Li-ions.

  4. Structural Relaxations and Thermodynamic Properties of Molecular Amorphous Solids by Mechanical Milling

    Science.gov (United States)

    Tsukushi, I.; Yamamuro, O.; Matsuo, T.

    The organic crystals of tri-O-methyl-β-cyclodextrin (TMCD) and its three clathrate compounds containing benzoic acid (BA), p-nitrobenzoic acid (NBA) and p-hydroxybenzoic acid (HBA), sucrose (SUC), salicin (SAL), phenolphthalein (PP), 1,3,5-tri-α-naphthylbenzene (TNB) were amorphized by milling with a vibrating mill for 2 ˜ 16 hours at room temperature. The amorphization was checked by differential scanning calorimetry (DSC) and X-ray powder diffraction. The heat capacities of crystals, liquid quenched glasses (LQG), and mechanically-milled amorphous solid (MMAS) of TMCD and TNB were measured with an adiabatic calorimeter in the temperature range between 12 and 375 K. For both compounds, the enthalpy relaxation of MMAS appeared in the wide temperature range below Tg and the released configurational enthalpy was much larger than that of LQG, indicating that MMAS is more disordered and strained than LQG.

  5. ZnO nanoparticles obtained by ball milling technique: Structural, micro-structure, optical and photo-catalytic properties

    Energy Technology Data Exchange (ETDEWEB)

    Balamurugan, S., E-mail: scandium.chemistry@gmail.com; Joy, Josny; Godwin, M. Anto; Selvamani, S.; Raja, T. S. Gokul [Advanced Nanomaterials Research Laboratory, Department of Nanotechnology, Noorul Islam Centre for Higher Education, Thuckalay, Kumaracoil - 629 180 (India)

    2016-05-23

    The ZnO nanoparticles were obtained by ball milling of commercial grade ZnO powder at 250 rpm for 20 h and studied their structural, micro-structure, optical and photo-catalytic properties. Due to ball milling significant decrease in lattice parameters and average crystalline size is noticed for the as-milled ZnO nano powder. The HRSEM images of the as-milled powder consist of agglomerated fine spherical nanoparticles in the range of ~10-20 nm. The room temperature PL spectrum of as-milled ZnO nano powder excited under 320 nm reveals two emission bands at ~406 nm (violet emission) and ~639 nm (green emission). Interestingly about 98 % of photo degradation of methylene (MB) by the ZnO catalyst is achieved at 100 minutes of solar light irradiation.

  6. Polycrystalline Nd2Fe14B/α-Fe nanocomposite flakes with a sub-micro/nanometre thickness prepared by surfactant-assisted high-energy ball milling

    International Nuclear Information System (INIS)

    Tang, Xin; Chen, Xi; Chen, Renjie; Yan, Aru

    2015-01-01

    Highlights: • Nd 2 Fe 14 B/α-Fe flakes are formed by peeling along preferential planes. • (0 0 l) planes are found to be preferential cleavage planes. • Magnetic properties degrade with increasing ball milling time. • Anisotropic nanocomposite magnets are fabricated. - Abstract: A surfactant-assisted high-energy ball milling technique was employed to synthesize Nd 2 Fe 14 B/α-Fe nanoparticles and nanoflakes from melt-spun nanocrystalline powders. The microstructure evolution in ball milling process was investigated. In the beginning stage (0–4 h) of ball milling, raw powders were crushed into micrometre-sized particles. While flakes were mainly formed by reducing thickness of particles via peeling layer by layer along preferential planes in the late stage (8–16 h). The selected area electron diffraction and high-resolution transmission electron microscopy images show that preferential cleavage planes are basal planes. With ball milling proceeding, more and more defects were induced by ball milling. As a result, the coercivity and remanence decreased to 1.6 kOe and 3.2 kGs, respectively. After 16 h ball milling, the exchange decoupling occurred due to severe amorphorization. A weakly-textured nanocomposite magnet was fabricated after 12 h ball milling and the anisotropy in magnetic properties can be further improved by employing settling down process to select particle size and aligning particles in external field

  7. Nitrogen-doped graphene by ball-milling graphite with melamine for energy conversion and storage

    International Nuclear Information System (INIS)

    Xue, Yuhua; Chen, Hao; Qu, Jia; Dai, Liming

    2015-01-01

    N-doped graphene was prepared by ball milling of graphite with melamine. It was found that ball-milling reduced the size of graphite particles from 30 to 1 μm and facilitated the exfoliation of the resultant small particles into few-layer N-doped graphene nanosheets under ultrasonication. The as-prepared N-doped graphene nanoplatelets (NGnPs) exhibited a nitrogen content as high as 11.4 at.%, making them attractive as efficient electrode materials in supercapacitors for energy storage and as highly-active metal-free catalysts for oxygen reduction in fuel cells for energy conversion. (paper)

  8. Reactive-inspired ball-milling synthesis of an ODS steel: study of the influence of ball-milling and annealing; Synthese et caracterisation d'un acier ODS prepare par un procede inspiredu broyage reactif: etude de l'influence des conditions de broyage et recuit

    Energy Technology Data Exchange (ETDEWEB)

    Brocq, M.

    2010-10-15

    In the context of the development of new ODS (Oxide Dispersion Strengthened) steels as core materials in future nuclear reactors, we investigated a new process inspired by reactive ball-milling which consists in using YFe{sub 3} andFe{sub 2}O{sub 3} as starting reactants instead of Y{sub 2}O{sub 3} to produce a dispersion of nano-oxides in a steel matrix and the influence of synthesis conditions on the nano-oxide characteristics were studied. For that aim, ODS steels were prepared by ball-milling and then annealed. Multi-scale characterizations were performed after each synthesis step, using notably atom probe tomography and small angle neutron scattering. The process inspired by reactive ball-milling was shown to be efficient for ODS steel synthesis, but it does not modify the nano-oxide characteristics as compared to those of oxides directly incorporated in the matrix by ball-milling. Broadly speaking, the nature of the starting oxygen bearing reactants has no influence on nano-oxide formation. Moreover, we showed that the nucleation of nano-oxides nucleation can start during milling and continues during annealing with a very fast kinetic. The final characteristics of nano-oxides formed in this way can be monitored through ball-milling parameters (intensity, temperature and atmosphere) and annealing parameters (duration and temperature). (author)

  9. Synthesis, thermal properties and recrystallization of ball-milled high Tc superconductors. (Topological stabilization of metastable phases)

    International Nuclear Information System (INIS)

    Schulz, R.; Lanteigne, J.; Simoneau, M.; Tessier, P.; Neste, A. van; Strom Olsen, J.O.

    1995-01-01

    Amorphous and nanocrystalline phases have been formed by ball-milling Y-Ba-Cu-O and Bi-Ca-Sr-Cu-O. The strong mechanical deformations induce disorder on the oxygen sublattice and on the cation sites. These order-disorder transformations often produce simple cubic perovskite structures. During recrystallization, the chemical order is restored. Small ordered regions nucleate, grow and produce particular metastable configurations which minimize the total elastic strain energy. The sequence of events giving rise to the various metastable phases has been followed by x-ray diffraction and differential scanning calorimetry and is explained in terms of free energy diagrams. The stress and strain fields associated with the Y-Ba disorder are calculated using the elastic properties of the Y-Ba-Cu-O superconductor. A simple model is proposed to explain the stability of the structures observed after thermal treatments. (orig.)

  10. Unravelling the relationship between degree of disorder and the dissolution behavior of milled glibenclamide

    DEFF Research Database (Denmark)

    Mah, Pei T; Laaksonen, Timo; Rades, Thomas

    2014-01-01

    Milling is an attractive method to prepare amorphous formulations as it does not require the use of solvents and is suitable for thermolabile drugs. One of the key critical quality attributes of milled amorphous formulations is their dissolution behavior. However, there are limited studies...... that have investigated the relationship between degree of disorder induced by milling and dissolution behavior. The main aim of this study was to identify the analytical technique used to characterize degree of disorder that correlates best with the recrystallization behavior during dissolution of milled...... glibenclamide samples. Solid state and surface changes during dissolution of milled glibenclamide samples were monitored in order to elucidate the processes that influence the dissolution behavior of milled glibenclamide samples. Glibenclamide was ball milled for different durations and analyzed using X...

  11. Microstructure and Mechanical Behavior of Microwave Sintered Cu50Ti50 Amorphous Alloy Reinforced Al Metal Matrix Composites

    Science.gov (United States)

    Reddy, M. Penchal; Ubaid, F.; Shakoor, R. A.; Mohamed, A. M. A.

    2018-06-01

    In the present work, Al metal matrix composites reinforced with Cu-based (Cu50Ti50) amorphous alloy particles synthesized by ball milling followed by a microwave sintering process were studied. The amorphous powders of Cu50Ti50 produced by ball milling were used to reinforce the aluminum matrix. They were examined by x-ray diffraction (XRD), scanning electron microscopy (SEM), microhardness and compression testing. The analysis of XRD patterns of the samples containing 5 vol.%, 10 vol.% and 15 vol.% Cu50Ti50 indicates the presence of Al and Cu50Ti50 peaks. SEM images of the sintered composites show the uniform distribution of reinforced particles within the matrix. Mechanical properties of the composites were found to increase with an increasing volume fraction of Cu50Ti50 reinforcement particles. The hardness and compressive strength were enhanced to 89 Hv and 449 MPa, respectively, for the Al-15 vol.% Cu50Ti50 composites.

  12. Effect of ball-milling time on the structural characteristics of biomedical porous Ti-Sn-Nb alloy

    Energy Technology Data Exchange (ETDEWEB)

    Nouri, Alireza, E-mail: alireza_nouri@yahoo.com [CQM-Centro de Quimica da Madeira, MMRG, Universidade da Madeira, Campus Universitario da Penteada, 9000-390 Funchal (Portugal); Institute for Technology Research and Innovation, Deakin University, Geelong, Victoria 3217 (Australia); Hodgson, Peter D. [Institute for Technology Research and Innovation, Deakin University, Geelong, Victoria 3217 (Australia); Wen Cuie [IRIS, Faculty of Engineering and Industrial Sciences, Swinburne University of Technology, 543-454 Burwood Road, Hawthorn, Victoria 3122 Australia (Australia)

    2011-07-20

    The structural characteristics of biomedical porous materials are crucial for bone tissue to grow into a porous structure and can also influence the fixation and remodeling between the implant and the human tissues. The current study has been investigating the effect of the ball-milling variable of time on the structural characteristics and pore morphology of a biomedical porous Ti-16Sn-4Nb (wt.%) alloy. The alloy was synthesized using high-energy ball milling for different periods of time, and the porous Ti-16Sn-4Nb alloy was fabricated by using a space holder sintering process. The resultant powder particles, bulk, and porous samples were characterized using a scanning electron microscope (SEM), laser particle-size analyzer, chemical analysis, X-ray diffraction analysis (XRD), and the Vickers hardness test. The results indicated that the inner pore surface, pore wall architecture, degree of porosity, pore size and the inter-pore connectivity of the sintered porous alloy are all considerably affected by ball-milling time.

  13. CNTs/Al5083 Composites of High-performance Uniform and Dispersion Fabricated by High-energy Ball-milling

    Directory of Open Access Journals (Sweden)

    GUO Li

    2017-11-01

    Full Text Available Carbon nanotubes (CNTs, mass fraction of 0%-2% reinforced Al5083 composites were fabricated by horizontal high-energy ball milling. The effects of ball milling time and CNTs contents on the properties of composite materials were studied. The micro morphology of CNTs/Al5083 composites was characterized by scanning electron microscopy(SEM and transmission electron microscopy(TEM, the tensile strength and microhardness of the composites were tested. The results indicate that after high-energy ball milling for 1.5h, the carbon nanotubes are dispersed homogeneously in the Al5083 matrix, and good interfacial bonding strength between CNTs and Al5083 is obtained at the addition of 1.5%CNTs. Under these conditions, the tensile strength and microhardness of CNTs/Al5083 composites are 188.8MPa and 136HV, respectively. Compared to Al5083 matrix without CNTs reinforcement, tensile strength and microhardness of CNTs/Al5083 composites are increased by 32.2% and 36%, respectively.

  14. Transformation of Goethite to Hematite Nanocrystallines by High Energy Ball Milling

    Directory of Open Access Journals (Sweden)

    O. M. Lemine

    2014-01-01

    Full Text Available α-Fe2O3 nanocrystallines were prepared by direct transformation via high energy ball milling treatment for α-FeOOH powder. X-ray diffraction, Rietveld analysis, TEM, and vibrating sample magnetometer (VSM are used to characterize the samples obtained after several milling times. Phase identification using Rietveld analysis showed that the goethite is transformed to hematite nanocrystalline after 40 hours of milling. HRTEM confirm that the obtained phase is mostly a single-crystal structure. This result suggested that the mechanochemical reaction is an efficient way to prepare some iron oxides nanocrystallines from raw materials which are abundant in the nature. The mechanism of the formation of hematite is discussed in text.

  15. Characterization of structures and novel magnetic response of Fe87.5Si7Al5.5 alloy processed by ball milling

    International Nuclear Information System (INIS)

    Duan, Yuping; Gu, Shuchao; Zhang, Zhonglun; Wen, Ming

    2012-01-01

    Highlights: ► The water atomized Fe 87.5 Si 7 Al 5.5 (Wt.%) alloy was processed by ball-milling. ► The microstructure and magnetic properties of alloy changed following milling. ► The powders milled for 10 h have the largest M s and strongest reflection loss. ► The permeability of the powders milled for 2 h is the largest. ► The charge exchange between Fe and Si is discussed base on first-principles. - Abstract: The water atomized Fe 87.5 Si 7 Al 5.5 (Wt.%) alloy was processed by a high-energy planetary ball-milling. The characterization of morphology, microstructure, and electromagnetic properties were measured by scanning electron microscope (SEM), X-ray diffractometer, vibrating sample magnetometer (VSM), vector network analyzer and the first principle method. The analysis results showed that the powders shape became flaky from fusiform. The powders showed a reduction of the average grain size and the increase of the internal strain, and then presented an adverse variation trend after 55 h milling. The powders that milled 10 h had the largest saturation magnetization M S (131 emu/g). The value μ′ of the powders decreased with increasing milling time at relatively lower frequency (2–8 GHz), but opposite variation tendency happened at higher frequency (8–18 GHz). Also, only short time milling can enhance the value of μ″ in the test frequency. The powders after 10 h milling showed excellent microwave absorption (RL < −10 dB) at the frequency 9.0–15.6 GHz and the absorption peak shifted regularly to the high frequency as the increased milling time. Furthermore, the effect of charge exchange between the Fe and Si on the saturation magnetization in the ball-milling process was also investigated by using density functional theory (DFT) of first principle.

  16. Development of amorphous and nanocrystalline Al65Cu35-xZrx alloys by mechanical alloying

    International Nuclear Information System (INIS)

    Manna, I.; Chattopadhyay, P.P.; Banhart, F.; Fecht, H.J.

    2004-01-01

    Mechanical alloying of Al 65 Cu 35-x Zr x (x=5, 15 and 25 at.% Zr) elemental powder blends by planetary ball milling up to 50 h yields amorphous and/or nanocrystalline products. Microstructure of the milled product at different stages of milling has been characterized by X-ray diffraction, (XRD) high-resolution transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS). Among the different alloys synthesized by mechanical alloying, Al 65 Cu 20 Zr 15 yields a predominantly amorphous product, while the other two alloys develop a composite microstructure comprising nanocrystalline and amorphous solid solutions in Al 65 Cu 10 Zr 25 and nano-intermetallic phase/compound in Al 65 Cu 30 Zr 5 , respectively. The genesis of solid-state amorphization in Al 65 Cu 20 Zr 15 and Al 65 Cu 10 Zr 25 is investigated

  17. The nature of the photoluminescence in amorphized PZT

    International Nuclear Information System (INIS)

    Silva, M.S.; Cilense, M.; Orhan, E.; Goes, M.S.; Machado, M.A.C.; Santos, L.P.S.; Paiva-Santos, C.O.; Longo, E.; Varela, J.A.; Zaghete, M.A.; Pizani, P.S.

    2005-01-01

    The polymeric precursor method was used to synthesize lead zirconate titanate powder (PZT). The crystalline powder was then amorphized by a high-energy ball milling process during 120 h. A strong photoluminescence emission was observed at room temperature for the amorphized PZT powder. The powders were characterized by XRD and the percentage of amorphous phase was calculated through Rietveld refinement. The microstructure for both phases was investigated by TEM. The optical gap was calculated through the Wood and Tauc method using the UV-Vis. data. Quantum mechanical calculations were carried out to give an interpretation of the photoluminescence in terms of electronic structure

  18. Highly anisotropic SmCo5 nanoflakes by surfactant-assisted ball milling at low temperature

    International Nuclear Information System (INIS)

    Liu, Lidong; Zhang, Songlin; Zhang, Jian; Ping Liu, J.; Xia, Weixing; Du, Juan; Yan, Aru; Yi, Jianhong; Li, Wei; Guo, Zhaohui

    2015-01-01

    Surfactant-assisted ball milling (SABM) has been shown to be a promising method for preparing rare earth-transition metal (RE-TM) nanoflakes and nanoparticles. In this work, we prepared SmCo 5 nanoflakes by SABM at low temperature, and 2-methyl pentane and trioctylamine were specially selected as solvent and surfactant, respectively, due to their low melting points. The effects of milling temperature on the morphology, microstructure and magnetic performance of SmCo 5 nanoflakes were investigated systematically. Comparing with the samples milled at room temperature, the SmCo 5 nanoflakes prepared at low temperature displayed more homogeneous morphology and lower oxygen content. Remarkably, better crystallinity, better grain alignment and larger remanence ratio were shown in the samples milled at low temperature, which resulted from the distinct microstructure caused by low milling temperature. The differences in structural evolution between the SmCo 5 nanoflakes milled at room temperature and low temperature, including the formation of nanocrystalline, grain boundary sliding, grain rotation, et al., were discussed. It was found that lowering the temperature of SABM was a powerful method for the fabrication of RE-TM nanoflakes, which showed better hard magnetic properties and lower oxygen content. This was important for the preparation of high-performance sintered magnets, bonded magnets and nanocomposite magnets. - Highlights: • We prepare SmCo 5 nanoflakes by surfactant-assisted ball milling at low temperature. • Better grain alignment and higher remanence ratio are achieved. • The oxygen content is reduced by lowering the milling temperature. • A distinct microstructural evolution caused by low milling temperature is clarified

  19. Polycrystalline Nd{sub 2}Fe{sub 14}B/α-Fe nanocomposite flakes with a sub-micro/nanometre thickness prepared by surfactant-assisted high-energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Xin, E-mail: tangshincn@gmail.com [Key Laboratory of Magnetic Materials and Devices, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201 (China); Chen, Xi [Mechanical and Electrical Engineering College, Xinxiang University, No. 192, Jinsui Road, Xinxiang, Henan 453003 (China); Chen, Renjie; Yan, Aru [Key Laboratory of Magnetic Materials and Devices, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201 (China)

    2015-09-25

    Highlights: • Nd{sub 2}Fe{sub 14}B/α-Fe flakes are formed by peeling along preferential planes. • (0 0 l) planes are found to be preferential cleavage planes. • Magnetic properties degrade with increasing ball milling time. • Anisotropic nanocomposite magnets are fabricated. - Abstract: A surfactant-assisted high-energy ball milling technique was employed to synthesize Nd{sub 2}Fe{sub 14}B/α-Fe nanoparticles and nanoflakes from melt-spun nanocrystalline powders. The microstructure evolution in ball milling process was investigated. In the beginning stage (0–4 h) of ball milling, raw powders were crushed into micrometre-sized particles. While flakes were mainly formed by reducing thickness of particles via peeling layer by layer along preferential planes in the late stage (8–16 h). The selected area electron diffraction and high-resolution transmission electron microscopy images show that preferential cleavage planes are basal planes. With ball milling proceeding, more and more defects were induced by ball milling. As a result, the coercivity and remanence decreased to 1.6 kOe and 3.2 kGs, respectively. After 16 h ball milling, the exchange decoupling occurred due to severe amorphorization. A weakly-textured nanocomposite magnet was fabricated after 12 h ball milling and the anisotropy in magnetic properties can be further improved by employing settling down process to select particle size and aligning particles in external field.

  20. Study of the preparation of Cu-TiC composites by reaction of soluble Ti and ball-milled carbon coating TiC

    Science.gov (United States)

    Xu, Xuexia; Li, Wenbin; Wang, Yong; Dong, Guozhen; Jing, Shangqian; Wang, Qing; Feng, Yanting; Fan, Xiaoliang; Ding, Haimin

    2018-06-01

    In this work, Cu-TiC composites have been successfully prepared by reaction of soluble Ti and carbon coating TiC. Firstly, the ball milling of graphite and TiC mixtures is used to obtain the carbon coating TiC which has fine size and improved reaction activity. After adding the ball milled carbon coating TiC into Cu-Ti melts, the soluble Ti will easily react with the carbon coating to form TiC. This process will also improve the wettability between Cu melts and TiC core. As a result, besides the TiC prepared by reaction of soluble Ti and carbon coating, the ball milled TiC will also be brought into the melts. Some of these ball-milled TiC particles will go on being coated by the formed TiC from the reaction of Ti and the coating carbon and left behind in the composites. However, most of TiC core will be further reacted with the excessive Ti and be transformed into the newly formed TiC with different stoichiometry. The results indicate that it is a feasible method to synthesize TiC in Cu melts by reaction of soluble Ti and ball-milled carbon coating TiC.

  1. XRD and HREM studies from the decomposition of icosahedral AlCuFe single-phase by high-energy ball milling

    International Nuclear Information System (INIS)

    Patino-Carachure, C.; Tellez-Vazquez, O.; Rosas, G.

    2011-01-01

    Highlights: → Point defects induced during milling leading to an order-disorder quasicrystal transition. → Nanoquasicrystalline regions of 12 nm are obtained. → Highly ordered i-phase with high symmetry transforms to a crystalline phase of intermetallic character and lower symmetry. - Abstract: In this investigation the Al 64 Cu 24 Fe 12 alloy was melted in an induction furnace and solidified under normal casting conditions. In order to obtain the icosahedral phase (i-phase) in a single-phase region, the as-cast sample was subject to a heat treatment at 700 deg. C under argon atmosphere. Subsequently, the i-phase was milled for different times in order to evaluate phase stability under heavy deformation. X-ray diffraction (XRD) and high-resolution electron microscopy (HREM) analysis were conducted to the structural characterization of ball-milled powders. XRD results indicated a reduction in quasicrystal size during mechanical ball milling to about 30 h. HREM analysis revealed the presence of aperiodic nano-domains, for example, with apparent fivefold symmetry axis. Therefore, the i-phase remains stable over the first 30 h of ball-milling time. However, among 30-50 h of mechanical milling the i-phase transforms progressively into β-cubic phase.

  2. XRD and HREM studies from the decomposition of icosahedral AlCuFe single-phase by high-energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Patino-Carachure, C.; Tellez-Vazquez, O. [Instituto de Investigaciones Metalurgicas, UMSNH, Edificio U, Ciudad Universitaria, Morelia, Michoacan 58000 (Mexico); Rosas, G., E-mail: grtrejo@umich.mx [Instituto de Investigaciones Metalurgicas, UMSNH, Edificio U, Ciudad Universitaria, Morelia, Michoacan 58000 (Mexico)

    2011-10-13

    Highlights: > Point defects induced during milling leading to an order-disorder quasicrystal transition. > Nanoquasicrystalline regions of 12 nm are obtained. > Highly ordered i-phase with high symmetry transforms to a crystalline phase of intermetallic character and lower symmetry. - Abstract: In this investigation the Al{sub 64}Cu{sub 24}Fe{sub 12} alloy was melted in an induction furnace and solidified under normal casting conditions. In order to obtain the icosahedral phase (i-phase) in a single-phase region, the as-cast sample was subject to a heat treatment at 700 deg. C under argon atmosphere. Subsequently, the i-phase was milled for different times in order to evaluate phase stability under heavy deformation. X-ray diffraction (XRD) and high-resolution electron microscopy (HREM) analysis were conducted to the structural characterization of ball-milled powders. XRD results indicated a reduction in quasicrystal size during mechanical ball milling to about 30 h. HREM analysis revealed the presence of aperiodic nano-domains, for example, with apparent fivefold symmetry axis. Therefore, the i-phase remains stable over the first 30 h of ball-milling time. However, among 30-50 h of mechanical milling the i-phase transforms progressively into {beta}-cubic phase.

  3. Kinetics and formation mechanism of amorphous Fe52Nb48 alloy powder fabricated by mechanical alloying

    International Nuclear Information System (INIS)

    El-Eskandarany, S.

    1999-01-01

    A single phase amorphous Fe 52 Nb 48 alloy has been synthesized through a solid state interdiffusion of pure polycrystalline Fe and Nb powders at room temperature, using a high-energy ball-milling technique. The mechanisms of metallic glass formation and competing crystallization processes in the mechanically deformed composite powders have been investigated by means of X-ray diffraction, Moessbauer spectroscopy, differential thermal analysis, scanning electron microscopy and transmission electron microscopy. The numerous intimate layered composite particles of the diffusion couples that formed during the first and intermediate stages of milling time (0-56 ks), are intermixed to form amorphous phase(s) upon heating to about 625 K by so-called thermally assisted solid state amorphization, TASSA. The amorphization heat of formation for binary system via the TASSA, ΔH a , was measured directly as a function of the milling time. Comparable with the TASSA, homogeneous amorphous alloys were fabricated directly without heating the composite multilayered particles upon milling these particles for longer milling time (86 ks-144 ks). The amorphization reaction here is attributed to the mechanical driven solid state amorphization. This single amorphous phase transforms into an order phase (μ phase) upon heating at 1088 K (crystallization temperature, T x ) with enthalpy change of crystallization, ΔH x , of -8.3 kJmol -1 . (orig.)

  4. Formation of amorphous Ti-50at.%Pt by solid state reactions during mechanical alloying

    CSIR Research Space (South Africa)

    Mahlatji, ML

    2013-10-01

    Full Text Available Mechanical alloying of an equiatomic mixture of crystalline elemental powders of Ti and Pt in a high-energy ball mill results in formation of an amorphous alloy by solid-state reactions. Mechanical alloying was carried out in an argon atmosphere...

  5. Characterization of prealloyed copper powders treated in high energy ball mill

    International Nuclear Information System (INIS)

    Rajkovic, Viseslava; Bozic, Dusan; Jovanovic, Milan T.

    2006-01-01

    The inert gas atomised prealloyed copper powders containing 3.5 wt.% Al were milled up to 20 h in the planetary ball mill in order to oxidize aluminium in situ with oxygen from the air. In the next procedure compacts from milled powder were synthesized by hot-pressing in argon atmosphere. Compacts from as-received Cu-3.5 wt.% Al powder and electrolytic copper powder were also prepared under the same conditions. Microstructural and morphological changes of high energy milled powder as well as changes of thermal stability and electrical conductivity of compacts were studied as a function of milling time and high temperature exposure at 800 deg. C. Optical, scanning electron microscopy (SEM) and X-ray diffraction analysis were performed for microstructural characterization, whereas thermal stability and electrical conductivity were evaluated by microhardness measurements and conductometer Sigmatest, respectively. The prealloyed 5 h-milled and compacted powder showed a significant increase in microhardness reaching the value of 2600 MPa, about 4 times greater than that of compacts synthesized from as-received electrolytic copper powder (670 MPa). The electrical conductivity of compacts from 5 h-milled powder was 52% IACS. The results were discussed in terms of the effect of small grain size and finely distributed alumina dispersoids on hardening and thermal stability of compacts

  6. Magnetic and mechanical properties of Cu (75 wt%) – 316L grade stainless steels synthesized by ball milling and annealing

    Energy Technology Data Exchange (ETDEWEB)

    Mondal, Bholanath, E-mail: bholanath_mondal@yahoo.co.in [Department of Central Scientific Services, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700032 (India); Chabri, Sumit [Department of Metallurgy and Materials Engineering, Indian Institute of Engineering Science and Technology, Shibpur, Howrah 711103 (India); Sardar, Gargi [Department of Zoology, Baruipur College, South 24 Parganas, 743610 (India); Bhowmik, Nandagopal [Department of Metallurgy and Materials Engineering, Indian Institute of Engineering Science and Technology, Shibpur, Howrah 711103 (India); Sinha, Arijit, E-mail: arijitsinha2@yahoo.co.in [School of Materials Science and Engineering, Indian Institute of Engineering Science and Technology, Shibpur, Howrah 711103 (India); Chattopadhyay, Partha Protim [Department of Metallurgy and Materials Engineering, Indian Institute of Engineering Science and Technology, Shibpur, Howrah 711103 (India)

    2015-05-01

    Elemental powders of Cu (75 wt%) and 316-stainless steel (25 wt%) has been subjected to ball milling upto 70 h followed by isothermal annealing at the temperature range of 350–750 °C for 1 h to investigate the microstructural evolution along with magnetic and mechanical properties. After 40 h of milling, the bcc Fe is almost dissolved in the solid solution of Cu but no significant change has been observed in the XRD pattern after 70 h of milling, Annealing of the alloy has resulted in precipitation of nanocrystalline bcc-Fe in Cu which triggers the soft ferromagnetic properties. The extensive mechanical characterization has been done at the microstructural scale by nanoindentation technique which demonstrates a hardening behavior of the compacted and annealed alloys due to possible precipitation of nanocrystalline bcc-Fe in Cu. - Highlights: • Nanocrystalline phases with partial amorphorization obtained after 70 h of milling. • Precipitation and grain coarsening of Fe and Cu after annealing as observed by XRD. • Annealing of the ball milled sample upto 550 {sup o}C has evolved ferromagnetic behavior. • Nanoindentation predicts a hardening behavior of annealed ball milled samples.

  7. Nanocrystalline Al-based alloys - lightweight materials with attractive mechanical properties

    International Nuclear Information System (INIS)

    Latuch, J; Cieslak, G; Dimitrov, H; Krasnowski, M; Kulik, T

    2009-01-01

    In this study, several ways of bulk nanocrystalline Al-based alloys' production by high-pressure compaction of powders were explored. The effect of chemical composition and compaction parameters on the structure, quality and mechanical properties of the bulk samples was studied. Bulk nanocrystalline Al-Mm-Ni-(Fe,Co) alloys were prepared by ball-milling of amorphous ribbons followed by consolidation. The maximum microhardness (540 HV0.1) was achieved for the samples compacted at 275 deg. C under 7.7 GPa (which resulted in an amorphous bulk) and nanocrystallised at 235 deg. C for 20 min. Another group of the produced materials were bulk nanocrystalline Al-Si-(Ni,Fe)-Mm alloys obtained by ball-milling of nanocrystalline ribbons and consolidation. The hardness of these samples achieved the value five times higher (350HV) than that of commercial 4xxx series Al alloys. Nanocrystalline Al-based alloys were also prepared by mechanical alloying followed by hot-pressing. In this group of materials, there were Al-Fe alloys containing 50-85 at.% of Al and ternary or quaternary Al-Fe-(Ti, Si, Ni, Mg, B) alloys. Microhardness of these alloys was in the range of 613 - 1235 HV0.2, depending on the composition.

  8. Mechanical intermixing of components in (CoMoNi)-based systems and the formation of (CoMoNi)/WC nanocomposite layers on Ti sheets under ball collisions

    Science.gov (United States)

    Romankov, S.; Park, Y. C.; Shchetinin, I. V.

    2017-11-01

    Cobalt (Co), molybdenum (Mo), and nickel (Ni) components were simultaneously introduced onto titanium (Ti) surfaces from a composed target using ball collisions. Tungsten carbide (WC) balls were selected for processing as the source of a cemented carbide reinforcement phase. During processing, ball collisions continuously introduced components from the target and the grinding media onto the Ti surface and induced mechanical intermixing of the elements, resulting in formation of a complex nanocomposite structure onto the Ti surface. The as-fabricated microstructure consisted of uniformly dispersed WC particles embedded within an integrated metallic matrix composed of an amorphous phase with nanocrystalline grains. The phase composition of the alloyed layers, atomic reactions, and the matrix grain sizes depended on the combination of components introduced onto the Ti surface during milling. The as-fabricated layer exhibited a very high hardness compared to industrial metallic alloys and tool steel materials. This approach could be used for the manufacture of both cemented carbides and amorphous matrix composite layers.

  9. Amorphization and evolution of magnetic properties during mechanical alloying of Co{sub 62}Nb{sub 6}Zr{sub 2}B{sub 30}: Dependence on starting boron microstructure

    Energy Technology Data Exchange (ETDEWEB)

    Moreno, L.M.; Blázquez, J.S., E-mail: jsebas@us.es; Ipus, J.J.; Conde, A.

    2014-02-05

    Highlights: • Mechanical alloying of Co{sub 62}Nb{sub 6}Zr{sub 2}B{sub 30} leads to amorphous phase with B inclusions. • Using optimized amorphous B, amorphization occurs earlier. • B is more effectively introduced in the matrix using amorphous B. • Magnetoelasic contribution to effective magnetic anisotropy is negligible. -- Abstract: Co{sub 62}Nb{sub 6}Zr{sub 2}B{sub 30} composition was mechanically alloyed using three different types of boron powders in the starting mixture: crystalline β-B, commercial amorphous B and optimized amorphous B via ball milling. Using optimized amorphous B, amorphization process of the alloy is more efficient but milling to optimize amorphous B introduces some iron contamination. Boron inclusions (100–150 nm in size) remain even after long milling times. However, using amorphous boron reduces the fraction of boron distributed as inclusions to ∼40% of the total B. Thermal stability at the end of the milling process is affected by the initial boron microstructure. Coercivity is reduced a half using amorphous B instead of crystalline B in the starting mixture.

  10. Effect of ball milling time on the hydrogen storage properties of TiF{sub 3}-doped LiAlH{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Shu-Sheng [Materials and Thermochemistry Laboratory, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian, Liaoning 116023 (China); Graduate School of Chinese Academy of Sciences, Beijing 100049 (China); Sun, Li-Xian; Zhang, Yao; Zhang, Jian; Chu, Hai-Liang; Fan, Mei-Qiang; Zhang, Tao [Materials and Thermochemistry Laboratory, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian, Liaoning 116023 (China); Xu, Fen [Faculty of Chemistry and Chemical Engineering, Liaoning Normal University, Dalian 116029 (China); Song, Xiao-Yan [College of Materials Science and Engineering, Key Laboratory of Advanced Functional Materials, Chinese Education Ministry, Beijing University of Technology, Beijing 100124 (China); Grolier, Jean Pierre [Laboratory of Thermodynamics of Solutions and Polymers, Blaise Pascal University, 24 Avenue des Landais, 63177-Aubiere Cedex (France)

    2009-10-15

    In the present work, the catalytic effect of TiF{sub 3} on the dehydrogenation properties of LiAlH{sub 4} has been investigated. Decomposition of LiAlH{sub 4} occurs during ball milling in the presence of 4 mol% TiF{sub 3}. Different ball milling times have been used, from 0.5 h to 18 h. With ball milling time increasing, the crystallite sizes of LiAlH{sub 4} get smaller (from 69 nm to 43 nm) and the dehydrogenation temperature becomes lower (from 80 C to 60 C). Half an hour ball milling makes the initial dehydrogenation temperature of doped LiAlH{sub 4} reduce to 80 C, which is 70 C lower than as-received LiAlH{sub 4}. About 5.0 wt.% H{sub 2} can be released from TiF{sub 3}-doped LiAlH{sub 4} after 18 h ball milling in the range of 60 C-145 C (heating rate 2 C min{sup -1}). TiF{sub 3} probably reacts with LiAlH{sub 4} to form the catalyst, TiAl{sub 3}. The mechanochemical and thermochemical reactions have been clarified. However, the rehydrogenation of LiAlH{sub 4}/Li{sub 3}AlH{sub 6} can not be realized under 95 bar H{sub 2} in the presence of TiF{sub 3} because of their thermodynamic properties. (author)

  11. Efficiency of ball milled South African bentonite clay for remediation of acid mine drainage

    CSIR Research Space (South Africa)

    Masindi, Vhahangwele

    2015-12-01

    Full Text Available The feasibility of using vibratory ball milled South African bentonite clay for neutralization and attenuation of inorganic contaminants from acidic and metalliferous mine effluents has been evaluated. Treatment of acid mine drainage (AMD...

  12. Highly anisotropic SmCo{sub 5} nanoflakes by surfactant-assisted ball milling at low temperature

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Lidong; Zhang, Songlin [Key Laboratory of Magnetic Materials and Devices, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Science, Ningbo 315201 (China); Zhejiang Province Key Laboratory of Magnetic Materials and Application Technology, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Science, Ningbo 315201 (China); Zhang, Jian, E-mail: zhangj@nimte.ac.cn [Key Laboratory of Magnetic Materials and Devices, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Science, Ningbo 315201 (China); Zhejiang Province Key Laboratory of Magnetic Materials and Application Technology, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Science, Ningbo 315201 (China); Ping Liu, J. [Department of Physics, University of Texas at Arlington, Arlington, TX 76019 (United States); Xia, Weixing; Du, Juan; Yan, Aru [Key Laboratory of Magnetic Materials and Devices, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Science, Ningbo 315201 (China); Zhejiang Province Key Laboratory of Magnetic Materials and Application Technology, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Science, Ningbo 315201 (China); Yi, Jianhong [Institute of Material Science and Engineering, Kunming University of Science and Technology, Kunming 650500 (China); Li, Wei; Guo, Zhaohui [Division of Functional Materials, Central Iron and Steel Research Institute, Beijing 100081 (China)

    2015-01-15

    Surfactant-assisted ball milling (SABM) has been shown to be a promising method for preparing rare earth-transition metal (RE-TM) nanoflakes and nanoparticles. In this work, we prepared SmCo{sub 5} nanoflakes by SABM at low temperature, and 2-methyl pentane and trioctylamine were specially selected as solvent and surfactant, respectively, due to their low melting points. The effects of milling temperature on the morphology, microstructure and magnetic performance of SmCo{sub 5} nanoflakes were investigated systematically. Comparing with the samples milled at room temperature, the SmCo{sub 5} nanoflakes prepared at low temperature displayed more homogeneous morphology and lower oxygen content. Remarkably, better crystallinity, better grain alignment and larger remanence ratio were shown in the samples milled at low temperature, which resulted from the distinct microstructure caused by low milling temperature. The differences in structural evolution between the SmCo{sub 5} nanoflakes milled at room temperature and low temperature, including the formation of nanocrystalline, grain boundary sliding, grain rotation, et al., were discussed. It was found that lowering the temperature of SABM was a powerful method for the fabrication of RE-TM nanoflakes, which showed better hard magnetic properties and lower oxygen content. This was important for the preparation of high-performance sintered magnets, bonded magnets and nanocomposite magnets. - Highlights: • We prepare SmCo{sub 5} nanoflakes by surfactant-assisted ball milling at low temperature. • Better grain alignment and higher remanence ratio are achieved. • The oxygen content is reduced by lowering the milling temperature. • A distinct microstructural evolution caused by low milling temperature is clarified.

  13. A Novel synthesis of MgS and its application as electrode material for lithium-ion batteries

    International Nuclear Information System (INIS)

    Wang, Minjuan; Li, Xiang; Gao, Mingxia; Pan, Hongge; Liu, Yongfeng

    2014-01-01

    Highlights: • Nanocrystallite MgS was synthesized by means of a reaction of MgH 2 of S via ball milling. • MgS was firstly investigated as anode material for lithium-ion batteries (LIBs). • MgS with acetylene black introduced by ball milling shows superior electrochemical property. • The mechanisms of the lithium insertion and extraction processes of MgS are discussed. • The work is considered helpful in developing new electrode material for LIBs. - Abstract: MgS was firstly investigated as an anode material for lithium-ion batteries (LIBs). A novel method for the synthesis of nano-sized MgS was conducted, i.e., by means of a reaction of MgH 2 of S via ball milling. Acetylene black (AB) was used as electron conductive agent and introduced by two approaches to the MgS anode material: the one is ball milling AB with the as-prepared MgS derived from MgH 2 and S; the other is pre-milling AB with S and then further milling the mixture with MgH 2 . X-ray diffraction, scanning electron microscopy, transmission electron microscopy (TEM) and high resolution TEM analyses show that MgS/AB composites with MgS nanocrystallites embedded in the AB matrix are formed via either of the approaches. The MgS anode derived from MgH 2 and the pre-milled S/AB mixture shows high capacity. Capacity fading occurs mainly in the initial several cycles. A capacity of 630 mA h/g is retained after 80 cycles. The electrochemical property is much better than that of the MgS/AB derived from MgS and AB, due to the much homogenous microstructure of the former. The mechanism of the lithium insertion and extraction process of MgS is primarily discussed. The work is considered helpful in developing new synthesis method for MgS and new electrode material for LIBs

  14. The microstructure of mechanically alloyed Al-Mg determined by X-ray diffraction peak profile analysis

    Energy Technology Data Exchange (ETDEWEB)

    Gubicza, J.; Kassem, M.; Ribarik, G.; Ungar, T

    2004-05-15

    The effect of the nominal Mg content and the milling time on the microstructure and the hardness of mechanically alloyed Al-rich Al-Mg solid solutions is studied. The crystallite size distribution and the dislocation structure are characterized by X-ray diffraction (XRD) peak profile analysis and the hardness is obtained from depth-sensing indentation tests. Magnesium gradually goes into solid solution during ball milling and after 3 h an almost complete solid solution is attained. With increasing milling time, the Mg concentration in solid solution, the dislocation density and the hardness increase, whereas the crystallite size decreases. A similar tendency of these parameters is observed at a particular duration of ball milling with increasing nominal Mg content. After 3 h milling there are no changes in both the microstructure and the hardness.

  15. Microstructure and hydrogen sorption kinetics of Mg nanopowders with catalyst

    International Nuclear Information System (INIS)

    Revesz, A.; Fatay, D.; Spassov, T.

    2007-01-01

    MgH 2 powders were ball-milled with and without catalysts (Nb 2 O 5 ) under hydrogen in a high-energy mill for 10 h. Morphological, structural and microstructural characterization of the nanocomposites, including particle and crystallite size distribution were carried out before and after hydrogen absorption. In order to study the above-mentioned microstructural parameters imaging and X-ray scattering techniques (high-resolution X-ray diffractometry) have been employed. The effect of the particle and grain size on the hydriding/dehydriding kinetics of ball-milled MgH 2 + catalyst powders was analyzed. The grain and particle size reduction enhances substantially the hydriding/dehydriding

  16. Magnetic properties of ball-milled Fe0.6Mn0.1Al0.3 alloys

    International Nuclear Information System (INIS)

    Rebolledo, A.F.; Romero, J.J.; Cuadrado, R.; Gonzalez, J.M.; Pigazo, F.; Palomares, F.J.; Medina, M.H.; Perez Alcazar, G.A.

    2007-01-01

    The FeMnAl-disordered alloy system exhibits, depending on the composition and the temperature, a rich variety of magnetic phases including the occurrence of ferromagnetism, antiferromagnetism, paramagnetism and spin-glass and reentrant spin glass behaviors. These latter phases result from the presence of atomic disorder and magnetic dilution and from the competing exchange interactions taking place between an Fe atom and its Mn and Fe first neighbors. The use of mechanical alloying in order to prepare these alloys is specially interesting since it allows to introduce in a progressive way large amounts of disorder. In this work, we describe the evolution with the milling time of the temperature dependence of the magnetic properties of mechanically alloyed Fe 0.6 Mn 0.1 Al 0.3 samples. The materials were prepared in a planetary ball mill using a balls-to-powder mass ratio of 15:1 and pure (99.95 at%) Fe, Mn and Al powders for times up to 19 h. The X-rays diffraction (XRD) spectra show the coexistence of three phases at short milling times. For milling times over 6 h, only the FeMnAl ternary alloy BCC phase is observed. Moesbauer spectroscopy reveals the complete formation of the FeMnAl alloy after 9 h milling time. The magnetic characterization showed that all the samples were ferromagnetic at room temperature with coercivities decreasing from 105 Oe (3 h milled sample) down to 5 Oe in the case of the sample milled for 19 h

  17. Solid-state amorphization in the Ni-Zr system investigated by positron lifetime spectroscopy

    International Nuclear Information System (INIS)

    Bernal, M.J.; De La Cruz, R.M.; Leguey, T.; Pareja, R.; Riveiro, J.M.

    1995-01-01

    The process of mechanical alloying and amorphization of Ni-Zr powders is investigated by positron lifetime spectroscopy, X-ray diffraction and differential scanning calorimetry. The short-lived component of the lifetime spectra is composition and milling-time dependent. The second lifetime component, found during the initial stages of the milling process, appears to be due to annihilation from states trapped at crystalline interface joints. The results indicate that the solid-state reactions induced by ball milling involve the transformation and disappearance of the crystalline interface joints in the powder particles. (orig.)

  18. Mg amorphous alloys for biodegradable implants

    International Nuclear Information System (INIS)

    Danez, G.P.; Koga, G.Y.; Tonucci, S.; Bolfarini, C.; Kiminami, C.S.; Botta Filho, W.J.

    2010-01-01

    The use of implants made from amorphous alloys magnesium-based with additions of zinc and calcium are promising. Properties such as biocompatibility, low density, high mechanical strength, low modulus (as compared to alloys such as stainless steel and titanium), corrosion resistance and wear resistance make it attractive for use in implants. Moreover, the by-products of corrosion and wear are not toxic and may contribute to fixation. Aiming to understand the tendency of this amorphous ternary (Mg-Zn-Ca) and expand the information about this system, this work involved the use of the topological criterion of instability (λ) and the criterion of electronegativity (Δe) to the choice of compositions. The alloys were processed into wedge-shaped and analyzed structurally and in X-ray diffraction and scanning electron microscopy. (author)

  19. First-principles study of crystalline and amorphous AlMgB14-based materials

    International Nuclear Information System (INIS)

    Ivashchenko, V. I.; Shevchenko, V. I.; Turchi, P. E. A.; Veprek, S.; Leszczynski, Jerzy; Gorb, Leonid; Hill, Frances

    2016-01-01

    We report first-principles investigations of crystalline and amorphous boron and M1 x M2 y X z B 14−z (M1, M2 = Al, Mg, Li, Na, Y; X = Ti, C, Si) phases (so-called “BAM” materials). Phase stability is analyzed in terms of formation energy and dynamical stability. The atomic configurations as well as the electronic and phonon density states of these phases are compared. Amorphous boron consists of distorted icosahedra, icosahedron fragments, and dioctahedra, connected by an amorphous network. The presence of metal atoms in amorphous BAM materials precludes the formation of icosahedra. For all the amorphous structures considered here, the Fermi level is located in the mobility gap independent of the number of valence electrons. The intra-icosahedral vibrations are localized in the range of 800 cm −1 , whereas the inter-icosahedral vibrations appear at higher wavenumbers. The amorphization leads to an enhancement of the vibrations in the range of 1100–1250 cm −1 . The mechanical properties of BAM materials are investigated at equilibrium and under shear and tensile strain. The anisotropy of the ideal shear and tensile strengths is explained in terms of a layered structure of the B 12 units. The strength of amorphous BAM materials is lower than that of the crystalline counterparts because of the partial fragmentation of the boron icosahedra in amorphous structures. The strength enhancement found experimentally for amorphous boron-based films is very likely related to an increase in film density, and the presence of oxygen impurities. For crystalline BAM materials, the icosahedra are preserved during elongation upon tension as well as upon shear in the (010)[100] slip system.

  20. Crystallization Behavior of A Bulk Amorphous Mg62Cu26Y12 Alloy

    Science.gov (United States)

    Wu, Shyue-Sheng; Chin, Tsung-Shune; Su, Kuo-Chang

    1994-07-01

    The crystallization temperature, the associated activation energy and the crystallized structure of a bulk amorphous Mg62Cu26Y12 alloy with a diameter of 2.5 mm were studied. It possesses a one-step crystallization behavior. The crystallization reaction was found to be represented by: AM(MG62Cu26Y12)→Mg2Cu+MgY+CuY+Mg, ( Tx=188°C, Eac=134 kJ/mol) where AM represents the amorphous state, T x the crystallization temperature at an infinitesimal heating rate, and E ac the associated activation energy. The amount of crystalline phases were found to be Mg2Cu:MgY:CuY=76:17:7. The Mg phase is identifiable only by high resolution electron microscopy, not by X-ray diffraction. The crystallization leads to a sharp rise in electrical resistivity which is reversed to those of iron-based amorphous alloys.

  1. Surface Generation Modeling in Ball Nose End Milling: a review of relevant literature

    DEFF Research Database (Denmark)

    Bissacco, Giuliano

    One of the most common metal removal operation used in industry is the milling process. This machining process is well known since the beginning of last century and has experienced, along the years, many improvements of the basic technology, as concerns tools, machine tools, coolants...... to be adjusted afterwards. Nevertheless, many efforts have been done during the last 50 years in order to realize prediction tools for machining processes and particularly for conventional turning and milling operations. Most of these models aim at prediction of cutting forces tool wear and tool life. However...... been addressed in this direction. Among all the machining operations, ball nose end milling has shown great potentials, particularly in machining of sculptured surfaces with high requirements in terms of surface finish; this is due to the good spatial agreement of the mill shape with the geometry...

  2. Application of a Salt Coformer in a Co-Amorphous Drug System Dramatically Enhances the Glass Transition Temperature: A Case Study of the Ternary System Carbamazepine, Citric Acid, and l-Arginine.

    Science.gov (United States)

    Ueda, Hiroshi; Wu, Wenqi; Löbmann, Korbinian; Grohganz, Holger; Müllertz, Anette; Rades, Thomas

    2018-04-13

    The use of co-amorphous systems containing a combination of low molecular weight drugs and excipients is a relatively new technology in the pharmaceutical field to improve the solubility of poorly water-soluble drugs. However, some co-amorphous systems show a lower glass transition temperature ( T g ) than many of their polymeric solid dispersion counterparts. In this study, we aimed at designing a stable co-amorphous system with an elevated T g . Carbamazepine (CBM) and citric acid (CA) were employed as the model drug and the coformer, respectively. co-amorphous CBM-CA at a 1:1 molar ratio was formed by ball milling, but a transition from the glassy to the supercooled melt state was observed under ambient conditions, due to the relatively low T g of 38.8 °C of the co-amorphous system and moisture absorption. To improve the T g of the coformer, salt formation of a combination of l-arginine (ARG) with CA was studied. First, ball milling of CA-ARG at molar ratios of 1:1, 1:2, and 1:3 forming co-amorphous systems was performed and led to a dramatic enhancement of the T g , depending on the CA-ARG ratio. Salt formation between CA and ARG was observed by infrared spectroscopy. Next, ball milling of CBM-CA-ARG at molar ratios of 1:1:1, 1:1:2, and 1:1:3 resulted in co-amorphous blends, which had a single T g at 77.8, 105.3, and 127.8 °C, respectively. These ternary co-amorphous samples remained in a solid amorphous form for 2 months at 40 °C. From these results, it can be concluded that blending of the salt coformer with a drug is a promising strategy to design stable co-amorphous formulations.

  3. Microstructural changes and effect of variation of lattice strain on positron annihilation lifetime parameters of zinc ferrite nanocomposites prepared by high enegy ball-milling

    Directory of Open Access Journals (Sweden)

    Abhijit Banerjee

    2012-12-01

    Full Text Available Zn-ferrite nanoparticles were synthesized at room temperature by mechanical alloying the stoichiometric (1:1 mol% mixture of ZnO and α-Fe2O3 powder under open air. Formation of both normal and inverse spinel ferrite phases was noticed after 30 minutes and 2.5 hours ball milling respectively and the content of inverse spinel phase increased with increasing milling time. The phase transformation kinetics towards formation of ferrite phases and microstructure characterization of ball milled ZnFe2O4 phases was primarily investigated by X-ray powder diffraction pattern analysis. The relative phase abundances of different phases, crystallite size, r.m.s. strain, lattice parameter change etc. were estimated from the Rietveld powder structure refinement analysis of XRD data. Positron annihilation lifetime spectra of all ball milled samples were deconvoluted with three lifetime parameters and their variation with milling time duration was explained with microstructural changes and formation of different phases with increase of milling time duration.

  4. Bioethanol production from ball milled bagasse using an on-site produced fungal enzyme cocktail and xylose-fermenting Pichia stipitis.

    Science.gov (United States)

    Buaban, Benchaporn; Inoue, Hiroyuki; Yano, Shinichi; Tanapongpipat, Sutipa; Ruanglek, Vasimon; Champreda, Verawat; Pichyangkura, Rath; Rengpipat, Sirirat; Eurwilaichitr, Lily

    2010-07-01

    Sugarcane bagasse is one of the most promising agricultural by-products for conversion to biofuels. Here, ethanol fermentation from bagasse has been achieved using an integrated process combining mechanical pretreatment by ball milling, with enzymatic hydrolysis and fermentation. Ball milling for 2 h was sufficient for nearly complete cellulose structural transformation to an accessible amorphous form. The pretreated cellulosic residues were hydrolyzed by a crude enzyme preparation from Penicillium chrysogenum BCC4504 containing cellulase activity combined with Aspergillus flavus BCC7179 preparation containing complementary beta-glucosidase activity. Saccharification yields of 84.0% and 70.4% for glucose and xylose, respectively, were obtained after hydrolysis at 45 degrees C, pH 5 for 72 h, which were slightly higher than those obtained with a commercial enzyme mixture containing Acremonium cellulase and Optimash BG. A high conversion yield of undetoxified pretreated bagasse (5%, w/v) hydrolysate to ethanol was attained by separate hydrolysis and fermentation processes using Pichia stipitis BCC15191, at pH 5.5, 30 degrees C for 24 h resulting in an ethanol concentration of 8.4 g/l, corresponding to a conversion yield of 0.29 g ethanol/g available fermentable sugars. Comparable ethanol conversion efficiency was obtained by a simultaneous saccharification and fermentation process which led to production of 8.0 g/l ethanol after 72 h fermentation under the same conditions. This study thus demonstrated the potential use of a simple integrated process with minimal environmental impact with the use of promising alternative on-site enzymes and yeast for the production of ethanol from this potent lignocellulosic biomass. 2009. Published by Elsevier B.V.

  5. Effects of processing parameters on the synthesis of (K0.5Na0.5)NbO3 nanopowders by reactive high-energy ball milling method.

    Science.gov (United States)

    Nguyen, Duc Van

    2014-01-01

    The effects of ball milling parameters, namely, the ball-to-powder mass ratio and milling speed, on the synthesis of (K0.5Na0.5)NbO3 nanopowders by high-energy ball milling method from a stoichiometric mixture containing Na2CO3, K2CO3, and Nb2O5 were investigated in this paper. The results indicated that the single crystalline phase of (K0.5Na0.5)NbO3 was received in as-milled samples synthesized using optimized ball-to-powder mass ratio of 35 : 1 and at a milling speed of 600 rpm for 5 h. In the optimized as-milled samples, no remaining alkali carbonates that can provide the volatilizable potassium-containing species were found and (K0.5Na0.5)NbO3 nanopowders were readily obtained via the formation of an intermediate carbonato complex. This complex was mostly transformed into (K0.5Na0.5)NbO3 at temperature as low as 350°C and its existence was no longer detected at spectroscopic level when calcination temperature crossed over 700°C.

  6. Fabrication mechanism of FeSe superconductors with high-energy ball milling aided sintering process

    International Nuclear Information System (INIS)

    Zhang, Shengnan; Liu, Jixing; Feng, Jianqing; Wang, Yao; Ma, Xiaobo; Li, Chengshan; Zhang, Pingxiang

    2015-01-01

    FeSe Superconducting bulks with high content of superconducting PbO-type β-FeSe phase were prepared with high-energy ball milling (HEBM) aided sintering process. During this process, precursor powders with certain Fe/Se ratio were ball milled first then sintered. The influences of HEBM process as well as initial Fe/Se ratio on the phase evolution process were systematically discussed. With HEBM process and proper initial Fe/Se ratio, the formation of non-superconducting hexagonal δ-FeSe phase were effectively avoided. FeSe bulk with the critical temperature of 9.0 K was obtained through a simple one-step sintering process with lower sintering temperature. Meanwhile, the phase evolution mechanism of the HEBM precursor powders during sintering was deduced based on both the thermodynamic analysis and step-by-step sintering results. The key function of the HEBM process was to provide a high uniformity of chemical composition distribution, thus to successfully avoide the formation of intermediate product during sintering, including FeSe 2 and Fe 7 Se 8 . Therefore, the fundamental principal for the synthesis of FeSe superconductors were concluded as: HEBM aided sintering process, with the sintering temperature of >635 °C and a slow cooling process. - Highlights: • A novel synthesis technique was developed for FeSe based superconductors. • FeSe bulks with high Tc and high β-FeSe phase content has been obtained. • Phase evolution process for the HEBM aided sintering process was proposed

  7. Ferromagnetic resonance parameters of ball-milled Ni-Zn ferrite nanoparticles

    International Nuclear Information System (INIS)

    Rao, B. Parvatheeswara; Caltun, Ovidiu; Dumitru, Ioan; Spinu, Leonard

    2006-01-01

    Ferrite nanoparticles of the size about 6 nm have been made by using high-energy ball mill on the sintered pellets of the system Ni 0.65 Zn 0.375 In x Ti 0.025 Fe 1.95- x O 4 . XRD, VSM and FMR techniques were used for structural and magnetic characterizations of the samples. The magnetic characteristics of indium-doped samples are compared with those for bulk samples. The differences are discussed in terms of the particle size and small-particle magnetism

  8. Influence of milling parameters on the sorption properties of the LiH–MgB{sub 2} system doped with TiCl{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Busch, Nina; Jepsen, Julian; Pistidda, Claudio [Institute of Materials Research, Helmholtz-Zentrum Geesthacht, Max-Planck-Straße 1, D-21502 Geesthacht (Germany); Puszkiel, Julián A. [Institute of Materials Research, Helmholtz-Zentrum Geesthacht, Max-Planck-Straße 1, D-21502 Geesthacht (Germany); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Combatientes de Malvinas 3150, 1427 Buenos Aires (Argentina); Karimi, Fahim [Institute of Materials Research, Helmholtz-Zentrum Geesthacht, Max-Planck-Straße 1, D-21502 Geesthacht (Germany); Milanese, Chiara [Pavia H_2 Lab, Department of Chemistry, Physical Chemistry Division, University of Pavia, Viale Taramelli 16, I-27100 Pavia (Italy); Tolkiehn, Martin [SRXPD Beamline HASYLAB, Deutsches-Elektronen-Synchrotron DESY, Notkestrasse 85, D-22607 Hamburg (Germany); Chaudhary, Anna-Lisa, E-mail: anna-lisa.chaudhary@hzg.de [Institute of Materials Research, Helmholtz-Zentrum Geesthacht, Max-Planck-Straße 1, D-21502 Geesthacht (Germany); Klassen, Thomas; Dornheim, Martin [Institute of Materials Research, Helmholtz-Zentrum Geesthacht, Max-Planck-Straße 1, D-21502 Geesthacht (Germany)

    2015-10-05

    Highlights: • The LiH–MgB{sub 2} system was doped with TiCl{sub 3} and milling conditions varied. • A heuristic model was used to estimate energy transfer from milling conditions. • Milling parameters were correlated with the energy transfer calculation. • 20 kJ g{sup −1} of energy transfer correlates to the optimum conditions for the system. - Abstract: Hydrogen sorption properties of the LiH–MgB{sub 2} system doped with TiCl{sub 3} were investigated with respect to milling conditions (milling times, ball to powder (BTP) ratios, rotation velocities and degrees of filling) to form the reactive hydride composite (RHC) LiBH{sub 4}–MgH{sub 2}. A heuristic model was applied to approximate the energy transfer from the mill to the powders. These results were linked to experimentally obtained quantities such as crystallite size, specific surface area (SSA) and homogeneity of the samples, using X-ray diffraction (XRD), the Brunauer–Emmett–Teller (BET) method and scanning electron microscopy (SEM), respectively. The results show that at approximately 20 kJ g{sup −1} there are no further benefits to the system with an increase in energy transfer. This optimum energy transfer value indicates that a plateau was reached for MgB{sub 2} crystallite size therefore the there was also no improvement of reaction kinetics due to no change in crystallite size. Therefore, this study shows that an optimum energy transfer value was reached for the LiH–MgB{sub 2} system doped with TiCl{sub 3}.

  9. Fabrication of Al/A206–Al2O3 nano/micro composite by combining ball milling and stir casting technology

    International Nuclear Information System (INIS)

    Tahamtan, S.; Halvaee, A.; Emamy, M.; Zabihi, M.S.

    2013-01-01

    Highlights: ► Uniform distribution of alumina particles in molten Al alloy by using MMMC. ► Improvement in wettability of alumina particles with molten Al alloy by using MMMC. ► Porosity content in Al/A206-alumina composite decreased by using MMMC. ► Improvement in tensile strength of Al/A206-alumina composite by using MMMC. ► Decrease in interfacial reaction product by incorporating MMMC in semi-solid state. - Abstract: Al206/5vol.%Al 2 O 3p cast composites were fabricated by the injection of reinforcing particles into molten Al alloy in two different forms, i.e. as Al 2 O 3 particles and milled particulates of alumina with Al and Mg powders. The resultant milled powders (Master Metal Matrix Composite (MMMC)) were then added into the molten Al alloy both in semi-solid state and above liquidus temperature. Effects of powder addition technique, reinforcement particle size and casting temperature on distribution and incorporation of reinforcing particles into molten Al alloy were investigated. Morphology evolution of powders during milling, microscopic examinations of composite and matrix alloy were studied by scanning electron microscopy (SEM). X-ray diffraction (XRD) analysis was also used to determine the possible interaction between powders after ball milling process. Results showed that injection of powders in the form of MMMC leads to considerable improvement in incorporation and distribution of Al 2 O 3p in the Al206 matrix alloy leading to the improvement in tensile properties. Improvement in tensile properties is attributed to the better wetting of Al 2 O 3p by melt as well as removing microchannels and roughness on alumina particles as a consequence of ball milling process

  10. Characterization of oxide layers on amorphous Mg-based alloys by Auger electron spectroscopy with sputter depth profiling

    Energy Technology Data Exchange (ETDEWEB)

    Baunack, S.; Wolff, U. [Leibniz-Institut fuer Festkoerper- und Werkstoffforschung Dresden, Postfach 270016, 01171, Dresden (Germany); Subba Rao, R.V. [Indira Ghandi Centre for Atomic Research, 603 102, Kalpakkam, Tamil Nadu (India)

    2003-04-01

    Amorphous ribbons of Mg-Y-TM-[Ag](TM: Cu, Ni), prepared by melt spinning, were subjected to electrochemical investigations. Oxide layers formed anodically under potentiostatic control in different electrolytes were investigated by AES and sputter depth profiling. Problems and specific features of characterization of the composition of oxide layers and amorphous ternary or quaternary Mg-based alloys have been investigated. In the alloys the Mg(KL{sub 23}L{sub 23}) peak exhibits a different shape compared to that in the pure element. Analysis of the peak of elastically scattered electrons proved the absence of plasmon loss features, characteristic of pure Mg, in the alloy. A different loss feature emerges in Mg(KL{sub 23}L{sub 23}) and Cu(L{sub 23}VV). The system Mg-Y-TM-[Ag] suffers preferential sputtering. Depletion of Mg and enrichment of TM and Y are found. This is attributed mainly to the preferential sputtering of Mg. Thickness and composition of the formed oxide layer depend on the electrochemical treatment. After removing the oxide by sputtering the concentration of the underlying alloy was found to be affected by the treatment. (orig.)

  11. The Effect of Powder Ball Milling on the Microstructure and Mechanical Properties of Sintered Fe-Cr-Mo-Mn-(Cu) Steel

    Science.gov (United States)

    Kulecki, P.; Lichańska, E.

    2017-12-01

    The effect of ball milling powder mixtures of Höganäs pre-alloyed iron Astaloy CrM, low-carbon ferromanganese Elkem, elemental electrolytic Cu and C-UF graphite on the sintered structure and mechanical properties was evaluated. The mixing was conducted using Turbula mixer for 30 minutes and CDI-EM60 frequency inverter for 1 and 2 hours. Milling was performed on 150 g mixtures with (in weight %) CrM + 1% Mn, CrM + 2% Mn, CrM + 1% Mn + 1% Cu and CrM + 2% Mn + 1% Cu, all with 0.6%C. The green compacts were single pressed at 660 MPa according to PN-EN ISO 2740. Sintering was carried out in a laboratory horizontal furnace Carbolite STF 15/450 at 1250°C for 60 minutes in 5%H2 - 95%N2 atmosphere with a heating rate of 75°C/min, followed by sintering hardening at 60°C/min cooling rate. All the steels were characterized by martensitic structures. Mechanical testing revealed that steels based on milled powders have slightly higher mechanical properties compared to those only mixed and sintered. The best combination of mechanical properties, for ball milled CrM + 1% Mn + 1% Cu was UTS 1046 MPa, TRS 1336 MPa and A 1.94%.

  12. Size effect of primary Y{sub 2}O{sub 3} additions on the characteristics of the nanostructured ferritic ODS alloys: Comparing as-milled and as-milled/annealed alloys using S/TEM

    Energy Technology Data Exchange (ETDEWEB)

    Saber, Mostafa, E-mail: msaber@ncsu.edu; Xu, Weizong; Li, Lulu; Zhu, Yuntian; Koch, Carl C.; Scattergood, Ronald O.

    2014-09-15

    The need for providing S/TEM evidence to clarify the mechanisms of nano-scale precipitate formation was the motivation of this investigation. In this study, an Fe–14Cr–0.4Ti alloy was ball-milled with different amounts of Y{sub 2}O{sub 3} content up to 10 wt.%, and then annealed at temperatures up to 1100 °C. Micron-size Y{sub 2}O{sub 3} particles were substituted for the nano-size counterpart to elucidate the mechanism of oxide precipitate formation. The S/TEM studies revealed that the microstructure of the alloy with 10 wt.% yttria contained amorphous undissolved Y{sub 2}O{sub 3} after ball milling, while a small part of the initial oxide particles were dissolved into the solid solution. Consequently, when the amount of yttria was reduced to 1 wt.%, the amorphous phase of the yttria vanished and the whole content of Y{sub 2}O{sub 3} was dissolved into the BCC solid solution. Defect analysis of precipitates on the annealed samples via S/TEM and micro-hardness studies revealed that the use of micron-size primary oxide particles can produce nano-size precipitates, stable up to temperatures as high as 1100 °C, and uniformly distributed throughout the microstructure. This study indicates that the use of high energy ball milling along with micron-size primary oxide particles can lead to nanostructured ferritic ODS alloys without the use of nano-size primary oxide additions.

  13. Grinding arrangement for ball nose milling cutters

    Science.gov (United States)

    Burch, C. F. (Inventor)

    1974-01-01

    A grinding arrangement for spiral fluted ball nose end mills and like tools includes a tool holder for positioning the tool relative to a grinding wheel. The tool is mounted in a spindle within the tool holder for rotation about its centerline and the tool holder is pivotably mounted for angular movement about an axis which intersects that centerline. A follower arm of a cam follower secured to the spindle cooperates with a specially shaped cam to provide rotation of the tool during the angular movement of the tool holder during the grinding cycle, by an amount determined by the cam profile. In this way the surface of the cutting edge in contact with the grinding wheel is maintained at the same height on the grinding wheel throughout the angular movement of the tool holder during the grinding cycle.

  14. Heat generation ability in AC magnetic field of nano MgFe2O4-based ferrite powder prepared by bead milling

    International Nuclear Information System (INIS)

    Hirazawa, Hideyuki; Aono, Hiromichi; Naohara, Takashi; Maehara, Tsunehiro; Sato, Mitsunori; Watanabe, Yuji

    2011-01-01

    Nanosized MgFe 2 O 4 -based ferrite powder having heat generation ability in an AC magnetic field was prepared by bead milling and studied for thermal coagulation therapy applications. The crystal size and the particle size significantly decreased by bead milling. The heat generation ability in an AC magnetic field improved with the milling time, i.e. a decrease in crystal size. However, the heat generation ability decreased for excessively milled samples with crystal sizes of less than 5.5 nm. The highest heat ability (ΔT=34 o C) in the AC magnetic field (370 kHz, 1.77 kA/m) was obtained for fine MgFe 2 O 4 powder having a ca. 6 nm crystal size (the samples were milled for 6-8 h using 0.1 mm φ beads). The heat generation of the samples was closely related to hysteresis loss, a B-H magnetic property. The reason for the high heat generation properties of the samples milled for 6-8 h using 0.1 mm φ beads was ascribed to the increase in hysteresis loss by the formation of a single domain. Moreover, the improvement in heating ability was obtained by calcination of the bead-milled sample at low temperature. In this case, the maximum heat generation (ΔT=41 o C) ability was obtained for a ca. 11 nm crystal size sample was prepared by crystal growth during the sample calcination. On the other hand, the ΔT value for Mg 0.5 Ca 0.5 Fe 2 O 4 was synthesized using a reverse precipitation method decreased by bead milling. - Research Highlights: →The crystal and particle size for MgFe 2 O 4 based ferrite were decreased by bead milling. →The highest heat ability was obtained for MgFe 2 O 4 having a ca. 6 nm crystal size. →This high heat generation ability was ascribed to the increase in hysteresis loss. →Hysteresis loss was increased by the formation of a single domain.

  15. Effects of additive Pd on the structures and electrochemical hydrogen storage properties of Mg{sub 67}Co{sub 33}-based composites or alloys with BCC phase

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yao; Zhuang, Xiangyang [School of Materials Science and Engineering, Southeast University, Nanjing 211189 (China); Zhu, Yunfeng [College of Materials Science and Engineering, Nanjing Tech University, 5 Xinmofan Road, Nanjing 210009 (China); Zhan, Leyu [School of Materials Science and Engineering, Southeast University, Nanjing 211189 (China); Pu, Zhenggan [College of Materials Science and Engineering, Nanjing Tech University, 5 Xinmofan Road, Nanjing 210009 (China); Wan, Neng [SEU-FEI Nano Pico Center, Key Laboratory of MEMS of Ministry of Education, School of Electronics Science and Engineering, Southeast University, Nanjing 210096 (China); Li, Liquan [College of Materials Science and Engineering, Nanjing Tech University, 5 Xinmofan Road, Nanjing 210009 (China)

    2015-02-15

    Highlights: • Additive Pd in Mg{sub 67}Co{sub 33} benefits to form a ternary BCC alloy. • Introducing 5.0 at.% Pd in Mg{sub 67}Co{sub 33} lifts the initial discharge capacity from 10 mAh/g to maximum 530 mAh/g. • Exchange current density was increased due to the homogeneously dispersed Pd. • Additive Pd slightly enhances the hydrogen diffusion coefficient of Mg-Co-Pd composites or alloys. - Abstract: Mg{sub 67}Co{sub 33} and Mg{sub 67}Co{sub 33}-Pd composites/alloys prepared by ball milling for 120 h possess nano-crystalline with body-centered cubic (BCC) structure, which was verified by high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) analyses. The introduced 5.0 at.% Pd significantly lifts the initial discharge capacity from 10 mAh g{sup -1} of Mg{sub 67}Co{sub 33} to maximum 530 mAh g{sup -1}. Pd also drives the Mg{sub 67}Co{sub 33}-Pd composite forming a full BCC alloy during ball milling. The distribution of Pd gradually becomes homogeneous with the augmentation of the ball milling time according to the analyses by scanning electron microscopy-energy dispersive spectrometer (SEM-EDS). Exchange current density increased with the milling time and can be ascribed to the homogeneously dispersion of Pd over the surface. The introduced Pd also enhances the hydrogen diffusion coefficient of the Mg{sub 67}Co{sub 33}-Pd composites/alloys.

  16. First-principles study of crystalline and amorphous AlMgB{sub 14}-based materials

    Energy Technology Data Exchange (ETDEWEB)

    Ivashchenko, V. I.; Shevchenko, V. I., E-mail: shev@materials.kiev.ua [Institute of Problems of Material Science, National Academy of Science of Ukraine, Krzhyzhanosky Str. 3, 03142 Kyiv (Ukraine); Turchi, P. E. A. [Lawrence Livermore National Laboratory (L-352), P.O. Box 808, Livermore, California 94551 (United States); Veprek, S. [Department of Chemistry, Technical University Munich, Lichtenbergstrasse 4, D-85747 Garching (Germany); Leszczynski, Jerzy [Department of Chemistry and Biochemistry, Interdisciplinary Center for Nanotoxicity, Jackson State University, Jackson, Mississippi 39217 (United States); Gorb, Leonid [Department of Chemistry and Biochemistry, Interdisciplinary Center for Nanotoxicity, Jackson State University, Jackson, Mississippi 39217 (United States); Badger Technical Services, LLC, Vicksburg, Mississippi 39180 (United States); Hill, Frances [U.S. Army ERDC, Vicksburg, Mississippi 39180 (United States)

    2016-05-28

    We report first-principles investigations of crystalline and amorphous boron and M1{sub x}M2{sub y}X{sub z}B{sub 14−z} (M1, M2 = Al, Mg, Li, Na, Y; X = Ti, C, Si) phases (so-called “BAM” materials). Phase stability is analyzed in terms of formation energy and dynamical stability. The atomic configurations as well as the electronic and phonon density states of these phases are compared. Amorphous boron consists of distorted icosahedra, icosahedron fragments, and dioctahedra, connected by an amorphous network. The presence of metal atoms in amorphous BAM materials precludes the formation of icosahedra. For all the amorphous structures considered here, the Fermi level is located in the mobility gap independent of the number of valence electrons. The intra-icosahedral vibrations are localized in the range of 800 cm{sup −1}, whereas the inter-icosahedral vibrations appear at higher wavenumbers. The amorphization leads to an enhancement of the vibrations in the range of 1100–1250 cm{sup −1}. The mechanical properties of BAM materials are investigated at equilibrium and under shear and tensile strain. The anisotropy of the ideal shear and tensile strengths is explained in terms of a layered structure of the B{sub 12} units. The strength of amorphous BAM materials is lower than that of the crystalline counterparts because of the partial fragmentation of the boron icosahedra in amorphous structures. The strength enhancement found experimentally for amorphous boron-based films is very likely related to an increase in film density, and the presence of oxygen impurities. For crystalline BAM materials, the icosahedra are preserved during elongation upon tension as well as upon shear in the (010)[100] slip system.

  17. Moessbauer Study of the Ball Milling Disordering Process of FeAl Intermetallic Compounds

    International Nuclear Information System (INIS)

    Oleszak, Dariusz; Bruna, Pere; Crespo, Daniel; Pradell, Trinitat

    2005-01-01

    Structural changes during ball milling of ordered Fe50Al50 intermetallic compounds were studied. X-Ray diffraction allowed the computation of a Long Range Order parameter (LRO) which dropped to zero after a short milling time. The initial B2 ordered structure gradually transforms into a disordered BCC structure, with a final crystallite size of about 25 nm. Moessbauer spectroscopy was used for obtaining a Chemical Short Range Order parameter (CSRO). Using a semiempirical n-body noncentral potential a model of the partially disordered B2 structure was built allowing computing the distribution of Quadrupole Splitting during the disordering process. Comparison between experimental and simulated Moessbauer spectra shows a maximum of disorder in the system for 5h milling, related to the highest value of the lattice spacing and the broader quadrupole hyperfine distribution. However, after milling for times longer than 5h, there is a change on the behavior of the experimental data that cannot be explained by the simple disordering process

  18. High anisotropic NdFeB submicro/nanoflakes prepared by surfactant-assisted ball milling at low temperature

    Science.gov (United States)

    An, Xiaoxin; Jin, Kunpeng; Abbas, Nadeem; Fang, Qiuli; Wang, Fang; Du, Juan; Xia, Weixing; Yan, Aru; Liu, J. Ping; Zhang, Jian

    2017-11-01

    Hard magnetic NdFeB submicro/nanoflakes were successfully prepared by surfactant-assisted ball milling at low temperature (SABMLT) by specially using 2-methyl pentane and trioctylamine (TOA) as solvent and surfactant, respectively. Influences of the amount of TOA and milling temperature on the crystal structure, morphology and magnetic performances of the as-prepared NdFeB powders were investigated systematically. There is significant difference on morphology between the NdFeB powders milled at room and low temperature. The NdFeB powders with flaky morphology could be obtained even with a small amount of TOA by SABMLT, which could not be achieved by surfactant-assisted ball milling at room temperature (SABMRT). The better crystallinity, better grain alignment, higher coercivity, larger saturation magnetization and remanence ratio were achieved in the samples prepared by SABMLT. Furthermore, the final NdFeB powders prepared by SABMLT possessed a lower amount of residual TOA than those prepared by SABMRT. It was demonstrated that SABMLT is a promising way to fabricate rare-earth-transition metal nanoflakes with high anisotropy for permanent magnetic materials. The effective method of preparing NdFeB flakes by lowering temperature will be also useful to fabricate flakes of other functional materials.

  19. Low-power, high-uniform, and forming-free resistive memory based on Mg-deficient amorphous MgO film with rough surface

    Science.gov (United States)

    Guo, Jiajun; Ren, Shuxia; Wu, Liqian; Kang, Xin; Chen, Wei; Zhao, Xu

    2018-03-01

    Saving energy and reducing operation parameter fluctuations remain crucial for enabling resistive random access memory (RRAM) to emerge as a universal memory. In this work, we report a resistive memory device based on an amorphous MgO (a-MgO) film that not only exhibits ultralow programming voltage (just 0.22 V) and low power consumption (less than 176.7 μW) but also shows excellent operative uniformity (the coefficient of variation is only 1.7% and 2.2% for SET and RESET voltage, respectively). Moreover, it also shows a forming-free characteristic. Further analysis indicates that these distinctive properties can be attributed to the unstable local structures and the rough surface of the Mg-deficient a-MgO film. These findings show the potential of using a-MgO in high-performance nonvolatile memory applications.

  20. Influence of Temperature on the Performance of LiNi1/3Co1/3Mn1/3O2 Prepared by High-Temperature Ball-Milling Method

    Directory of Open Access Journals (Sweden)

    Ming Tian

    2018-01-01

    Full Text Available Aiming at the preparation of high electrochemical performance LiNi1/3Co1/3Mn1/3O2 cathode material for lithium-ion battery, LiNi1/3Co1/3Mn1/3O2 was prepared with lithium carbonate, nickel (II oxide, cobalt (II, III oxide, and manganese dioxide as raw materials by high-temperature ball-milling method. Influence of ball-milling temperature was investigated in this work. It was shown that the fine LiNi1/3Co1/3Mn1/3O2 powder with high electrochemical performance can be produced by the high-temperature ball-milling process, and the optimal ball-milling temperature obtained in the current study was 750°C. Its initial discharge capacity was 146.0 mAhg−1 at the rate of 0.1 C, and over 50 cycles its capacity retention rate was 90.2%.

  1. Magnetic Properties of Nanocrystalline FexCu1-x Alloys Prepared by Ball Milling

    International Nuclear Information System (INIS)

    Yousif, A.; Bouziane, K.; Elzain, M. E.; Ren, X.; Berry, F. J.; Widatallah, H. M.; Al Rawas, A.; Gismelseed, A.; Al-Omari, I. A.

    2004-01-01

    X-ray diffraction, Moessbauer and magnetization measurements were used to study Fe x Cu 1-x alloys prepared by ball-milling. The X-ray data show the formation of a nanocrystalline Fe-Cu solid solution. The samples with x≥0.8 and x≤0.5 exhibit bcc or fcc phase, respectively. Both the bcc and fcc phases are principally ferromagnetic for x≥0.2, but the sample with x=0.1 remains paramagnetic down to 78 K. The influence of the local environment on the hyperfine parameters and the local magnetic moment are discussed using calculations based on the discrete-variational method in the local density approximation.

  2. Improved oral bioavailability of probucol by dry media-milling.

    Science.gov (United States)

    Li, Jia; Yang, Yan; Zhao, Meihui; Xu, Hui; Ma, Junyuan; Wang, Shaoning

    2017-09-01

    The polymer/probucol co-milled mixtures were prepared to improve drug dissolution rate and oral bioavailability. Probucol, a BCS II drug, was co-milled together with Copovidone (Kollidon VA64, VA64), Soluplus, or MCC using the dry media-milling process with planetary ball-milling equipment. The properties of the milled mixtures including morphology, crystal form, vitro drug dissolution and in vivo oral bioavailability in rats were evaluated. Probucol existed as an amorphous in the matrix of the co-milled mixtures containing VA64, which helped to enhance drug dissolution. The ternary mixture composed of VA64, RH40, and probucol showed increased dissolution rates in both sink and non-sink conditions. It also had a higher oral bioavailability compared to the reference formulation. Dry-media milling of binary or ternary mixtures composed of drug, polymer and surfactant possibly have wide applications to improve dissolution rate and oral bioavailability of water-insoluble drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Structure and electrochemical hydrogen storage properties of Ti2Ni alloy synthesized by ball milling

    International Nuclear Information System (INIS)

    Hosni, B.; Li, X.; Khaldi, C.; ElKedim, O.; Lamloumi, J.

    2014-01-01

    Highlights: • The Ti 2 Ni alloy activation requires only one cycle of charge and discharge, regardless of the temperature. • By increasing the temperature the capacity loss, undergoes an increase and it is more pronounced for the 60 °C. • A good correlation is found between the evolutions of the different electrochemical parameters according to the temperature. - Abstract: The structure and the electrochemical hydrogen storage properties of amorphous Ti 2 Ni alloy synthesized by ball milling and used as an anode in nickel–metal hydride batteries were studied. Nominal Ti 2 Ni was synthesized under argon atmosphere at room temperature using a planetary high-energy ball mill. The structural and morphological characterization of the amorphous Ti 2 Ni alloy is carried out by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The electrochemical characterization of the Ti 2 Ni electrodes is carried out by the galvanostatic charging and discharging, the constant potential discharge, the open circuit potential and the potentiodynamic polarization techniques. The Ti 2 Ni alloy activation requires only one cycle of charge and discharge, regardless of the temperature. The electrochemical discharge capacity of the Ti 2 Ni alloy, during the first eight cycles, and at a temperature of 30 °C, remained practically unchanged and a good held cycling is observed. By increasing the temperature, the electrochemical discharge capacity loss after eight cycles undergoes an increase and it is more pronounced for the temperature 60 °C. At 30 °C, the anodic corrosion current density is 1 mA cm −2 and then it undergoes a rapid drop, remaining substantially constant (0.06 mA cm −2 ) in the range 40–60 °C, before undergoing a slight increase to 70 °C (0.3 mA cm −2 ). This variation is in good agreement with the maximum electrochemical discharge capacity values found for the different temperatures. By increasing the

  4. Characterization of Amorphous and Co-Amorphous Simvastatin Formulations Prepared by Spray Drying

    Directory of Open Access Journals (Sweden)

    Goedele Craye

    2015-12-01

    Full Text Available In this study, spray drying from aqueous solutions, using the surface-active agent sodium lauryl sulfate (SLS as a solubilizer, was explored as a production method for co-amorphous simvastatin–lysine (SVS-LYS at 1:1 molar mixtures, which previously have been observed to form a co-amorphous mixture upon ball milling. In addition, a spray-dried formulation of SVS without LYS was prepared. Energy-dispersive X-ray spectroscopy (EDS revealed that SLS coated the SVS and SVS-LYS particles upon spray drying. X-ray powder diffraction (XRPD and differential scanning calorimetry (DSC showed that in the spray-dried formulations the remaining crystallinity originated from SLS only. The best dissolution properties and a “spring and parachute” effect were found for SVS spray-dried from a 5% SLS solution without LYS. Despite the presence of at least partially crystalline SLS in the mixtures, all the studied formulations were able to significantly extend the stability of amorphous SVS compared to previous co-amorphous formulations of SVS. The best stability (at least 12 months in dry conditions was observed when SLS was spray-dried with SVS (and LYS. In conclusion, spray drying of SVS and LYS from aqueous surfactant solutions was able to produce formulations with improved physical stability for amorphous SVS.

  5. Characterization of Amorphous and Co-Amorphous Simvastatin Formulations Prepared by Spray Drying.

    Science.gov (United States)

    Craye, Goedele; Löbmann, Korbinian; Grohganz, Holger; Rades, Thomas; Laitinen, Riikka

    2015-12-03

    In this study, spray drying from aqueous solutions, using the surface-active agent sodium lauryl sulfate (SLS) as a solubilizer, was explored as a production method for co-amorphous simvastatin-lysine (SVS-LYS) at 1:1 molar mixtures, which previously have been observed to form a co-amorphous mixture upon ball milling. In addition, a spray-dried formulation of SVS without LYS was prepared. Energy-dispersive X-ray spectroscopy (EDS) revealed that SLS coated the SVS and SVS-LYS particles upon spray drying. X-ray powder diffraction (XRPD) and differential scanning calorimetry (DSC) showed that in the spray-dried formulations the remaining crystallinity originated from SLS only. The best dissolution properties and a "spring and parachute" effect were found for SVS spray-dried from a 5% SLS solution without LYS. Despite the presence of at least partially crystalline SLS in the mixtures, all the studied formulations were able to significantly extend the stability of amorphous SVS compared to previous co-amorphous formulations of SVS. The best stability (at least 12 months in dry conditions) was observed when SLS was spray-dried with SVS (and LYS). In conclusion, spray drying of SVS and LYS from aqueous surfactant solutions was able to produce formulations with improved physical stability for amorphous SVS.

  6. A co-production of sugars, lignosulfonates, cellulose, and cellulose nanocrystals from ball-milled woods.

    Science.gov (United States)

    Du, Lanxing; Wang, Jinwu; Zhang, Yang; Qi, Chusheng; Wolcott, Michael P; Yu, Zhiming

    2017-08-01

    This study demonstrated the technical potential for the large-scale co-production of sugars, lignosulfonates, cellulose, and cellulose nanocrystals. Ball-milled woods with two particle sizes were prepared by ball milling for 80min or 120min (BMW 80 , BMW 120 ) and then enzymatically hydrolyzed. 78.3% cellulose conversion of BMW 120 was achieved, which was three times as high as the conversion of BMW 80 . The hydrolyzed residues (HRs) were neutrally sulfonated cooking. 57.72g/L and 88.16g/L lignosulfonate concentration, respectively, were harvested from HR 80 and HR 120 , and 42.6±0.5% lignin were removed. The subsequent solid residuals were purified to produce cellulose and then this material was acid-hydrolyzed to produce cellulose nanocrystals. The BMW 120 maintained smaller particle size and aspect ratio during each step of during the multiple processes, while the average aspect ratio of its cellulose nanocrystals was larger. The crystallinity of both materials increased with each step of wet processing, reaching to 74% for the cellulose. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Hydrophilic functionalized silicon nanoparticles produced by high energy ball milling

    Science.gov (United States)

    Hallmann, Steffen

    The mechanochemical synthesis of functionalized silicon nanoparticles using High Energy Ball Milling (HEBM) is described. This method facilitates the fragmentation of mono crystalline silicon into the nanometer regime and the simultaneous surface functionalization of the formed particles. The surface functionalization is induced by the reaction of an organic liquid, such as alkynes and alkenes with reactive silicon sites. This method can be applied to form water soluble silicon nanoparticles by lipid mediated micelle formation and the milling in organic liquids containing molecules with bi-functional groups, such as allyl alcohol. Furthermore, nanometer sized, chloroalkyl functionalized particles can be synthesized by milling the silicon precursor in the presence of an o-chloroalkyne with either alkenes or alkynes as coreactants. This process allows tuning of the concentration of the exposed, alkyl linked chloro groups, simply by varying the relative amounts of the coreactant. The silicon nanoparticles that are formed serve as the starting point for a wide variety of chemical reactions, which may be used to alter the surface properties of the functionalized nanoparticles. Finally, the use of functionalized silicon particles for the production of superhydrophobic films is described. Here HEBM proves to be an efficient method to produce functionalized silicon particles, which can be deposited to form a stable coating exhibiting superhydrophobic properties. The hydrophobicity of the silicon film can be tuned by the milling time and thus the resulting surface roughness of the films.

  8. Improved critical current densities in bulk FeSe superconductor using ball milled powders and high temperature sintering

    Energy Technology Data Exchange (ETDEWEB)

    Muralidhar, M.; Furutani, K.; Murakami, M. [Graduate School of Science and Engineering, Superconducting Materials Laboratory, Shibaura Institute of Technology, Tokyo (Japan); Kumar, Dinesh; Rao, M.S. Ramachandra [Department of Physics, Nano Functional Materials Technology Centre and Materials Science Research Centre, Indian Institute of Technology Madras, Chennai (India); Koblischka, M.R. [Institute of Experimental Physics, Saarland University, Saarbruecken (Germany)

    2016-12-15

    The present study is investigating the effect of high temperature sintering combined with ball milled powders for the preparation of FeSe material via solid state sintering technique. The commercial powders of Fe (99.9% purity) and Se (99.9% purity) were mixed in a nominal ratio Fe:Se = 1:1 and thoroughly ground and ball-milled in a glove box during 6 h. Then, the powder mixture was pressed into pellets of 5 mm in diameter and 2 mm thickness using an uniaxial pressure of 100 MPa. The samples were sealed in quartz tubes and sintered at 600 C for 24 h. Then, the pellets were again thoroughly ground and ball-milled in the glove box and pressed into pellets, and the final sintering was performed at two different temperatures, namely at 900 C for 24 h and at 950 C for 24 h. X-ray diffraction results confirmed that both samples showed mainly of the β-FeSe with tetragonal structure. The temperature dependence of magnetization (M-T) curves revealed a sharp superconducting transition T{sub c,} {sub onset} = 8.16 K for the sample sintered at 900 C. Further, scanning electron microscopy observations proved that samples sintered at 900 C show a platelike grain structure with high density. As a result, improved irreversibility fields around 5 T and the critical current density (J{sub c}) values of 6252 A cm{sup -2} at 5 K and self-field are obtained. Furthermore, the normalized volume pinning force versus the reduced field plots indicated a peak position at 0.4 for the sample sintered at 900 C. Improved flux pinning and the high J{sub c} values are attributed to the textured microstructure of the material, produced by a combination of high temperature sintering and ball milling. (copyright 2016 The Authors. Phys. Status Solidi A published by WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Mechanochemical Synthesis of Nanostructured MgXNi1-XO Compound by Mg-NiO Mixture

    Directory of Open Access Journals (Sweden)

    Nader Setoudeh

    2017-06-01

    Full Text Available Synthesis of magnesium nickel oxide phase such as MgxNi1-xO solid solutions has been studied in this research article using mechnochmical reaction between magnesium and nickel oxide. Mixtures of magnesium powder and nickel oxide (Mg+NiO with stoichiometric compositions were milled for different times in a planetary ball mill. Reduction reaction of nickel oxide by magnesium via a mechanically induced self-sustaining reaction (MSR was confirmed in the XRD measurements of the as-milled samples. Formation of nanostructured magnesium nickel oxide phases (such as Mg0.4Ni0.6O or MgNiO2 was observed after isothermal heating of the 30 minutes milled samples at 1000°C where nickel phase seems to disappear in XRD patterns. The traces of phases such as Mg0.4Ni0.6O or MgNiO2 were also observed in the as-milled mixtures. Therefore, the XRD results of the as-milled samples suggested that the formation of magnesium nickel oxide phases could be possible even after prolonged milling. The XRD and SEM results of both as-milled and isothermally heated samples indicated that the crystallite size and particle size of the final products reached to nanoscale after milling. Morphological and compositional evolution of the samples after heat treatment was monitored through SEM imaging and elemental analyses. The results confirmed that the composition of final product is close to Mg0.4Ni0.6O compound.

  10. Microstructures, Mechanical Properties and Thermal Conductivities of W-0.5 wt.%TiC Alloys Prepared via Ball Milling and Wet Chemical Method

    Science.gov (United States)

    Lang, Shaoting; Yan, Qingzhi; Sun, Ningbo; Zhang, Xiaoxin; Ge, Changchun

    2017-10-01

    Two kinds of W-0.5 wt.%TiC alloys were prepared, one by ball milling and the other by the wet chemical method. For comparison, pure tungsten powders were chemically prepared and sintered by the same process. The microstructures, mechanical properties and thermal conductivities of the prepared samples were characterized. It has been found that the wet chemical method resulted in finer sizes and more uniform distribution of TiC particles in the sintered tungsten matrix than the ball milling method. The W-TiC alloy prepared by the wet chemical method achieved the highest bending strength (1065.72 MPa) among the samples. Further, it also exhibited obviously higher thermal conductivities in the temperature range of room temperature to 600°C than did the W-TiC alloy prepared by ball milling, but the differences in their thermal conductivities could be ignored in the range of 600-800°C.

  11. Amorphization of Fe-based alloy via wet mechanical alloying assisted by PCA decomposition

    Energy Technology Data Exchange (ETDEWEB)

    Neamţu, B.V., E-mail: Bogdan.Neamtu@stm.utcluj.ro [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 103-105, Muncii Avenue, 400641, Cluj-Napoca (Romania); Chicinaş, H.F.; Marinca, T.F. [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 103-105, Muncii Avenue, 400641, Cluj-Napoca (Romania); Isnard, O. [Université Grenoble Alpes, Institut NEEL, F-38042, Grenoble (France); CNRS, Institut NEEL, 25 rue des martyrs, BP166, F-38042, Grenoble (France); Pană, O. [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath Street, 400293, Cluj-Napoca (Romania); Chicinaş, I. [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 103-105, Muncii Avenue, 400641, Cluj-Napoca (Romania)

    2016-11-01

    Amorphization of Fe{sub 75}Si{sub 20}B{sub 5} (at.%) alloy has been attempted both by wet and dry mechanical alloying starting from a mixture of elemental powders. Powder amorphization was not achieved even after 140 hours of dry mechanical alloying. Using the same milling parameters, when wet mechanical alloying was used, the powder amorphization was achieved after 40 h of milling. Our assumption regarding the powder amorphization capability enhancement by contamination with carbon was proved by X-ray Photoelectron Spectroscopy (XPS) measurements which revealed the presence of carbon in the chemical composition of the wet mechanically alloyed sample. Using shorter milling times and several process control agents (PCA) (ethanol, oleic acid and benzene) with different carbon content it was proved that the milling duration required for powder amorphization is linked to the carbon content of the PCA. Differential Scanning Calorimetry (DSC), thermomagnetic (TG) and X-ray Diffraction (XRD) measurements performed to the heated samples revealed the fact that, the crystallisation occurs at 488 °C, thus leading to the formation of Fe{sub 3}Si and Fe{sub 2}B. Thermogravimetry measurements performed under H{sub 2} atmosphere, showed the same amount of contamination with C, which is about 2.3 wt%, for the amorphous samples regardless of the type of PCA. Saturation magnetisation of the wet milled samples decreases upon increasing milling time. In the case of the amorphous samples wet milled with benzene up to 20 h and with oleic acid up to 30 h, the saturation magnetisation has roughly the same value, indicating the same degree of contamination. The XRD performed on the samples milled using the same parameters, revealed that powder amorphization can be achieved even via dry milling, just by adding the equivalent amount of elemental C calculated from the TG plots. This proves that in this system by considering the atomic species which can contaminate the powder, they can be

  12. Catalytic effect of halide additives ball milled with magnesium hydride

    Energy Technology Data Exchange (ETDEWEB)

    Malka, I.E.; Bystrzycki, J. [Department of Advanced Materials and Technologies, Military University of Technology, Kaliskiego 2, 00-908 Warsaw (Poland); Czujko, T. [Department of Advanced Materials and Technologies, Military University of Technology, Kaliskiego 2, 00-908 Warsaw (Poland); CanmetENERGY, Hydrogen Fuel Cells and Transportation Energy, Natural Resources (Canada)

    2010-02-15

    The influence of various halide additives milled with magnesium hydride (MgH{sub 2}) on its decomposition temperature was studied. The optimum amount of halide additive and milling conditions were evaluated. The MgH{sub 2} decomposition temperature and energy of activation reduction were measured by temperature programmed desorption (TPD) and differential scanning calorimetry (DSC). The difference in catalytic efficiency between chlorides and fluorides of the various metals studied is presented. The effects of oxidation state, valence and position in the periodic table for selected halides on MgH{sub 2} decomposition temperature were also studied. The best catalysts, from the halides studied, for magnesium hydride decomposition were ZrF{sub 4}, TaF{sub 5}, NbF{sub 5}, VCl{sub 3} and TiCl{sub 3}. (author)

  13. Conductometry and Size Characterization of Polypyrrole Nanoparticles Produced by Ball Milling

    OpenAIRE

    Abbasi, Abdul Malik Rehan; Marsalkova, Miroslava; Militky, Jiri

    2013-01-01

    Polypyrrole (PPy), one of the most extensively investigated conducting polymers, has attracted a great deal of interest because of its good electrical conductivity, environmental stability, and easy synthesis. PPy films were produced by polymerization of pyrrole and tosylate (TsO−) as dopants in the presence of oxidant FeCl3 and polyethylene glycol (Mw 8000) at −5°C for 48 h. High energy milling was carried out at 850 rpm in the dry media with the balls of 10 mm. Particles were then character...

  14. Influence of variation in molar ratio on co-amorphous drug-amino acid systems

    DEFF Research Database (Denmark)

    Jensen, Katrine Birgitte Tarp; Larsen, Flemming Hofmann; Löbmann, Korbinian

    2016-01-01

    Molecular interactions were investigated within four different co-amorphous drug-amino acid systems, namely indomethacin-tryptophan (Ind-Trp), furosemide-tryptophan (Fur-Trp), indomethacin-arginine (Ind-Arg) and furosemide-arginine (Fur-Arg). The co-amorphous systems were prepared by ball milling...... observed in the 50mol% drug (1:1M ratio) mixtures, with the exception of co-amorphous Ind-Arg where the interactions within the 40mol% drug samples appear equally strong. A particularly large deviation between the theoretical and actual Tgs was observed within co-amorphous Ind-Arg and Fur-Arg systems......-amorphous mixture without additional interactions. The modified equation described the Tgs of the co-amorphous Ind-Arg with excess Arg less well indicating possible further interactions; however, the FTIR and ssNMR data did not support the presence of additional intermolecular drug-amino acid interactions....

  15. Synthesis of Amorphous Powders of Ni-Si and Co-Si Alloys by Mechanical Alloying

    Science.gov (United States)

    Omuro, Keisuke; Miura, Harumatsu

    1991-05-01

    Amorphous powders of the Ni-Si and Co-Si alloys are synthesized by mechanical alloying (MA) from crystalline elemental powders using a high energy ball mill. The alloying and amorphization process is examined by X-ray diffraction, differential scanning calorimetry (DSC), and scanning electron microscopy. For the Ni-Si alloy, it is confirmed that the crystallization temperature of the MA powder, measured by DSC, is in good agreement with that of the powder sample prepared by mechanical grinding from the cast alloy ingot products of the same composition.

  16. Bulk amorphous Mg-based alloys

    DEFF Research Database (Denmark)

    Pryds, Nini

    2004-01-01

    are discussed in this paper. On the basis of these measurements phase diagrams of the different systems were constructed. Finally, it is demonstrated that when pressing the bulk amorphous alloy onto a metallic dies at temperatures within the supercooled liquid region, the alloy faithfully replicates the surface...

  17. Hydroamination reactions of alkynes with ortho-substituted anilines in ball mills: synthesis of benzannulated N-heterocycles by a cascade reaction.

    Science.gov (United States)

    Weiße, Maik; Zille, Markus; Jacob, Katharina; Schmidt, Robert; Stolle, Achim

    2015-04-20

    It was demonstrated that ortho-substituted anilines are prone to undergo hydroamination reactions with diethyl acetylenedicarboxylate in a planetary ball mill. A sequential coupling of the intermolecular hydroamination reaction with intramolecular ring closure was utilized for the syntheses of benzooxazines, quinoxalines, and benzothiazines from readily available building blocks, that is, electrophilic alkynes and anilines with OH, NH, or SH groups in the ortho position. For the heterocycle formation, it was shown that several stress conditions were able to initiate the reaction in the solid state. Processing in a ball mill seemed to be advantageous over comminution with mortar and pestle with respect to process control. In the latter case, significant postreaction modification occurred during solid-state analysis. Cryogenic milling proved to have an adverse effect on the molecular transformation of the reagents. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. A vertical ball mill as a new reactor design for biomass hydrolysis and fermentation process

    DEFF Research Database (Denmark)

    de Assis Castro, Rafael Cunha; Mussatto, Solange I.; Conceicao Roberto, Inês

    2017-01-01

    A vertical ball mill (VBM) reactor was evaluated for use in biomass conversion processes. The effects of agitation speed (100–200 rpm), number of glass spheres (0–30 units) and temperature (40–46 °C) on enzymatic hydrolysis of rice straw and on glucose fermentation by a thermotolerant Kluyveromyces...

  19. Development of MgB2 superconductor wire with high critical current

    International Nuclear Information System (INIS)

    Kim, Chan Joong; Jun, Byung Hyuk; Park, Soon Dong; Kim, Nam Kyu; Kim, Yi Jeong; Yi, Ji Hye; Lee, Ji Hyun; Tan, Kai Sin

    2009-07-01

    The MgB 2 superconductor with smaller grain size could improve its critical properties by providing flux pinning centers with high grain boundary density. The effects of C doping such as charcoal, paper ash and glycerin on the superconducting properties was investigated for in situ processed MgB 2 samples using low purity semi-crystalline B powder. The results show a decrease in Tc and an enhancement of Jc at high fields for the C-doped samples as compared to the un-doped samples. A combined process of a mechanical ball milling and liquid glycerin (C 3 H 8 O 3 ) treatment of B powder has been conducted to enhance the superconducting properties of MgB 2 . The mechanical ball milling was effective for grain refinement, and a lattice disorder was easily achieved by glycerin addition. With the combined process, the critical properties was further increased due to a higher grain boundary density and a greater C substitution. To get fine grain structure of MgB 2 with high critical current properties, mechanical milling for as-received B powder and low temperature solid-state reaction of 550 or 600 .deg. C were attempted to in situ powder-in-tube processed MgB 2 /Fe wires. The critical current properties of the MgB 2 wires using the milled B powder were enhanced due to a smaller grain size and an increased volume of the superconducting phase. The solid-state reaction of a low temperature process for the samples using the milled B powder resulted in a poorer crystallinity with a smaller grain size, which improved superconducting properties. We established the system to measure the transport current properties of the MgB 2 wires. The field dependence of the transport Jc was evaluated for the MgB 2 wires heat-treated at different heat treatment conditions using ball-milled and glycerin-treated B powder. The MgB 2 magnet was developed and the AC loss of MgB 2 wire was also investigated. A conduction cooling device to cool the MgB 2 coil down to 4 K has been fabricated and the

  20. Structure and electrochemical hydrogen storage properties of Ti{sub 2}Ni alloy synthesized by ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Hosni, B. [Equipe des Hydrures Métalliques, Laboratoire de Mécanique, Matériaux et Procédés, Ecole Nationale Supérieure d’Ingénieurs de Tunis, ENSIT Ex ESSTT, Université de Tunis, 5 Avenue Taha Hussein, 1008 Tunis (Tunisia); Li, X. [FEMTO-ST, MN2S, Université de Technologie de Belfort-Montbéliard, Site de Sévenans, 90010 Belfort cedex (France); Khaldi, C., E-mail: chokri.khaldi@esstt.rnu.tn [Equipe des Hydrures Métalliques, Laboratoire de Mécanique, Matériaux et Procédés, Ecole Nationale Supérieure d’Ingénieurs de Tunis, ENSIT Ex ESSTT, Université de Tunis, 5 Avenue Taha Hussein, 1008 Tunis (Tunisia); ElKedim, O. [FEMTO-ST, MN2S, Université de Technologie de Belfort-Montbéliard, Site de Sévenans, 90010 Belfort cedex (France); Lamloumi, J. [Equipe des Hydrures Métalliques, Laboratoire de Mécanique, Matériaux et Procédés, Ecole Nationale Supérieure d’Ingénieurs de Tunis, ENSIT Ex ESSTT, Université de Tunis, 5 Avenue Taha Hussein, 1008 Tunis (Tunisia)

    2014-12-05

    Highlights: • The Ti{sub 2}Ni alloy activation requires only one cycle of charge and discharge, regardless of the temperature. • By increasing the temperature the capacity loss, undergoes an increase and it is more pronounced for the 60 °C. • A good correlation is found between the evolutions of the different electrochemical parameters according to the temperature. - Abstract: The structure and the electrochemical hydrogen storage properties of amorphous Ti{sub 2}Ni alloy synthesized by ball milling and used as an anode in nickel–metal hydride batteries were studied. Nominal Ti{sub 2}Ni was synthesized under argon atmosphere at room temperature using a planetary high-energy ball mill. The structural and morphological characterization of the amorphous Ti{sub 2}Ni alloy is carried out by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The electrochemical characterization of the Ti{sub 2}Ni electrodes is carried out by the galvanostatic charging and discharging, the constant potential discharge, the open circuit potential and the potentiodynamic polarization techniques. The Ti{sub 2}Ni alloy activation requires only one cycle of charge and discharge, regardless of the temperature. The electrochemical discharge capacity of the Ti{sub 2}Ni alloy, during the first eight cycles, and at a temperature of 30 °C, remained practically unchanged and a good held cycling is observed. By increasing the temperature, the electrochemical discharge capacity loss after eight cycles undergoes an increase and it is more pronounced for the temperature 60 °C. At 30 °C, the anodic corrosion current density is 1 mA cm{sup −2} and then it undergoes a rapid drop, remaining substantially constant (0.06 mA cm{sup −2}) in the range 40–60 °C, before undergoing a slight increase to 70 °C (0.3 mA cm{sup −2}). This variation is in good agreement with the maximum electrochemical discharge capacity values found for the

  1. Production and properties of light-metal base amorphous alloys

    International Nuclear Information System (INIS)

    Inoue, Akihisa; Masumoto, Tsuyoshi

    1993-01-01

    Light-metal base alloys with high specific strength and good corrosion resistance were produced through amorphization of Al and Mg-based alloys. The amorphous phase is formed in rapidly solidified Al-TM-Ln and Mg-TM-Ln (TM=transition metal, Ln=lanthanide metal) alloys. The highest tensile strength (σ f ) reaches 1,330 MPa for the Al base and 830 MPa for the Mg base. Furthermore, the Mg-based alloys have a large glass-forming capacity which enables to produce an amorphous phase by a metallic mold casting method. The extrusion of the Al-based amorphous powders at temperatures above crystallization temperature caused the formation of high strength materials with finely mixed structure consisting of dispersed intermetallic compounds in an Al matrix. The highest values of σ f and fatigue limit are as high as 940 and 313 MPa, respectively, at room temperature and 520 and 165 MPa at 473 K. The extruded Al-Ni-Mm alloy has already been used as machine parts and subsequent further development as practical materials is expected by taking these advantages

  2. Biodistribution of nanoparticles of hydrophobic gadopentetic-acid derivative prepared with a planetary ball mill for neutron-capture therapy of cancer

    International Nuclear Information System (INIS)

    Nabeta, Chika; Ichikawa, Hideki; Fukumori, Yoshinobu

    2006-01-01

    Nanoparticles of hydrophobic gadopentetic-acid derivatives (Gd-nanoGR) were prepared with a wet ball-milling process for gadolinium neutron-capture therapy. Ball-milling of solid mass of gadopentetic acid distearylamide with soybean lecithin as a dispersant in the presence of water and subsequent sonication at 70degC resulted in the Gd-nanoGR with the particle size of 63 nm. Biodistribution study using melanoma-bearing hamsters demonstrated that the i.v. injection of the Gd-nanoGR made a higher gadolinium accumulation in tumor (109 μg Gd/g wet tumor at 6h after administration), when compared with the gadolinium-loaded micellar-like nanoparticles previously reported. (author)

  3. Thermodynamics, kinetics, and catalytic effect of dehydrogenation from MgH2 stepped surfaces and nanocluster: a DFT study

    Science.gov (United States)

    Reich, Jason; Wang, Linlin; Johnson, Duane

    2013-03-01

    We detail the results of a Density Functional Theory (DFT) based study of hydrogen desorption, including thermodynamics and kinetics with(out) catalytic dopants, on stepped (110) rutile and nanocluster MgH2. We investigate competing configurations (optimal surface and nanoparticle configurations) using simulated annealing with additional converged results at 0 K, necessary for finding the low-energy, doped MgH2 nanostructures. Thermodynamics of hydrogen desorption from unique dopant sites will be shown, as well as activation energies using the Nudged Elastic Band algorithm. To compare to experiment, both stepped structures and nanoclusters are required to understanding and predict the effects of ball milling. We demonstrate how these model systems relate to the intermediary sized structures typically seen in ball milling experiments.

  4. Synthesis of Cu(In,Ga)Se{sub 2} crystals using a crank ball mill

    Energy Technology Data Exchange (ETDEWEB)

    Yamada, Suzuka; Noji, Hideki; Akaki, Yoji [Miyakonojo National College of Technology, 473-1 Yoshio, Miyakonojo Miyazaki 885-8567 (Japan); Okamoto, Tomoichiro [Nagaoka University of Technology, 1603-1 Kamitomioka, Nagaoka, Niigata 940-2188 (Japan)

    2015-06-15

    Cu(In,Ga)Se{sub 2} (CIGS) crystals were synthesized by a mechanochemical (MC) process using a crank ball mill. The molar ratios of starting materials were Cu:In:Ga:Se=1:1-x:x:2 (0≤x≤1) and Cu:In:Ga:Se=1:0.7:0.3:y (2≤y≤3). The reaction time reduced with decreasing Se and Ga molar ratios. The collection rate decreased with longer reaction times. From XRD patterns, we confirmed that the CuInSe{sub 2} and/or CuGaSe{sub 2}crystals were successfully grown when the powders reacted. Although the crystals grown with a selenium molar ration of 2 were Se-poor, those grown at a molar ratio of 3 were Se-rich. When Se increasing molar ratio, Cu, In, and Ga were away from the stoichiometric. With a molar ratio of Cu:In:Ga:Se=1:0.7:0.3:2.5∝2.7, their composition became stoichiometric. Crystal morphology was varied. CIGS crystals were thus successfully synthesized using a crank ball mill. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  5. Integrated modeling and analysis of ball screw feed system and milling process with consideration of multi-excitation effect

    Science.gov (United States)

    Zhang, Xing; Zhang, Jun; Zhang, Wei; Liang, Tao; Liu, Hui; Zhao, Wanhua

    2018-01-01

    The present researches about feed drive system and milling process are almost independent with each other, and ignore the interaction between the two parts, especially the influence of nonideal motion of feed drive system on milling process. An integrated modeling method of ball screw feed system and milling process with multi-excitation effect is proposed in this paper. In the integrated model, firstly an analytical model of motor harmonic torque with consideration of asymmetrical drive circuit and asymmetrical permanent magnet is given. Then, the numerical simulation procedure of cutter/workpiece engagement during milling process with displacement fluctuation induced by harmonic torque is put forward, which is followed by the solving flow for the proposed integrated model. Based on the integrated model, a new kind of quality defect shown as contour low frequency oscillation on machined surface is studied by experiments and simulations. The results demonstrate that the forming mechanism of the contour oscillation can be ascribed to the multi-excitation effect with motor harmonic torque and milling force. Moreover, the influence of different milling conditions on the contour oscillation characteristics, particularly on surface roughness, are further discussed. The results indicate that it is necessary to explain the cause of the new kind of quality defect with a view of system integration.

  6. Generation of drugs coated iron nanoparticles through high energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Radhika Devi, A.; Murty, B. S. [Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600036 (India); Chelvane, J. A. [Defence Metallurgical Research Laboratory, Hyderabad 500058 (India); Prabhakar, P. K.; Padma Priya, P. V.; Doble, Mukesh [Department of Biotechnology, Indian Institute of Technology Madras, Chennai 600036 (India)

    2014-03-28

    The iron nanoparticles coated with oleic acid and drugs such as folic acid/Amoxicillin were synthesized by high energy ball milling and characterized by X-ray diffraction, Transmission electron microscope, zeta potential, dynamic light scattering, Fourier Transform Infra red (FT-IR) measurements, and thermo gravimetric analysis (TGA). FT-IR and TGA measurements show good adsorption of drugs on oleic acid coated nanoparticles. Magnetic measurements indicate that saturation magnetization is larger for amoxicillin coated particles compared to folic acid coated particles. The biocompatibility of the magnetic nanoparticles prepared was evaluated by in vitro cytotoxicity assay using L929 cells as model cells.

  7. Controlling the number of walls in multi walled carbon nanotubes/alumina hybrid compound via ball milling of precipitate catalyst

    Energy Technology Data Exchange (ETDEWEB)

    Nosbi, Norlin [School of Materials and Mineral Resources Engineering, Engineering Campus, Universiti Sains Malaysia (USM), 14300 Nibong Tebal, Seberang Perai Selatan, Pulau Pinang (Malaysia); Akil, Hazizan Md, E-mail: hazizan@usm.my [School of Materials and Mineral Resources Engineering, Engineering Campus, Universiti Sains Malaysia (USM), 14300 Nibong Tebal, Seberang Perai Selatan, Pulau Pinang (Malaysia); Cluster for Polymer Composite (CPC), Science and Engineering Research Centre, Engineering Campus, Universiti Sains Malaysia (USM), 14300 Nibong Tebal, Seberang Perai Selatan, Pulau Pinang (Malaysia)

    2015-06-15

    Graphical abstract: - Highlights: • We report that, to manipulate carbon nanotubes geometry and number of walls are by controlling the precipitate catalyst size. • Number of walls and geometry effects depend on the milling time of the precipitate catalyst. • Increasing milling of time will decrease the carbon nanotubes number of walls. • Increasing milling of time will increase the carbon nanotubes thermal conductivity. - Abstract: This paper reports the influence of milling time on the structure and properties of the precipitate catalyst of multi walled carbon nanotubes (MWCNT)/alumina hybrid compound, produced through the chemical vapour deposition (CVD) process. For this purpose, light green precipitate consisted of aluminium, nickel(II) nitrate hexahydrate and sodium hydroxide mixture was placed in a planetary mill equipped with alumina vials using alumina balls at 300 rpm rotation speed for various milling time (5–15 h) prior to calcinations and CVD process. The compound was characterized using various techniques. Based on high-resolution transmission electron microscopy analysis, increasing the milling time up to 15 h decreased the diameter of MWCNT from 32.3 to 13.1 nm. It was noticed that the milling time had a significant effect on MWCNT wall thickness, whereby increasing the milling time from 0 to 15 h reduced the number of walls from 29 to 12. It was also interesting to note that the carbon content increased from 23.29 wt.% to 36.37 wt.% with increasing milling time.

  8. Methods of amorphization and investigation of the amorphous state

    OpenAIRE

    EINFALT, TOMAŽ; PLANINŠEK, ODON; HROVAT, KLEMEN

    2013-01-01

    The amorphous form of pharmaceutical materials represents the most energetic solid state of a material. It provides advantages in terms of dissolution rate and bioavailability. This review presents the methods of solid-state amorphization described in literature (supercooling of liquids, milling, lyophilization, spray drying, dehydration of crystalline hydrates), with the emphasis on milling. Furthermore, we describe how amorphous state of pharmaceuticals differ depending on method of prepara...

  9. Moessbauer spectroscopy study of the synthesis of SnFe2O4 by high energy ball milling (HEBM) of SnO and α-Fe2O3

    International Nuclear Information System (INIS)

    Uwakweh, Oswald N C; Perez Moyet, Richard; Mas, Rita; Morales, Carolyn; Vargas, Pedro; Silva, Josue; Rossa, Angel; Lopez, Neshma

    2010-01-01

    The formation of single phase nanoparticles of spinel structured ferrite, SnFe 2 O 4 , by mechanochemical syntheses using HEBM of stoichiometric amounts of solid SnO and α-Fe 2 O 3 with acetone as surfactant was achieved progressively as function of ball milling time. Single phase SnFe 2 O 4 formation commenced from five hours of continuous ball milling, and reached completion after 22 hours, thereby yielding a material with a lattice parameter of 8.543 A, and particle size of 10.91 nm. The coercivity was 4.44 mT, magnetic saturation value of 17.75 Am 2 /kg, and remanent magnetizations of 1.50 Am 2 /kg, correspondingly. The nanosized particles exhibited superparamagnetic behavior phenomenon based on Moessbauer spectroscopy measurements. The kinetic analyses based on the modified Kissinger method yielded four characteristic stages during the thermal evolution of the 22 hours milled state with activation energies of 0.23 kJ/mol, 2.52 kJ/mol, 0.024 kJ/mol, and 1.57 kJ/mol respectively.

  10. Nanocrystalline FeSiBNbCu alloys: Differences between mechanical and thermal crystallization process in amorphous precursors

    International Nuclear Information System (INIS)

    Lopez, M.; Marin, P.; Agudo, P.; Carabias, I.; Venta, J. de la; Hernando, A.

    2007-01-01

    Nanocrystalline magnetic particles obtained by high energy ball milling of FeSiBNbCu alloy were prepared from rapidly quenched ribbons as a starting material. Structural characterization was made by using X-ray diffraction (XRD), differential scanning calorimetry (DSC), atomic force microscopy (AFM) and Moessbauer spectroscopy. The structural changes observed in this amorphous material suggest that nanocrystallization process takes place in a different way from the one induced by thermal treatments. Our different studies reveals that after short grinding times (up to 40 h) the material is composed by a two phase system of very fine nanocrystals embedded in a residual amorphous phase, while for largest periods of milling (from 140 h) the sample consists of a very fine nanocrystalline phase with a large fraction of grain boundary

  11. Hot Melt Extrusion and Spray Drying of Co-amorphous Indomethacin-Arginine With Polymers

    DEFF Research Database (Denmark)

    Lenz, Elisabeth; Löbmann, Korbinian; Rades, Thomas

    2017-01-01

    Co-amorphous drug-amino acid systems have gained growing interest as an alternative to common amorphous formulations which contain polymers as stabilizers. Several preparation methods have recently been investigated, including vibrational ball milling on a laboratory scale or spray drying......, and stability. Results were compared to those of spray-dried formulations with the same compositions and to spray-dried indomethacin-copovidone. Overall, stable co-amorphous systems could be prepared by extrusion without or with copovidone, which exhibited comparable molecular interaction properties...... to the respective spray-dried products, while phase separation was detected by differential scanning calorimetry in several cases. The formulations containing indomethacin in combination with arginine and copovidone showed enhanced dissolution behavior over the formulations with only copovidone or arginine....

  12. Enhanced Physical Stability of Amorphous Drug Formulations via Dry Polymer Coating.

    Science.gov (United States)

    Capece, Maxx; Davé, Rajesh

    2015-06-01

    Although amorphous solid drug formulations may be advantageous for enhancing the bioavailability of poorly soluble active pharmaceutical ingredients, they exhibit poor physical stability and undergo recrystallization. To address this limitation, this study investigates stability issues associated with amorphous solids through analysis of the crystallization behavior for acetaminophen (APAP), known as a fast crystallizer, using a modified form of the Avrami equation that kinetically models both surface and bulk crystallization. It is found that surface-enhanced crystallization, occurring faster at the free surface than in the bulk, is the major impediment to the stability of amorphous APAP. It is hypothesized that a novel use of a dry-polymer-coating process referred to as mechanical-dry-polymer-coating may be used to inhibit surface crystallization and enhance stability. The proposed process, which is examined, simultaneously mills and coats amorphous solids with polymer, while avoiding solvents or solutions, which may otherwise cause stability or crystallization issues during coating. It is shown that solid dispersions of APAP (64% loading) with a small particle size (28 μm) could be prepared and coated with the polymer, carnauba wax, in a vibratory ball mill. The resulting amorphous solid was found to have excellent stability as a result of inhibition of surface crystallization. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

  13. Si@SiOx/Graphene nanosheet anode materials for lithium-ion batteries synthesized by ball milling process

    Science.gov (United States)

    Tie, Xiaoyong; Han, Qianyan; Liang, Chunyan; Li, Bo; Zai, Jiantao; Qian, Xuefeng

    2017-12-01

    Si@SiOx/Graphene nanosheet (GNS) nanocomposites as high performance anode materials for lithium-ion batteries are synthesized by mechanically blending the mixture of expanded graphite with Si nanoparticles, and characterized by X-ray diffraction, Raman spectrum, field emission scanning electron microscopy and transmission electron microscopy. During the ball milling process, the size of Si nanoparticles will decrease, and the layer of expanded graphite can be peeled off to thin multilayers. Electrochemical performances reveal that the obtained Si@SiOx/GNS nanocomposites exhibit improved cycling stability, high reversible lithium storage capacity and superior rate capability, e.g. the discharge capacity is kept as high as 1055 mAh g-1 within 50 cycles at a current density of 200 mA g-1, retaining 63.6% of the initial value. The high performance of the obtained nanocomposites can be ascribed to GNS prepared through heat-treat and ball-milling methods, the decrease in the size of Si nanoparticles and SiOx layer on Si surface, which enhance the interactions between Si and GNS.

  14. Transformation of Mg-bearing amorphous calcium carbonate to Mg-calcite - In situ monitoring

    Science.gov (United States)

    Purgstaller, Bettina; Mavromatis, Vasileios; Immenhauser, Adrian; Dietzel, Martin

    2016-02-01

    The formation of Mg-bearing calcite via an amorphous precursor is a poorly understood process that is of relevance for biogenic and abiogenic carbonate precipitation. In order to gain an improved insight on the controls of Mg incorporation in calcite formed via an Mg-rich amorphous calcium carbonate (Mg-ACC) precursor, the precipitation of Mg-ACC and its transformation to Mg-calcite was monitored by in situ Raman spectroscopy. The experiments were performed at 25.0 ± 0.03 °C and pH 8.3 ± 0.1 and revealed two distinct pathways of Mg-calcite formation: (i) At initial aqueous Mg/Ca molar ratios ⩽ 1:6, Mg-calcite formation occurs via direct precipitation from solution. (ii) Conversely, at higher initial Mg/Ca molar ratios, Mg-calcite forms via an intermediate Mg-rich ACC phase. In the latter case, the final product is a calcite with up to 20 mol% Mg. This Mg content is significant higher than that of the Mg-rich ACC precursor phase. Thus, a strong net uptake of Mg ions from the solution into the crystalline precipitate throughout and also subsequent to ACC transformation is postulated. Moreover, the temporal evolution of the geochemical composition of the reactive solution and the Mg-ACC has no significant effect on the obtained ;solubility product; of Mg-ACC. The enrichment of Mg in calcite throughout and subsequent to Mg-ACC transformation is likely affected by the high aqueous Mg/Ca ratio and carbonate alkalinity concentrations in the reactive solution. The experimental results have a bearing on the formation mechanism of Mg-rich calcites in marine early diagenetic environments, where high carbonate alkalinity concentrations are the rule rather than the exception, and on the insufficiently investigated inorganic component of biomineralisation pathways in many calcite secreting organisms.

  15. Band gap-engineered ZnO and Ag/ZnO by ball-milling method and their photocatalytic and Fenton-like photocatalytic activities

    International Nuclear Information System (INIS)

    Choi, Young In; Jung, Hye Jin; Shin, Weon Gyu; Sohn, Youngku

    2015-01-01

    Graphical abstract: - Highlights: • Ag/ZnO hybrid materials were prepared by a ball-milling method. • Adsorption and photocatalytic dye degradation were tested for pure RhB under visible light. • Adsorption and photocatalytic dye degradation were tested for mixed dye (MO + RhB + MB) under visible light. • Fenton-like photocatalytic activity (H 2 O 2 addition effects) was examined. - Abstract: The hybridization of ZnO with Ag has been performed extensively to increase the efficiency of ZnO in various applications, including catalysis. In this study, a wet (w) and dry (d) ball-milling method was used to hybridize Ag with ZnO nanoparticles, and their physicochemical properties were examined. Visible light absorption was enhanced and the band gap was engineered by ball-milling and Ag hybridization. Their photocatalytic activities were tested with rhodamine B (RhB) and a mixed dye (methyl orange + RhB + methylene blue) under visible light irradiation. For pure RhB, the photocatalytic activity was decreased by ball-milling and was observed in the order of ZnO(d) < Ag/ZnO(d) < ZnO(w) < Ag/ZnO(w) ≤ ZnO(ref). For the degradation of RhB and methylene blue (MB) in the mixed dye (or the simulated real contaminated water), the photocatalytic activity was observed in the order of Ag/ZnO(d) < ZnO(d) < ZnO(w) < Ag/ZnO(w) ≤ ZnO(ref). When the photodegradation tested with H 2 O 2 addition, however, the Fenton-like photocatalytic activity was reversed and the ZnO(ref) showed the poorest activity for the degradation of RhB and methylene blue (MB). In the mixed dye over all the catalysts, methyl orange (MO) was degraded most rapidly. The relative degradation rates of RhB and MB were found to be dependent on the catalyst and reaction conditions.

  16. Bismuth-ceramic nanocomposites through ball milling and liquid crystal synthetic methods

    Science.gov (United States)

    Dellinger, Timothy Michael

    Three methods were developed for the synthesis of bismuth-ceramic nanocomposites, which are of interest due to possible use as thermoelectric materials. In the first synthetic method, high energy ball milling of bismuth metal with either MgO or SiO2 was found to produce nanostructured bismuth dispersed on a ceramic material. The morphology of the resulting bismuth depended on its wetting behavior with respect to the ceramic: the metal wet the MgO, but did not wet on the SiO2. Differential Scanning Calorimetry measurements on these composites revealed unusual thermal stability, with nanostructure retained after multiple cycles of heating and cooling through the metal's melting point. The second synthesis methodology was based on the use of lyotropic liquid crystals. These mixtures of water and amphiphilic molecules self-assemble to form periodic structures with nanometer-scale hydrophilic and hydrophobic domains. A novel shear mixing methodology was developed for bringing together reactants which were added to the liquid crystals as dissolved salts. The liquid crystals served to mediate synthesis by acting as nanoreactors to confine chemical reactions within the nanoscale domains of the mesophase, and resulted in the production of nanoparticles. By synthesizing lead sulfide (PbS) and bismuth (Bi) particles as proof-of-concept, it was shown that nanoparticle size could be controlled by controlling the dimensionality of the nanoreactors through control of the liquid crystalline phase. Particle size was shown to decrease upon going from three-dimensionally percolating nanoreactors, to two dimensional sheet-like nanoreactors, to one dimensional rod-like nanoreactors. Additionally, particle size could be controlled by varying the precursor salt concentration. Since the nanoparticles did not agglomerate in the liquid crystal immediately after synthesis, bismuth-ceramic nanocomposites could be prepared by synthesizing Bi nanoparticles and mixing in SiO2 particles which

  17. Crystallographic alignment evolution and magnetic properties of anisotropic Sm{sub 0.6}Pr{sub 0.4}Co{sub 5} nanoflakes prepared by surfactant-assisted ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Xu, M.L.; Wu, Q.; Li, Y.Q.; Liu, W.Q.; Lu, Q.M.; Yue, M., E-mail: yueming@bjut.edu.cn

    2015-08-01

    The microstructure, crystal structure and magnetic properties were studied for Sm{sub 0.6}Pr{sub 0.4}Co{sub 5} nanoflakes prepared by surfactant-assisted high-energy ball milling (SAHEBM). Effect of ball-milling time on the c-axis crystallographic alignment, morphology and magnetic properties of Sm{sub 0.6}Pr{sub 0.4}Co{sub 5} nanoflakes was systematically investigated. With increasing milling time from 1 h to 7 h, the intensity ratio between (002) and (111) reflection peaks indicating degree of c-axis crystal texture of the (Sm, Pr)Co{sub 5} phase increases first, peaks at 3 h, then drops again, revealing that the strongest c-axis crystal texture was obtained in the nanoflakes milled for 3 h. On the other hand, the coercivity (H{sub ci}) of the flakes increases gradually from 1.71 to 14.65 kOe with the increase of ball milling time. As a result, an optimal magnetic properties of M{sub r} of 10.23 kGs, H{sub ci} of 11.45 kOe and (BH){sub max} of 24.40 MGOe was obtained in Sm{sub 0.6}Pr{sub 0.4}Co{sub 5} nanoflakes milled for 3 h, which also displayed a high aspect ratio, small in-plane size, pronounced (001) out-of-plane texture. - Highlights: • Anisotropic Sm{sub 0.6}Pr{sub 0.4}Co{sub 5} nanoflakes with strong c-axis texture were prepared. • Effects of ball-milling time on structure and magnetic properties were studied. • (BH){sub max} value of Sm{sub 0.6}Pr{sub 0.4}Co{sub 5} nanoflakes is larger than that of SmCo{sub 5} nanoflakes.

  18. Cold compaction behavior and pressureless sinterability of ball milled WC and WC/Cu powders

    Directory of Open Access Journals (Sweden)

    Hashemi Seyed R.

    2016-01-01

    Full Text Available In this research, cold compaction behavior and pressureless sinterability of WC, WC-10%wtCu and WC-30%wtCu powders were investigated. WC and WC/Cu powders were milled in a planetary ball mill for 20h. The milled powders were cold compacted at 100, 200, 300 and 400 MPa pressures. The compressibility behavior of the powders was evaluated using the Heckel, Panelli-Ambrosio and Ge models. The results showed that the Panelli-Ambrosio was the preferred equation for description the cold compaction behavior of the milled WC and WC-30%wtCu powders. Also, the most accurate model for describing the compressibility of WC-10%wtCu powders was the Heckel equation. The cold compacts were sintered at 1400°C. It was found that by increasing the cold compaction pressure of powder compacts before sintering, the sinterability of WC-30%wtCu powder compacts was enhanced. However, the cold compaction magnitude was not affected significantly on the sinterability of WC and WC-10%wtCu powders. The microstructural investigations of the sintered samples by Scanning Electron Microscopy (SEM confirmed the presence of porosities at the interface of copper-tungsten carbide phases.

  19. A morphological evaluation of a duplex stainless steel processed by high energy Ball Mill

    International Nuclear Information System (INIS)

    Yonekubo, Ariane Emi; Cintho, Osvaldo Mitsuyuki; Aguiar, Denilson Jose Marcolino de; Capocchi, Jose Deodoro Trani

    2009-01-01

    The duplex stainless steels are formed by a ferrite and austenite mixture, giving them a combination of properties. Commercially, these steels are hot rolled, developing an anisotropic, alternated ferrite and austenite elongated lamellae microstructure. In this work, a duplex stainless steel was produced by the mixture of elementary powders with the composition Fe-19.5Cr-5Ni processed in an ATTRITOR ball mill during periods up to 15 hours. The powders obtained were compressed in specimens and were heat treated in the temperatures of 900, 1050 and 1200 °C during 1 hour and analysed by x ray diffraction, optic microscopy, scanning electron microscopy and energy dispersion spectroscopy. An optimized microstructure with ultrafine, equiaxial and regular duplex microstructure was obtained in the 15 hour milling and 1200 °C heat treatment. Afterwards, a commercially super duplex stainless steel UNS S32520 was aged at 800 °C aiming the precipitation of σ phase in order to reduce its toughness and then, milled in SPEX mill. The resulting microstructure was a very fine duplex type with irregular grain boundary morphology duo to the grain growth barrier promoted by the renascent σ phase particles during sintering process. (author)

  20. Functional nanometers for hydrogen storage produced by ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Czujko, T. [Waterloo Univ., ON (Canada). Dept. of Mechanical and Mechatronics Engineering]|[Military Univ. of Technology, Warsaw (Poland). Dept. of Advanced Materials and Technologies; Varin, R.A. [Waterloo Univ., ON (Canada). Dept. of Mechanical and Mechatronics Engineering; Wronski, Z.S. [Natural Resources Canada, Ottawa, ON (Canada). CANMET Energy Technology Centre, Hydrogen Fuel Cells and Transportation; Zaranski, Z. [Military Univ. of Technology, Warsaw (Poland). Dept. of Advanced Materials and Technologies

    2008-07-01

    It is becoming increasingly important to switch to cleaner alternative energy carriers such as hydrogen, as environmental concerns over greenhouse gas emissions from the burning of fossil fuel increase. Specifically, there is a need for efficient on-board hydrogen storage technologies for vehicular applications. This paper discussed three different methods of hydrogen desorption temperature reduction and desorption kinetics of nanostructured hydrides. The first method was based on substantial hydride particle size refinement. The second method utilized catalytic effects of nanometric n-alumina (Al{sub 2}O{sub 3}), n-yttrium oxide powder (Y{sub 2}O{sub 3}) and n-nickel (Ni) additives. The third method was based on a composite of nanohydride mixtures. The composite approach was applied to the magnesium hydride (MgH{sub 2}) plus sodium tetrahydridoborate (NaBH{sub 4}) and lithium aluminum hydride (LiAlH{sub 4}) systems. The paper presented the effects of nanostructuring and nanocatalytic additives on Mg hydride desorption properties as well as a composite behaviour of nanostructured complex hydrides. It was concluded that milling of commercial MgH{sub 2} with the nano-oxide additives had a limited effect on improving the hydrogen storage properties. The addition of specialty Inco nanometric Ni reduced the hydrogen desorption temperature considerably. 28 refs., 1 tab., 9 figs.

  1. Mechanical alloying and sitering of TI - 10WT.% MG powders

    CSIR Research Space (South Africa)

    Machio, Christopher N

    2009-06-01

    Full Text Available A Ti-10wt.%Mg powder alloy has been produced by mechanical alloying. Elemental powders of Ti and Mg were ball milled in a Zoz-Simoloyer CM01 for 16 and 20 hours under argon. Mechanical alloying was followed by XRD, SEM and particle size analysis...

  2. Comparison of hydrogen storage properties of pure Mg and milled ...

    Indian Academy of Sciences (India)

    Administrator

    increase the hydriding and dehydriding rates, pure Mg was ground under hydrogen atmosphere (reactive .... Hydrogen storage properties of pure Mg and milled pure Mg. 833. Figure 3. ... elongated and flat shapes via collisions with the steel.

  3. Synthesis and characterization of FePt nanoparticles by high energy ball milling with and without surfactant

    International Nuclear Information System (INIS)

    Velasco, V.; Martinez, A.; Recio, J.; Hernando, A.; Crespo, P.

    2012-01-01

    Highlights: ► Fe and Pt powders in the presence of surfactants don’t alloyed by HEBM technique. ► FePt alloys obtained by dry milling exhibit particle sizes of around 10 μm. ► FePt alloys obtained by dry milling exhibit soft magnetic behavior. ► A thermal treatment induces a phase transformation from FCC to FCT. - Abstract: FePt nanoparticles were prepared by high energy ball milling (HEBM) in two different ways. In the first one, elemental powders were mixed and milled whereas in the second one the milling was performed in the presence of oleyl amine and oleic acid as surfactants and hexane as a solvent. X-ray diffraction shows that when the milling is performed in dry conditions, Fe and Pt are alloyed after 5 h, whereas in the wet milling procedure alloying does not take place. In the first case, the diffraction pattern corresponds to the disordered FCC phase. This behavior is also corroborated by the evolution of the magnetic characteristics. In the case of the alloy obtained in dry conditions, the powder was heat treated in order to induce the transformation to the ordered phase. Coercivities of 2.5 kOe are obtained after 650 °C for 2 h.

  4. Si/C composite lithium-ion battery anodes synthesized from coarse silicon and citric acid through combined ball milling and thermal pyrolysis

    International Nuclear Information System (INIS)

    Gu Peng; Cai Rui; Zhou Yingke; Shao Zongping

    2010-01-01

    Silicon and related materials have recently received considerable attention as potential anodes in Li-ion batteries for their high theoretical specific capacities. To overcome the problem of volume variations during the Li insertion/extraction process, in this work, Si/C composites with low carbon content were synthesized from cheap coarse silicon and citric acid by simple ball milling and subsequent thermal treatment. The effects of ball milling time and calcination temperature on the structure, composition and morphology of the composites were systematically investigated by the determination of specific surface area (BET) and particle-size distribution, X-ray diffraction (XRD), O 2 -TPO, and scanning electron microscopy (SEM). The capacity and cycling stability of the composites were systematically evaluated by electrochemical charge/discharge tests. It was found that both the initial capacity and the cycling stability of the composites were dependent on the milling and calcination conditions, and attractive overall electrochemical performance could be obtained by optimizing the synthesis process.

  5. Preparation, characterization and optoelectronic properties of nanodiamonds doped zinc oxide nanomaterials by a ball milling technique

    Science.gov (United States)

    Ullah, Hameed; Sohail, Muhammad; Malik, Uzma; Ali, Naveed; Bangash, Masroor Ahmad; Nawaz, Mohsan

    2016-07-01

    Zinc oxide (ZnO) is one of the very important metal oxides (MOs) for applications in optoelectronic devices which work in the blue and UV regions. However, to meet the challenges of obtaining ZnO nanomaterials suitable for practical applications, various modifications in physico-chemical properties are highly desirable. One of the ways adopted for altering the properties is to synthesize composite(s) of ZnO with various reinforcements. Here we report on the tuning of optoelectronic properties of ZnO upon doping by nanodiamonds (NDs) using the ball milling technique. A varying weight percent (wt.%) of NDs were ball milled for 2 h with ZnO nanoparticles prepared by a simple precipitation method. The effects of different parameters, the calcination temperature of ZnO, wt.% of NDs and mechanical milling upon the optoelectronic properties of the resulting ZnO-NDs nanocomposites have been investigated. The ZnO-NDs nanocomposites were characterized by IR spectroscopy, powder x-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDX). The UV-vis spectroscopy revealed the alteration in the bandgap energy (Eg ) of ZnO as a function of the calcination temperature of ZnO, changing the concentration of NDs, and mechanical milling of the resulting nanocomposites. The photoluminescence (PL) spectroscopy showed a decrease in the deep level emission (DLE) peaks and an increase in near-band-edge transition peaks as a result of the increasing concentration of NDs. The decrease in DLE and increase in band to band transition peaks were due to the strong interaction between the NDs and the Zn+; consequently, the Zn+ concentration decreased on the interstitial sites.

  6. Assessment of crystalline disorder in cryo-milled samples of indomethacin using atomic pair-wise distribution functions

    DEFF Research Database (Denmark)

    Bøtker, Johan P; Karmwar, Pranav; Strachan, Clare J

    2011-01-01

    to analyse the cryo-milled samples. The high similarity between the ¿-indomethacin cryogenic ball milled samples and the crude ¿-indomethacin indicated that milled samples retained residual order of the ¿-form. The PDF analysis encompassed the capability of achieving a correlation with the physical......The aim of this study was to investigate the usefulness of the atomic pair-wise distribution function (PDF) to detect the extension of disorder/amorphousness induced into a crystalline drug using a cryo-milling technique, and to determine the optimal milling times to achieve amorphisation. The PDF...... properties determined from DSC, ss-NMR and stability experiments. Multivariate data analysis (MVDA) was used to visualize the differences in the PDF and XRPD data. The MVDA approach revealed that PDF is more efficient in assessing the introduced degree of disorder in ¿-indomethacin after cryo-milling than...

  7. Influence of cation disorder on the magnetic properties of ball-milled ilmenite (FeTiO3)

    DEFF Research Database (Denmark)

    Mørup, Steen; Rasmussen, Helge Kildahl; Brok, Erik

    2012-01-01

    We have investigated the evolution of crystal structure, cation disorder and magnetic properties of ilmenite (FeTiO3) after increasing time of high-energy ball-milling in an inert atmosphere. Refinement of X-ray diffraction data show that the hexagonal crystal structure of ilmenite is maintained...

  8. Niobium Carbide-Reinforced Al Matrix Composites Produced by High-Energy Ball Milling

    Science.gov (United States)

    Travessa, Dilermando Nagle; Silva, Marina Judice; Cardoso, Kátia Regina

    2017-06-01

    Aluminum and its alloys are key materials for the transportation industry as they contribute to the development of lightweight structures. The dispersion of hard ceramic particles in the Al soft matrix can lead to a substantial strengthening effect, resulting in composite materials exhibiting interesting mechanical properties and inspiring their technological use in sectors like the automotive and aerospace industries. Powder metallurgy techniques are attractive to design metal matrix composites, achieving a homogeneous distribution of the reinforcement into the metal matrix. In this work, pure aluminum has been reinforced with particles of niobium carbide (NbC), an extremely hard and stable refractory ceramic. Its use as a reinforcing phase in metal matrix composites has not been deeply explored. Composite powders produced after different milling times, with 10 and 20 vol pct of NbC were produced by high-energy ball milling and characterized by scanning electron microscopy and by X-ray diffraction to establish a relationship between the milling time and size, morphology, and distribution of the particles in the composite powder. Subsequently, an Al/10 pct NbC composite powder was hot extruded into cylindrical bars. The strength of the obtained composite bars is comparable to the commercial high-strength, aeronautical-grade aluminum alloys.

  9. Magnetic Properties of Nanocrystalline Fe{sub x}Cu{sub 1-x} Alloys Prepared by Ball Milling

    Energy Technology Data Exchange (ETDEWEB)

    Yousif, A.; Bouziane, K., E-mail: bouzi@squ.edu.om; Elzain, M. E. [Sultan Qaboos University, Physics Department, College of Science (Oman); Ren, X.; Berry, F. J. [The Open University, Department of Chemistry (United Kingdom); Widatallah, H. M. [Sudan Atomic Energy Commission, Institute of Nuclear Research (Sudan); Al Rawas, A.; Gismelseed, A.; Al-Omari, I. A. [Sultan Qaboos University, Physics Department, College of Science (Oman)

    2004-12-15

    X-ray diffraction, Moessbauer and magnetization measurements were used to study Fe{sub x}Cu{sub 1-x} alloys prepared by ball-milling. The X-ray data show the formation of a nanocrystalline Fe-Cu solid solution. The samples with x{>=}0.8 and x{<=}0.5 exhibit bcc or fcc phase, respectively. Both the bcc and fcc phases are principally ferromagnetic for x{>=}0.2, but the sample with x=0.1 remains paramagnetic down to 78 K. The influence of the local environment on the hyperfine parameters and the local magnetic moment are discussed using calculations based on the discrete-variational method in the local density approximation.

  10. A novel fabrication technology of in situ TiB2/6063Al composites: High energy ball milling and melt in situ reaction

    International Nuclear Information System (INIS)

    Zhang, S.-L.; Yang, J.; Zhang, B.-R.; Zhao, Y.-T.; Chen, G.; Shi, X.-X.; Liang, Z.-P.

    2015-01-01

    Highlights: • This paper presents a novel technology to fabricate the TiB 2 /6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB 2 /6063Al matrix composites are fabricated from Al–TiO 2 –B 2 O 3 system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO 2 –B 2 O 3 system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB 2 particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB 2 particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB 2 /6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character

  11. Morphology and magnetic properties of CeCo5 submicron flakes prepared by surfactant-assisted high-energy ball milling

    International Nuclear Information System (INIS)

    Zhang, J.J.; Gao, H.M.; Yan, Y.; Bai, X.; Su, F.; Wang, W.Q.; Du, X.B.

    2012-01-01

    CeCo 5 permanent magnetic alloy has been processed by surfactant assisted high energy ball milling. Heptane and oleic acid were used as the solvent and surfactant, respectively. The amount of surfactant used was 50% by weight of the starting powder. The produced particles were deposited on a piece of copper (4 mm in length and width) under a magnetic field of 27 kOe applied along the copper surface and immobilized by ethyl α-cyanoacrylate. Scanning electron microscope pictures show that the particles are flakes, several μm in length and width and tens of nm in thickness. X-ray diffraction patterns and magnetic measurements prove that the flakes are crystalline with c-axes magnetic anisotropy. The easy magnetization axis is oriented perpendicular to the surface of the flake. A maximum coercivity of 3.3 kOe was obtained for the sample milled for 40 min. - Highlights: ► CeCo 5 permanent magnetic alloy has been processed by surfactant assisted high energy ball milling (HEBM). ► The particles show a flake-like morphology with several μm in length and width and tens nm in thickness. ► The flakes are crystallographic and magnetic anisotropic and the c-axes, also the easy magnetization directions are oriented perpendicular to the surface of the flake. ► Maximum coercivity of 3.3 kOe has been obtained for the sample milled for 40 min.

  12. Milling and dispersion of multi-walled carbon nanotubes in texanol

    Science.gov (United States)

    Darsono, Nono; Yoon, Dang-Hyok; Kim, Jaemyung

    2008-03-01

    Rheological results were used to determine the optimum type of dispersant and its concentration for six commercial dispersants for the dispersion of multi-walled carbon nanotube (MWCNT) agglomerates in texanol. An unsaturated polycarboxylic acid copolymer (BYK P-104) exhibited the optimum performance with the lowest MWCNT slurry viscosity in texanol. The cutting and dispersion efficiencies of MWCNTs with 20 wt.% of BYK P-104 dispersant were compared using conventional ball milling and high energy milling, whereby the latter was found to be more effective. High energy milling for 2 h produced a large portion of MWCNT agglomerates smaller than 150 nm, showing a drastic increase in slurry viscosity due to the dispersion into individual CNTs. On the other hand, 120 h ball milling was required to achieve the agglomerate size of 300 nm with less viscosity increase upon milling. Decrease in the degree of MWCNT crystallinity was observed by both milling, even though 2 h high energy milling showed slightly less damage than 120 h ball milling based on XRD and Raman spectroscopy results.

  13. Mg2FeH6 Synthesis Efficiency Map

    Directory of Open Access Journals (Sweden)

    Katarzyna Witek

    2018-02-01

    Full Text Available The influences of the processing parameters on the Mg2FeH6 synthesis yield were studied. Mixtures of magnesium hydride (MgH2 and iron (Fe were mechanically milled in a planetary ball mill under argon for 0.5-, 1-, 2- and 3-h periods and subsequently sintered at temperatures from 300–500 ∘ C under hydrogen. The reaction yield, phase content and hydrogen storage properties of the received materials were investigated. The morphologies of the powders after synthesis were studied by SEM. The synthesis effectiveness map was presented. The obtained results prove that synthesis parameters, such as the milling time and synthesis temperature, greatly influence the reaction yield and material properties and show that extended mechanical milling may not be beneficial to the reaction efficiency.

  14. Fabrication of a Micro-Lens Array Mold by Micro Ball End-Milling and Its Hot Embossing

    Directory of Open Access Journals (Sweden)

    Peng Gao

    2018-02-01

    Full Text Available Hot embossing is an efficient technique for manufacturing high-quality micro-lens arrays. The machining quality is significant for hot embossing the micro-lens array mold. This study investigates the effects of micro ball end-milling on the machining quality of AISI H13 tool steel used in the micro-lens array mold. The micro ball end-milling experiments were performed under different machining strategies, and the surface roughness and scallop height of the machined micro-lens array mold are measured. The experimental results showed that a three-dimensional (3D offset spiral strategy could achieve a higher machining quality in comparison with other strategies assessed in this study. Moreover, the 3D offset spiral strategy is more appropriate for machining the micro-lens array mold. With an increase of the cutting speed and feed rate, the surface roughness of the micro-lens array mold slightly increases, while a small step-over can greatly reduce the surface roughness. In addition, a hot embossing experiment was undertaken, and the obtained results indicated higher-quality production of the micro-lens array mold by the 3D offset spiral strategy.

  15. Highly Al-doped TiO2 nanoparticles produced by Ball Mill Method: structural and electronic characterization

    International Nuclear Information System (INIS)

    Santos, Desireé M. de los; Navas, Javier; Sánchez-Coronilla, Antonio; Alcántara, Rodrigo; Fernández-Lorenzo, Concha; Martín-Calleja, Joaquín

    2015-01-01

    Highlights: • Highly Al-doped TiO 2 nanoparticles were synthesized using a Ball Mill Method. • Al doping delayed anatase to rutile phase transformation. • Al doping allow controlling the structural and electronic properties of nanoparticles. - Abstract: This study presents an easy method for synthesizing highly doped TiO 2 nanoparticles. The Ball Mill method was used to synthesize pure and Al-doped titanium dioxide, with an atomic percentage up to 15.7 at.% Al/(Al + Ti). The samples were annealed at 773 K, 973 K and 1173 K, and characterized using ICP-AES, XRD, Raman spectroscopy, FT-IR, TG, STEM, XPS, and UV–vis spectroscopy. The effect of doping and the calcination temperature on the structure and properties of the nanoparticles were studied. The results show high levels of internal doping due to the substitution of Ti 4+ ions by Al 3+ in the TiO 2 lattice. Furthermore, anatase to rutile transformation occurs at higher temperatures when the percentage of doping increases. Therefore, Al doping allows us to control the structural and electronic properties of the nanoparticle synthesized. So, it is possible to obtain nanoparticles with anatase as predominant phase in a higher range of temperature

  16. Research kinetic of motion of milling bodies in ball mill, outfit heat-exchange unit and calculation of its energy performance

    Science.gov (United States)

    Romanovich, A. A.; Romanovich, M. A.; Apukhtina, I. V.

    2018-03-01

    The article considers topical issues of energy saving in cement production with the use of a technological grinding complex, which includes a press roller grinder and a ball mill. Rational conditions of grinding are proposed for pre-shredded material through the installation of blade energy exchange devices (BEED) in the mill drum. The loading level in the first chamber varies periodically depending on the drum rotation angle, equipped with BEED. In the zone of BEED’s active action, there is a “scooping” of a part of grinding bodies together with crushed material, raising them to a height and giving them a longitudinally transverse movement, which is different from movement created in the mill without BEED. At the same time, additional work that consumes engine power is being done. A technique is proposed for calculating the additional engine power consumption of a mill, equipped with a BEED. This power is spent on creating a longitudinal-transverse motion of grinding bodies and its first and second chambers in areas of active influence of the BEED. Comparative analysis of results obtained experimentally and calculations of proposed equations show a high convergence of results. These analytical dependencies may be interest to Russian and foreign organizations that carry out their activities in the field of design and manufacture of cement equipment, as well as to cement producers.

  17. Utilization of aluminum to obtaining a duplex type stainless steel using high energy ball milling

    International Nuclear Information System (INIS)

    Pavlak, I.E.; Cintho, O.M.; Capocchi, J.D.T.

    2010-01-01

    The obtaining of stainless steel using aluminum in its composition - FeMnAl system, has been researches subject since the sixties, by good mechanical properties and resistance to oxidation presented, when compared with conventional FeNiCr stainless steel system. In another point, the aluminum and manganese are low cost then traditional elements. This work, metallic powders of iron, manganese and pure aluminum, were processed in a Spex type high-energy ball mill in nitrogen atmosphere. The milling products were compressed into pastille form and sintered under inert atmosphere. The final products were characterized by optical and electronic microscopy and microhardness test. The metallographic analysis shows a typical austenite and ferrite duplex type microstructure. The presence of these phases was confirmed according X ray diffraction analysis. (author)

  18. Quenching ilmenite with a high-temperature and high-pressure phase using super-high-energy ball milling.

    Science.gov (United States)

    Hashishin, Takeshi; Tan, Zhenquan; Yamamoto, Kazuhiro; Qiu, Nan; Kim, Jungeum; Numako, Chiya; Naka, Takashi; Valmalette, Jean Christophe; Ohara, Satoshi

    2014-04-25

    The mass production of highly dense oxides with high-temperature and high-pressure phases allows us to discover functional properties that have never been developed. To date, the quenching of highly dense materials at the gramme-level at ambient atmosphere has never been achieved. Here, we provide evidence of the formation of orthorhombic Fe2TiO4 from trigonal FeTiO3 as a result of the high-temperature (>1250 K) and high-pressure (>23 GPa) condition induced by the high collision energy of 150 gravity generated between steel balls. Ilmenite was steeply quenched by the surrounding atmosphere, when iron-rich ilmenite (Fe2TiO4) with a high-temperature and high-pressure phase was formed by planetary collisions and was released from the collision points between the balls. Our finding allows us to infer that such intense planetary collisions induced by high-energy ball milling contribute to the mass production of a high-temperature and high-pressure phase.

  19. Microstructural characteristics and mechanical properties of carbon nanotube reinforced aluminum alloy composites produced by ball milling

    International Nuclear Information System (INIS)

    Raviathul Basariya, M.; Srivastava, V.C.; Mukhopadhyay, N.K.

    2014-01-01

    Highlights: • 6082 Al alloy composite with 2 wt% multiwalled carbon nanotubes prepared by milling. • Effect of milling time on structure and property evolution has been studied. • The reinforced composite powders showed a drastic crystallite size refinement. • The presence of carbon nanotube led to a two fold increase in the hardness and modulus. • The composite powder showed good thermal stability studied by DTA. - Abstract: The influence of milling time on the structure, morphology and thermal stability of multi-walled carbon nanotubes (MWCNTs) reinforced EN AW6082 aluminum alloy powders has been studied. After structural and microstructural characterization of the mechanically milled powders micro- and nano-hardness of the composite powder particles were evaluated. The morphological and X-ray diffraction studies on the milled powders revealed that the carbon nanotubes (CNTs) were uniformly distributed and embedded within the aluminum matrix. No reaction products were detected even after long milling up to 50 h. Nanotubes became shorter in length as they fractured under the impact and shearing action during the milling process. A high hardness of about 436 ± 52 HV is achieved for the milled powders, due to the addition of MWCNTs, after milling for 50 h. The increased elastic modulus and nanohardness can be attributed to the finer grain size evolved during high energy ball milling and to the uniform distribution of hard CNTs in the Al-alloy matrix. The hardness values of the composite as well as the matrix alloy compares well with that predicted by the Hall–Petch relationship

  20. Moessbauer study of Mg-Ni(Fe) alloys processed as materials for solid state hydrogen storage

    Energy Technology Data Exchange (ETDEWEB)

    Palade, P.; Principi, G., E-mail: giovanni.principi@unipd.it; Sartori, S.; Maddalena, A. [Universita di Padova, Settore Materiali, DIM (Italy); Lo Russo, S. [Universita di Padova, Dipartimento di Fisica (Italy); Schinteie, G.; Kuncser, V.; Filoti, G. [National Institute for Materials Physics, Solid State Magnetism Department (Romania)

    2006-02-15

    Mg-Ni-Fe magnesium-rich intermetallic compounds were prepared following two distinct routes. A Mg{sub 88}Ni{sub 11}Fe{sub 1} sample (A) was prepared by melt spinning Mg-Ni-Fe pellets and then by high-energy ball milling for 6 h the obtained ribbons. A (MgH{sub 2}){sub 88}Ni{sub 11}Fe{sub 1} sample (B) was obtained by high-energy ball milling for 20 h a mixture of Ni, Fe and MgH{sub 2} powders in the due proportions. A SPEX8000 shaker mill with a 10:1 ball to powder ratio was used for milling in argon atmosphere. The samples were submitted to repeated hydrogen absorption/desorption cycles in a Sievert type gas-solid reaction controller at temperatures in the range 520 - 590 K and a maximum pressure of 2.5 MPa during absorption. The samples were analysed before and after the hydrogen absorption/desorption cycles by X-ray diffraction and Moessbauer spectroscopy. The results concerning the hydrogen storage properties of the studied compounds are discussed in connection with the micro-structural characteristics found by means of the used analytical techniques. The improved kinetics of hydrogen desorption for sample A, in comparison to sample B, has been ascribed to the different behaviour of iron atoms in the two cases, as proved by Moessbauer spectroscopy. In fact, iron results homogeneously distributed in sample A, partly at the Mg{sub 2}Ni grain boundaries, with catalytic effect on the gas-solid reaction; in sample B, instead, iron is dispersed inside the hydride powder as metallic iron or superparamagnetic iron.

  1. Magnesium substitution in carbonated hydroxyapatite: Structural and microstructural characterization by Rietveld's refinement

    Energy Technology Data Exchange (ETDEWEB)

    Lala, S. [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India); Ghosh, M.; Das, P.K. [Department of Biological Chemistry, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032 (India); Das, D. [UGC-DAE Consortium for Scientific Research, Kolkata 700098 (India); Kar, T. [Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700032 (India); Pradhan, S.K., E-mail: skpradhan@phys.buruniv.ac.in [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India)

    2016-02-15

    Four stoichiometric compositions of nanocrystalline Mg doped carbonated hydroxyapatite (cHAp) powders are synthesized by mechanical alloying (ball milling) the powder mixtures of CaCO{sub 3}, CaHPO{sub 4}.2H{sub 2}O and MgO in open air at room temperature. FTIR analysis confirms the A-type carbonation in all milled HAp powder samples (A-cHAp). Microstructure characterization in terms of lattice imperfections and phase quantification of ball milled samples are made by analyzing XRD patterns employing Rietveld's structure refinement method. Transmission electron microscopy (TEM) study of 15 mol % Mg doped A-cHAp sample reveals microstructure similar to that obtained from XRD pattern analysis. Cumulative effect of Mg substitution and mechanical alloying results in amorphization of a major part of crystalline A-cHAp, analogous to native bone mineral. Rietveld analysis reveals that the Ca2 vacancy site is energetically more favorable for occupation of Mg substitution. MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assay test reveals sufficiently high percentage cell viability confirming the cytocompatibility of the sample. - Graphical abstract: Mg substitution for Ca2 site. - Highlights: • Single phase Mg doped A-cHAp synthesized by mechanical alloying (MA). • FTIR analysis confirms A-type carbonation in HAp. • Amorphization of a part of crystalline A-cHAp due to MA and Mg insertion. • Mg{sup 2+} ions substitute the Ca2 vacancy site. • High cell viability under MTT assay.

  2. Synthesis and characterization of FePt nanoparticles by high energy ball milling with and without surfactant

    Energy Technology Data Exchange (ETDEWEB)

    Velasco, V., E-mail: vvjimeno@fis.ucm.es [Instituto de Magnetismo Aplicado, UCM-ADIF-CSIC, 28230 Las Rozas (Spain); Martinez, A.; Recio, J. [Instituto de Magnetismo Aplicado, UCM-ADIF-CSIC, 28230 Las Rozas (Spain); Hernando, A.; Crespo, P. [Instituto de Magnetismo Aplicado, UCM-ADIF-CSIC, 28230 Las Rozas (Spain); Dpto. de Fisica de Materiales, UCM, 28040 Madrid (Spain)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Fe and Pt powders in the presence of surfactants don't alloyed by HEBM technique. Black-Right-Pointing-Pointer FePt alloys obtained by dry milling exhibit particle sizes of around 10 {mu}m. Black-Right-Pointing-Pointer FePt alloys obtained by dry milling exhibit soft magnetic behavior. Black-Right-Pointing-Pointer A thermal treatment induces a phase transformation from FCC to FCT. - Abstract: FePt nanoparticles were prepared by high energy ball milling (HEBM) in two different ways. In the first one, elemental powders were mixed and milled whereas in the second one the milling was performed in the presence of oleyl amine and oleic acid as surfactants and hexane as a solvent. X-ray diffraction shows that when the milling is performed in dry conditions, Fe and Pt are alloyed after 5 h, whereas in the wet milling procedure alloying does not take place. In the first case, the diffraction pattern corresponds to the disordered FCC phase. This behavior is also corroborated by the evolution of the magnetic characteristics. In the case of the alloy obtained in dry conditions, the powder was heat treated in order to induce the transformation to the ordered phase. Coercivities of 2.5 kOe are obtained after 650 Degree-Sign C for 2 h.

  3. Fe-FeS2 adsorbent prepared with iron powder and pyrite by facile ball milling and its application for arsenic removal.

    Science.gov (United States)

    Min, Xiaobo; Li, Yangwenjun; Ke, Yong; Shi, Meiqing; Chai, Liyuan; Xue, Ke

    2017-07-01

    Arsenic is one of the major pollutants and a worldwide concern because of its toxicity and chronic effects on human health. An adsorbent of Fe-FeS 2 mixture for effective arsenic removal was successfully prepared by mechanical ball milling. The products before and after arsenic adsorption were characterized with scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The adsorbent shows high arsenic removal efficiency when molar ratio of iron to pyrite is 5:5. The experimental data of As(III) adsorption are fitted well with the Langmuir isotherm model with a maximal adsorption capacity of 101.123 mg/g. And As(V) data were described perfectly by the Freundlich model with a maximal adsorption capacity of 58.341 L/mg. As(III) is partial oxidized to As(V) during the adsorption process. High arsenic uptake capability and cost-effectiveness of waste make it potentially attractive for arsenic removal.

  4. Band gap-engineered ZnO and Ag/ZnO by ball-milling method and their photocatalytic and Fenton-like photocatalytic activities

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Young In [School of Chemistry and Biochemistry, Yeungnam University, Gyeongsan, Gyeongbuk 38541 (Korea, Republic of); Jung, Hye Jin [Department of Mechanical Engineering, Chungnam National University, Daejeon 34134 (Korea, Republic of); Shin, Weon Gyu, E-mail: wgshin@cnu.ac.kr [Department of Mechanical Engineering, Chungnam National University, Daejeon 34134 (Korea, Republic of); Sohn, Youngku, E-mail: youngkusohn@ynu.ac.kr [School of Chemistry and Biochemistry, Yeungnam University, Gyeongsan, Gyeongbuk 38541 (Korea, Republic of)

    2015-11-30

    Graphical abstract: - Highlights: • Ag/ZnO hybrid materials were prepared by a ball-milling method. • Adsorption and photocatalytic dye degradation were tested for pure RhB under visible light. • Adsorption and photocatalytic dye degradation were tested for mixed dye (MO + RhB + MB) under visible light. • Fenton-like photocatalytic activity (H{sub 2}O{sub 2} addition effects) was examined. - Abstract: The hybridization of ZnO with Ag has been performed extensively to increase the efficiency of ZnO in various applications, including catalysis. In this study, a wet (w) and dry (d) ball-milling method was used to hybridize Ag with ZnO nanoparticles, and their physicochemical properties were examined. Visible light absorption was enhanced and the band gap was engineered by ball-milling and Ag hybridization. Their photocatalytic activities were tested with rhodamine B (RhB) and a mixed dye (methyl orange + RhB + methylene blue) under visible light irradiation. For pure RhB, the photocatalytic activity was decreased by ball-milling and was observed in the order of ZnO(d) < Ag/ZnO(d) < ZnO(w) < Ag/ZnO(w) ≤ ZnO(ref). For the degradation of RhB and methylene blue (MB) in the mixed dye (or the simulated real contaminated water), the photocatalytic activity was observed in the order of Ag/ZnO(d) < ZnO(d) < ZnO(w) < Ag/ZnO(w) ≤ ZnO(ref). When the photodegradation tested with H{sub 2}O{sub 2} addition, however, the Fenton-like photocatalytic activity was reversed and the ZnO(ref) showed the poorest activity for the degradation of RhB and methylene blue (MB). In the mixed dye over all the catalysts, methyl orange (MO) was degraded most rapidly. The relative degradation rates of RhB and MB were found to be dependent on the catalyst and reaction conditions.

  5. Hydrogen kinetics studies of MgH2-FeTi composites

    Science.gov (United States)

    Meena, Priyanka; Jangir, Mukesh; Singh, Ramvir; Sharma, V. K.; Jain, I. P.

    2018-05-01

    MgH2 + x wt% FeTi (x=10, 25, 50) nano composites were ball milled to get nano structured material and characterized for structural, morphological and thermal properties. XRD of the milled samples revealed the formation of MgH2, FeTi, Fe2Ti and H0.06FeTi phases. Morphological studies by SEM were undertaken to investigate the effect of hydrogenation of nanostructure alloy. EDX confirmed elemental composition of the as-prepared alloy. TGA studies showed higher desorption temperature for milled MgH2 compared to x wt% FeTi added MgH2. Activation energy for hydrogen desorption was found to be -177.90, -215.69, -162.46 and -87.93 kJ/mol for milled MgH2 and Mg2+x wt% FeTi (10, 25, 50), showing 89.97 kJ/ mol reduction in activation energy for 50 wt% alloy additives resulting in improved hydrogen storage capacity. DSC investigations were carried out to investigate the effect of alloy on hydrogen absorption behavior of MgH2.

  6. Preparation of MgB2 superconducting microbridges by focused ion beam direct milling

    Science.gov (United States)

    Zhang, Xuena; Li, Yanli; Xu, Zhuang; Kong, Xiangdong; Han, Li

    2017-01-01

    MgB2 superconducting microbridges were prepared by focused ion beam (FIB) direct milling on MgB2 films. The surface topography of the microbridges were observed using SEM and AFM and the superconductivity was measured in this paper. Lots of cracks and holes were found near the milled area. And the superconducting transition temperature was decreased a lot and the bridges prepared were not superconducting due to ion damage after milled with large dose. Through these works, we explored the effect regular of FIB milling and experimental parameters on the performance of microbridges.

  7. Preparation and Properties of Mg-Cu-Y-Al bulk Amorphous Alloys

    DEFF Research Database (Denmark)

    Pryds, Nini; Eldrup, Morten Mostgaard; Ohnuma, M.

    2000-01-01

    Bulk amorphous (Mg(1-gamma)Al(gamma))(60)CU(30)Y(10) alloys were prepared using a relatively simple technique of rapid cooling of the melt in a copper wedge mould. The temperature vs, time was recorded during the cooling and solidification process of the melt and compared with a spacial and tempo......Bulk amorphous (Mg(1-gamma)Al(gamma))(60)CU(30)Y(10) alloys were prepared using a relatively simple technique of rapid cooling of the melt in a copper wedge mould. The temperature vs, time was recorded during the cooling and solidification process of the melt and compared with a spacial...... temperatures in specimens containing a few percent Al. The alloy with no Al crystallises apparently without the formation of nanoparticles. The critical cooling rate for the formation of an amorphous Mg(60)CU(30)Y(10) specimen was determined experimentally by a combination of DSC data and temperature vs, time...

  8. Development of a Hydrogen Uptake-Release Mg-Based Alloy by Adding a Polymer CMC (Carboxymethylcellulose, Sodium Salt) via Reaction-Accompanying Milling

    Science.gov (United States)

    Kwak, Young Jun; Choi, Eunho; Song, Myoung Youp

    2018-03-01

    The addition of carboxymethylcellulose, sodium salt (CMC) might improve the hydrogen uptake and release properties of Mg since it has a relatively low melting point and the melting of CMC during milling in hydrogen (reaction-accompanying milling) may make the milled samples be in good states to absorb and release hydrogen rapidly and to have a large hydrogen-storage capacity. Samples with compositions of 95 w/o Mg + 5 w/o CMC (named Mg-5CMC) and 90 w/o Mg + 10 w/o CMC (named Mg-10CMC) were prepared by adding CMC via reaction-accompanying milling. Activation of Mg-10CMC was completed after about 3 hydrogen uptake-release cycles. Mg-10CMC had a higher initial hydrogen uptake rate and a larger amount of hydrogen absorbed in 60 min, U (60 min), than Mg-5CMC before and after activation. At the cycle number of three (CN = 3), Mg-10CMC had a very high initial hydrogen uptake rate (1.56 w/o H/min) and a large U (60 min) (5.57 w/o H) at 593 K in hydrogen of 12 bar, showing that the activated Mg-10CMC has an effective hydrogen-storage capacity of about 5.6 w/o at 593 K in hydrogen of 12 bar at CN = 3. At CN = 2, Mg-10CMC released 1.00 w/o H in 2.5 min, 4.67 w/o H in 10 min, and 4.76 w/o H in 60 min at 648 K in hydrogen of 1.0 bar. The milling in hydrogen of Mg with CMC is believed to generate imperfections and cracks and reduce the particle size. The addition of 10 w/o CMC was more effective on the initial hydrogen uptake rate and U (60 min) compared with the 10 w/o additions of NbF5, TaF5, Fe2O3, and MnO, and the 10 w/o simultaneous addition of Ni, Fe, and Ti. To the best of our knowledge, this study is the first in which a polymer CMC is added to Mg by reaction-accompanying milling to improve the hydrogen storage properties of Mg.

  9. Insight into poor cycling stability of MgH2 anodes

    DEFF Research Database (Denmark)

    Huen, Priscilla; Ravnsbæk, Dorthe B.

    2017-01-01

    . The effects of different preparation methods on cell efficiency and cycle stability are examined, showing that crystallite size reduction and ball milling together with the selected carbon source is important both for increasing capacity and limiting polarization. Furthermore, the conversion mechanism......During recent years, MgH2 has received significant interest as conversion-type anode for Li-ion batteries due to the high theoretical capacity of 2038 mAh/g at ~0.5 V vs. Li+/Li. However, the practical reversible capacity and the cycle stability are generally poor and vary significantly among...... literature reports. The latter may be due to differences in preparation procedures for electrodes as well as the precise cycling conditions. In this study, a series of MgH2 samples was systematically prepared by ball milling with different conductive carbon sources and use of hydrogenation treatments...

  10. Contribution to the study of the amorphization mechanisms of intermetallic compounds by mechanical grinding; Contribution a l`etude des mecanismes d`amorphisation par sollicitation mecanique de composes intermetalliques

    Energy Technology Data Exchange (ETDEWEB)

    Galy, D

    1995-01-11

    This work aims at identifying the mechanisms responsible for amorphization of NiZr and NiZr{sub 2} compounds under ball-milling. In the first part, the effect of a localized deformation is studied: the deformation is produced by indentation on bulk samples, very high local strains can be achieved by this technique. The resulting microstructure is studied by transmission electron microscopy (TEM). No evidence for amorphization is found in these compounds, contrary to what is known to occur in silicon and germanium. Despite of their high brittleness, the NiZr and NiZr{sub 2} compounds accommodate the multiaxial localized stress by plastic deformation: dislocations multiplication and glide, micro-twinning. Dislocations (both perfect and imperfect) and micro-twins have been analysed into details for the first time. The twinning mechanism in NiZr{sub 2} has been elucidated. In the second part of this work, the microstructure of NiZr{sub 2} in the course of amorphization by ball-milling is studied by TEM observation are prepared by ultra-microtomy. The following evolution is observed: first, the material is fragmented and plastically deformed; the microstructure is refined by polygonation. Second, aggregates are formed by a fragmentation and sticking process, leading to a stationary size for the aggregates. The aggregates themselves are made of a mixture of nanocrystalline (about 10 nm) material and coarser crystallites. As milling proceeds, the latter disappear to the benefit of the former. Once aggregates are 100% nanocrystalline, the amorphous phase appears and develops to the expense of the nanocrystalline phase. At late stages, small crystallites embedded in an amorphous matrix are observed. No massive chemical disordering is observed but a small amount can not be ruled out. It is suggested that amorphization occurs by chemical disordering at interfaces, induced by shear waves. (Author). 76 refs., 57 figs., 12 tabs.

  11. A novel fabrication technology of in situ TiB{sub 2}/6063Al composites: High energy ball milling and melt in situ reaction

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, S.-L.; Yang, J. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Zhang, B.-R. [School of Mechanical Engineering, Qilu University of Technology, Jinan, Shandong 250022 (China); Zhao, Y.-T., E-mail: 278075525@qq.com [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Chen, G.; Shi, X.-X.; Liang, Z.-P. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China)

    2015-08-05

    Highlights: • This paper presents a novel technology to fabricate the TiB{sub 2}/6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB{sub 2}/6063Al matrix composites are fabricated from Al–TiO{sub 2}–B{sub 2}O{sub 3} system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO{sub 2}–B{sub 2}O{sub 3} system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB{sub 2} particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB{sub 2} particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB{sub 2}/6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character.

  12. Memory effect of ball-milled and annealed nanosized hematite

    International Nuclear Information System (INIS)

    Bercoff, P.G.; Bertorello, H.R.; Oliva, M.I.

    2007-01-01

    Fine particles of hematite (mean size 55 nm) were produced by ball milling a mixture of hematite and pure Fe and annealing at 1000 o C. X-ray diffraction (XRD) and Moessbauer spectroscopy show that only α-Fe 2 O 3 is present in the final product, with lattice and Moessbauer parameters that correspond to bulk hematite. ZFC and FC magnetization measurements were performed from 5 to 300 K, at different applied fields. Two magnetic regimes were observed: one at low temperatures (≤100 K) that we ascribe to the magnetic moments in the outer shell of the particles that couple to the magnetic moments in the core, and another at higher temperature that corresponds to the Morin transition, finding that the Morin temperature is T M =246 K. The memory effect is clearly observed in magnetic measurements that start from different remanence states and explained as dependent on the ordering of the magnetic moments within the particles

  13. Experimental and theoretical study of phase transitions under ball milling; Etude experimentale et modelisation des changements de phases sous broyage a haute energie

    Energy Technology Data Exchange (ETDEWEB)

    Pochet, P

    1998-12-31

    The aim of this work was to determine how phase transition s under ball-milling depend on the milling conditions and to find out if one can rationalize such transitions with the theory of driven alloys. We have chosen two phase transitions: the order-disorder transition in Fe Al and the precipitation-dissolution NiGe. In the case of Fe Al we have found that the steady-state long range order parameter achieved under ball milling intensity; moreover the same degree of order is achieved starting from an ordered alloy or a disordered solid solution. On the way to fully disordered state the degree of order either decreases monotonically or goes through a short lived transient state. This behaviour is reminiscent of a first order transition while the equilibrium transition is second order. All the above features are well reproduced by a simple model of driven alloys, which was originally build for alloys under irradiation. The stationary degree of order results of two competitive atomic jump mechanisms: the forced displacements induced by the shearing of the grains, and the thermally activated jumps caused by vacancies migrations. Finally we have performed atomistic simulations with a Monte Carlo kinetic algorithm, which revealed the role of the fluctuations in the intensity of the forcing. Moreover we have shown that specific atomistic mechanisms are active in a dilute NiGe solid solution which might lead to ball milling induced precipitation in under-saturated solid solution. (author). 149 refs.

  14. Experimental and theoretical study of phase transitions under ball milling; Etude experimentale et modelisation des changements de phases sous broyage a haute energie

    Energy Technology Data Exchange (ETDEWEB)

    Pochet, P

    1997-12-31

    The aim of this work was to determine how phase transition s under ball-milling depend on the milling conditions and to find out if one can rationalize such transitions with the theory of driven alloys. We have chosen two phase transitions: the order-disorder transition in Fe Al and the precipitation-dissolution NiGe. In the case of Fe Al we have found that the steady-state long range order parameter achieved under ball milling intensity; moreover the same degree of order is achieved starting from an ordered alloy or a disordered solid solution. On the way to fully disordered state the degree of order either decreases monotonically or goes through a short lived transient state. This behaviour is reminiscent of a first order transition while the equilibrium transition is second order. All the above features are well reproduced by a simple model of driven alloys, which was originally build for alloys under irradiation. The stationary degree of order results of two competitive atomic jump mechanisms: the forced displacements induced by the shearing of the grains, and the thermally activated jumps caused by vacancies migrations. Finally we have performed atomistic simulations with a Monte Carlo kinetic algorithm, which revealed the role of the fluctuations in the intensity of the forcing. Moreover we have shown that specific atomistic mechanisms are active in a dilute NiGe solid solution which might lead to ball milling induced precipitation in under-saturated solid solution. (author). 149 refs.

  15. Structural evolution of Ni-20Cr alloy during ball milling of elemental powders

    International Nuclear Information System (INIS)

    Lopez B, I.; Trapaga M, L. G.; Martinez F, E.; Zoz, H.

    2011-01-01

    The ball milling (B M) of blended Ni and Cr elemental powders was carried out in a Simoloyer performing on high-energy scale mode at maximum production to obtain a nano structured Ni-20Cr alloy. The phase transformations and structural changes occurring during mechanical alloying were investigated by X-ray diffraction (XRD) and optical microscopy (Om). A gradual solid solubility of Cr and the subsequent formation of crystalline metastable solid solutions described in terms of the Avrami-Ero fe ev kinetics model were calculated. The XRD analysis of the structure indicates that cumulative lattice strain contributes to the driving force for solid solution between Ni and Cr during B M. Microstructure evolution has shown, additionally to the lamellar length refinement commonly observed, the folding of lamellae in the final processing stage. Om observations revealed that the lamellar spacing of Ni rich zones reaches a steady value near 500 nm and almost disappears after 30 h of milling. (Author)

  16. Structural evolution of Ni-20Cr alloy during ball milling of elemental powders

    Energy Technology Data Exchange (ETDEWEB)

    Lopez B, I.; Trapaga M, L. G. [IPN, Centro de Investigacion y de Estudios Avanzados, Unidad Queretaro, Libramiento Norponiente No. 2000, Juriquilla, 76230 Queretaro (Mexico); Martinez F, E. [Centro de Investigacion e Innovacion Tecnologica, Cerrada de Cecati s/n, Col. Santa Catarina Azcapotzalco, 02250 Mexico D. F. (Mexico); Zoz, H., E-mail: israelbaez@gmail.co [Zoz GmbH, D-57482, Wenden (Germany)

    2011-07-01

    The ball milling (B M) of blended Ni and Cr elemental powders was carried out in a Simoloyer performing on high-energy scale mode at maximum production to obtain a nano structured Ni-20Cr alloy. The phase transformations and structural changes occurring during mechanical alloying were investigated by X-ray diffraction (XRD) and optical microscopy (Om). A gradual solid solubility of Cr and the subsequent formation of crystalline metastable solid solutions described in terms of the Avrami-Ero fe ev kinetics model were calculated. The XRD analysis of the structure indicates that cumulative lattice strain contributes to the driving force for solid solution between Ni and Cr during B M. Microstructure evolution has shown, additionally to the lamellar length refinement commonly observed, the folding of lamellae in the final processing stage. Om observations revealed that the lamellar spacing of Ni rich zones reaches a steady value near 500 nm and almost disappears after 30 h of milling. (Author)

  17. Performance comparison between crystalline and co-amorphous salts of indomethacin-lysine

    DEFF Research Database (Denmark)

    Kasten, Georgia; Nouri, Khatera; Grohganz, Holger

    2017-01-01

    The introduction of a highly water soluble amino acid as co-amorphous co-former has previously been shown to significantly improve the dissolution rate of poorly water soluble drugs. In this work, dry ball milling (DBM) and liquid assisted grinding (LAG) were used to prepare different physical...... forms of salts of indomethacin (IND) with the amino acid lysine (LYS), allowing the direct comparison of their solid-state properties to their in vitro performance. X-ray powder diffraction and Fourier-transformed infrared spectroscopy showed that DBM experiments led to the formation of a fully co......-amorphous salt, while LAG resulted in a crystalline salt. Differential scanning calorimetry showed that the samples prepared by DBM had a single glass transition temperature (Tg) of approx. 100°C for the co-amorphous salt, while a new melting point (223°C) was obtained for the crystalline salt prepared by LAG...

  18. Morphology and magnetic properties of CeCo{sub 5} submicron flakes prepared by surfactant-assisted high-energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, J.J.; Gao, H.M.; Yan, Y.; Bai, X.; Su, F.; Wang, W.Q. [State key Laboratory for Superhard Materials and Department of Physics, Jilin University, Changchun 130012 (China); Du, X.B., E-mail: duxb@jlu.edu.cn [State key Laboratory for Superhard Materials and Department of Physics, Jilin University, Changchun 130012 (China)

    2012-10-15

    CeCo{sub 5} permanent magnetic alloy has been processed by surfactant assisted high energy ball milling. Heptane and oleic acid were used as the solvent and surfactant, respectively. The amount of surfactant used was 50% by weight of the starting powder. The produced particles were deposited on a piece of copper (4 mm in length and width) under a magnetic field of 27 kOe applied along the copper surface and immobilized by ethyl {alpha}-cyanoacrylate. Scanning electron microscope pictures show that the particles are flakes, several {mu}m in length and width and tens of nm in thickness. X-ray diffraction patterns and magnetic measurements prove that the flakes are crystalline with c-axes magnetic anisotropy. The easy magnetization axis is oriented perpendicular to the surface of the flake. A maximum coercivity of 3.3 kOe was obtained for the sample milled for 40 min. - Highlights: Black-Right-Pointing-Pointer CeCo{sub 5} permanent magnetic alloy has been processed by surfactant assisted high energy ball milling (HEBM). Black-Right-Pointing-Pointer The particles show a flake-like morphology with several {mu}m in length and width and tens nm in thickness. Black-Right-Pointing-Pointer The flakes are crystallographic and magnetic anisotropic and the c-axes, also the easy magnetization directions are oriented perpendicular to the surface of the flake. Black-Right-Pointing-Pointer Maximum coercivity of 3.3 kOe has been obtained for the sample milled for 40 min.

  19. Behaviour of CaO coating of gas atomized Mg powders using mechanical milling process

    International Nuclear Information System (INIS)

    Kim, Sun-Mi; Kim, Yong Hwan; Kim, Young Do; Kim, Taek-Soo

    2011-01-01

    Highlights: → This work is very new, since behaviour of CaO coating with milling time as desulfurizer is not frequently reported. → The manuscript reports the new manner of Mg powders desulfurizer development by the innovative process. - Abstract: In order to synthesize a thermally stable Mg powder as a desulfurizer of iron, pure Mg was gas atomized to powders and coated by CaO powders, to produce a thermally stable desulfurizer using a mechanical milling process. Since the effect of desulfurization is dependent on the degree of surface modification, coating behaviours such as the size, morphology and layer thickness were investigated as a function of milling condition. As the milling conducted from 10 min to 30 min, 1 h, 3 h, 6 h, 12 h, CaO particles began to stick on the surface of Mg powders. The layer of CaO formed from 1 h milling was about 17 μm thick and gradually thickened to be 28 μm, 32 μm and 37 μm with increasing the milling time to 3 h, 6 h and 12 h, respectively. The shape of coated powder became more spherical after 1 h milling, being mostly spherical after 6 h. Desulfurization rate and uniformity were evaluated for the various thickness of the coating layer.

  20. Phase evolution and thermal stability of 2 Mg–Cu alloys processed by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Martínez, C., E-mail: carola.martinezu@usach.cl [Departamento de Ingeniería Metalúrgica, Facultad de Ingeniería, Universidad de Santiago de Chile, Av. Lib. Bernardo O’Higgins 3363, Casilla de correo 10233, Santiago (Chile); Ordoñez, S., E-mail: stella.ordonez@usach.cl [Departamento de Ingeniería Metalúrgica, Facultad de Ingeniería, Universidad de Santiago de Chile, Av. Lib. Bernardo O’Higgins 3363, Casilla de correo 10233, Santiago (Chile); Guzmán, D. [Departamento de Ingeniería en Metalurgia, Facultad de Ingeniería, Universidad de Atacama y CRIDESAT, Av. Copayapu 485, Casilla de Correo 240, Copiapó (Chile); Serafini, D. [Departamento de Física, Facultad de Ciencia, Universidad de Santiago de Chile, Av. Lib. Bernardo O’Higgins 3363, Casilla de correo 307, Santiago (Chile); Iturriza, I. [CEIT, Manuel de Lardizábal 15, 20018 San Sebastián, España (Spain); Bustos, O. [Departamento de Ingeniería Metalúrgica, Facultad de Ingeniería, Universidad de Santiago de Chile, Av. Lib. Bernardo O’Higgins 3363, Casilla de correo 10233, Santiago (Chile)

    2013-12-25

    Highlights: •Study of phase evolution of elemental powders Mg and Cu by mechanical alloying. •The presence of an amorphous precursor which crystallizes to Mg{sub 2}Cu can be observed. •Establishing the sequence of phase transformations leading to the formation of Mg{sub 2}Cu. •The feasibility to obtain Mg{sub 2}Cu by means two possible routes has been established. -- Abstract: Phase evolution during mechanical alloying (MA) of elemental Mg and Cu powders and their subsequent heat treatment is studied. Elemental Mg and Cu powders in a 2:1 atomic ratio were mechanically alloyed in a SPEX 8000D mill using a 10:1 ball-to-powder ratio. X-ray diffraction (XRD) shows that the formation of the intermetallic Mg{sub 2}Cu takes place between 3 and 4 h of milling, although traces of elemental Cu are still present after 10 h of milling. The thermal behavior of different powder mixtures was evaluated by differential scanning calorimetry (DSC). The combination of DSC, heat treatment and XRD has shown a sequence of phase transformations that results in the intermetallic Mg{sub 2}Cu from an amorphous precursor. This amorphous phase is converted into Mg{sub 2}Cu by heating at low temperature (407 K). Short MA times and the formation of the amorphous precursor, together with its subsequent transformation into Mg{sub 2}Cu at low temperatures; represent an advantageous alternative route for its preparation.

  1. Determination of rational parameters for process of grinding materials pre-crushed by pressure in ball mill

    Science.gov (United States)

    Romanovich, A. A.; Romanovich, L. G.; Chekhovskoy, E. I.

    2018-03-01

    The article presents the results of experimental studies on the grinding process of a clinker preliminarily ground in press roller mills in a ball mill equipped with energy exchange devices. The authors studied the influence of the coefficients of loading for grinding bodies of the first and second mill chambers, their lengths, angles of inclination, and the mutual location of energy exchange devices (the ellipse segment and the double-acting blade) on the output parameters of the grinding process (productivity, drive power consumption and specific energy consumption). It is clarified that the best results of the disaggregation and grinding process, judging by the minimum specific energy consumption in the grinding of clinker with an anisotropic texture after force deformation between the rolls of a press roller shredder, are achieved at a certain angle of ellipse segment inclination; the length of the first chamber and the coefficients of loading the chambers with grinding bodies.

  2. Characterization of microstructure and mechanical properties of friction stir welded AlMg5- Al_2O_3 nanocomposites

    International Nuclear Information System (INIS)

    Babu, N. Kishore; Kallip, Kaspar; Leparoux, Marc; AlOgab, Khaled A.; Reddy, G.M.; Talari, M.K.

    2016-01-01

    In the present study, powder metallurgy processed unmilled AlMg5, milled AlMg5 and milled AlMg5-0.5 vol% Al_2O_3 nanocomposite have been successfully friction stir welded (FSW). The effect of friction stir welding on the evolution of weld microstructures; hardness and tensile properties were studied and discussed in detail. FSW of unmilled AlMg5 resulted in significant grain refinement and strain hardening in the nugget zone induced by the thermo-mechanical processing, thereby increasing the stir zone hardness and tensile strengths to 100 HV and 324 MPa when compared to 80 HV and 300 MPa of base metal, respectively. In contrast, the FSW of milled AlMg5 and milled AlMg5-0.5 vol% Al_2O_3 samples showed a reduction in UTS values to 375 MPa and 401 MPa in the stir zone compared to 401 MPa and 483 MPa of respective base metal values. Transmission electron microscopic (TEM) investigation of weld stir zones revealed the homogenous distribution of Al_4C_3 nanophases in milled AlMg5 and Al_2O_3 nanoparticles in milled AlMg5-0.5 vol% Al_2O_3 samples throughout the aluminium matrix. It was revealed that the pre-stored energy from the prior ball milling and hot pressing processes, higher deformation energy and grain boundary pinning effect due to the presence of reinforcement particles has resulted in a higher recrystallization tendency and retarded grain growth during FSW of milled samples. The welds prepared with milled AlMg5-0.5 vol% Al_2O_3 exhibited higher hardness and tensile strength in the stir zone when compared to all other conditions which was attributed to Hall Petch effect due to fine grain size and Orowan strengthening effect due to Al_2O_3 reinforcements.

  3. Abridged acid-base wet-milling synthesis of high purity hydroyapatite

    Directory of Open Access Journals (Sweden)

    Sandi Carolina Ruiz-Mendoza

    2008-06-01

    Full Text Available There is a plethora of routes to produce hydroxyapatite(HA and in general calcium phosphates(CP but production usually leads to a mixture of several phases. Besides ionic contamination, most of these methods are cumbersome, restricted to small volumes of product and require a lot of thermal energy. The acid-base route eliminates foreign ions or additives and its only byproduct is water. Heterogeneous reaction drawback is that solid reactants do not easily come in contact with each other and therefore addition and stirring times become very lengthy and still the product is a mixture. The synthesis started from calcium hydroxide and phosphoric acid (PA. Ball milling was used to favor kinetics and stoichiometry. Six sets of PA addition, paddle stirring and ball milling times were used. Products were evaluated by X ray diffraction (XRD, Fourier Transform Infrared (FTIR, scanning electron microscopy (SEM, X ray fluorescence (XRF and Ca/P ratio. Chemical analysis for calcium proceeded through oxalate precipitate and phosphorus by the phosphomolibdate technique. A set of conditions yielding high purity HA was established.

  4. The Effect of Toluene Solution on the Hydrogen Absorption of the Mg-Ti Alloy Prepared by Synthetic Alloying

    Directory of Open Access Journals (Sweden)

    H. Suwarno

    2009-07-01

    Full Text Available The synthesis and characterization of the Mg–Ti alloy have been carried out through a mechanical alloying technique under toluene solution. The Mg and Ti powders are milled for 10, 20, and 30 h in a high energy ball mill. The milled alloys are then hydrided at a temperature of 300 oC in order to investigate the possibility used for hydrogen storage materials. The refinement analyses of the x-ray diffraction patterns show that mechanical alloying of the Mg–Ti powders under toluene solution results in the formation of the TiH2 and Mg2Ti phases. Quantitative analyses indicate that the mass fractions of the TiH2 and Mg2Ti phases are 62.90 % and 30.60 %, while the value for Mg and Ti amount to 2.6 wt% and 1.25 wt%. On hydriding at a temperature of 300 oC, the milled powders are transformed into Mg2TiH4, TiH2 and γ-MgH2 phases with the mass fractions of 25.48 wt%, 64.0 wt%, and 10.52 wt%, respectively. Microstructure analyses show that before milling the shape of particle is mostly a ball shape, after 30 h of milling the shape of particles changes into polygonal shape, and upon hydriding the shape of particles changes from a polygonal shape into an irregular one. The final composition of the specimen after hydriding exhibits that Mg-Ti alloy can be promoted as a hydrogen storage material.

  5. Influence of B4C-doping and high-energy ball milling on phase formation and critical current density of (Bi,Pb)-2223 HTS

    Science.gov (United States)

    Margiani, N. G.; Mumladze, G. A.; Adamia, Z. A.; Kuzanyan, A. S.; Zhghamadze, V. V.

    2018-05-01

    In this paper, the combined effects of B4C-doping and planetary ball milling on the phase evolution, microstructure and transport properties of Bi1.7Pb0.3Sr2Ca2Cu3Oy(B4C)x HTS with x = 0 ÷ 0.125 were studied through X-ray diffraction (XRD), scanning electron microscopy (SEM), resistivity and critical current density measurements. Obtained results have shown that B4C additive leads to the strong acceleration of high-Tc phase formation and substantial enhancement in Jc. High-energy ball milling seems to produce a more homogeneous distribution of refined doped particles in the (Bi,Pb)-2223 HTS which results in an improved intergranular flux pinning and better self-field Jc performance.

  6. Characterization of steel 70XL used in the manufacture of balls for the clinker's milling

    Directory of Open Access Journals (Sweden)

    Eider Gresesqui-Lobaina

    2017-10-01

    Full Text Available The present article deals with the wear of the balls used for the grinding of the clinker in the processes of obtaining cement. Three specimens of different steel were made: one of steel AISI 4140, with which balls are forged for the milling process; another 70XL steel (70 XL with normalized, tempered and tempered thermal treatments; and the third, of equal material that the second but without treatment. For the metallographic observation the samples were made with dimensions of 10 mm in diameter and 8 mm in thickness, revealing for AISI 4140 steel a structure of martensitic type with some presence of acicular ferrite. For the 70XL steel without heat treatment the presence of ferrite and cementite was observed, while the steel 70XL with heat treatment showed in the limits of free cementite grain in a pearly matrix, which resulted in a higher hardness (up to HRC 59 , 8 and lower gravimetric wear compared to other materials. Therefore it is recommended as the most suitable for the manufacture of balls for grinding minerals 70XL steel with heat treatment.

  7. Preparation and Cycling Performance of Iron or Iron Oxide Containing Amorphous Al-Li Alloys as Electrodes

    Directory of Open Access Journals (Sweden)

    Franziska Thoss

    2014-12-01

    Full Text Available Crystalline phase transitions cause volume changes, which entails a fast destroying of the electrode. Non-crystalline states may avoid this circumstance. Herein we present structural and electrochemical investigations of pre-lithiated, amorphous Al39Li43Fe13Si5-powders, to be used as electrode material for Li-ion batteries. Powders of master alloys with the compositions Al39Li43Fe13Si5 and Al39Li43Fe13Si5 + 5 mass-% FeO were prepared via ball milling and achieved amorphous/nanocrystalline states after 56 and 21.6 h, respectively. In contrast to their Li-free amorphous pendant Al78Fe13Si9, both powders showed specific capacities of about 400 and 700 Ah/kgAl, respectively, after the third cycle.

  8. Application of mechanical alloying to synthesis of intermetallic phases based alloys

    International Nuclear Information System (INIS)

    Dymek, S.

    2001-01-01

    Mechanical alloying is the process of synthesis of powder materials during milling in high energetic mills, usually ball mills. The central event in mechanical alloying is the ball-powder-ball collision. Powder particles are trapped between the colliding balls during milling and undergo deformation and/or fracture. Fractured parts are cold welded. The continued fracture and cold welding results in a uniform size and chemical composition of powder particles. The main applications of mechanical alloying are: processing of ODS alloys, syntheses of intermetallic phases, synthesis of nonequilibrium structures (amorphous alloys, extended solid solutions, nanocrystalline, quasi crystals) and magnetic materials. The present paper deals with application of mechanical alloying to synthesis Ni A l base intermetallic phases as well as phases from the Nb-Al binary system. The alloy were processed from elemental powders. The course of milling was monitored by scanning electron microscopy and X-ray diffraction. After milling, the collected powders were sieved by 45 μm grid and hot pressed (Nb alloys and NiAl) or hot extruded (NiAl). The resulting material was fully dense and exhibited fine grain (< 1 μm) and uniform distribution of oxide dispersoid. The consolidated material was compression and creep tested. The mechanical properties of mechanically alloys were superior to properties of their cast counterparts both in the room and elevated temperatures. Higher strength of mechanically alloyed materials results from their fine grains and from the presence of dispersoid. At elevated temperatures, the Nb-Al alloys have higher compression strength than NiAl-based alloys processed at the same conditions. The minimum creep rates of mechanically alloyed Nb alloys are an order of magnitude lower than analogously processed NiAl-base alloys. (author)

  9. Fabrication, characterization and application of Cu{sub 2}ZnSn(S,Se){sub 4} absorber layer via a hybrid ink containing ball milled powders

    Energy Technology Data Exchange (ETDEWEB)

    Li, Chunran [State Key Laboratory of Superhard Materials and College of Physics, Jilin University, Changchun 130023 (China); Key Laboratory of Physics and Technology for Advanced Batteries (Ministry of Education), College of Physics, Jilin University, Changchun 130012 (China); College of Mathematics and Physics, Bohai University, Jinzhou 121013 (China); Yao, Bin, E-mail: binyao@jlu.edu.cn [State Key Laboratory of Superhard Materials and College of Physics, Jilin University, Changchun 130023 (China); Key Laboratory of Physics and Technology for Advanced Batteries (Ministry of Education), College of Physics, Jilin University, Changchun 130012 (China); Li, Yongfeng, E-mail: liyongfeng@jlu.edu.cn [Key Laboratory of Physics and Technology for Advanced Batteries (Ministry of Education), College of Physics, Jilin University, Changchun 130012 (China); Xiao, Zhenyu [State Key Laboratory of Superhard Materials and College of Physics, Jilin University, Changchun 130023 (China); Ding, Zhanhui [Key Laboratory of Physics and Technology for Advanced Batteries (Ministry of Education), College of Physics, Jilin University, Changchun 130012 (China); Zhao, Haifeng; Zhang, Ligong; Zhang, Zhenzhong [State Key Laboratory of Luminescence and Applications, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, No. 3888 Dongnanhu Road, Changchun 130033 (China)

    2015-09-15

    Highlights: • CZTS powders are prepared from binary sulfides by a low cost ball milling process. • Elaborated on phase evolution and formation mechanism of CZTS. • Proposed a hybrid ink approach to resolve difficulty in deposition of CZTS film. • CZTSSe solar cells with highest efficiency of 4.2% are fabricated. • Small-grained CZTS layer hinders the collection of minority carriers. - Abstract: Cu{sub 2}ZnSnS{sub 4} (CZTS) powder with kesterite structure was prepared by ball milling of mixture of Cu{sub 2}S, ZnS and SnS{sub 2} powders for more than 15 h. By dispersing the milled CZTS powder in a Cu-, Zn- and Sn-chalcogenide precursor solution, a hybrid ink was fabricated. With the hybrid ink, a precursor CZTS film was deposited on Mo coated soda-lime glass by spin-coating. In order to obtain Cu{sub 2}ZnSn(S,Se){sub 4} (CZTSSe) absorber film with kesterite structure, the CZTS film was annealed at 560 °C for 15 min in Se ambient. It is demonstrated that the annealed film is dominated by a thick layer of kesterite CZTSSe with larger grain size and Cu{sub 8}Fe{sub 3}Sn{sub 2}(S,Se){sub 12} impurity phase with the exception of a very thin layer of kesterite CZTS with smaller grain size at interface between the CZTSSe and Mo layers. Solar cell device was fabricated by using the annealed CZTSSe film as absorber layer, and its conversion efficiency reached 4.2%. Mechanism of formation of the kesterite CZTS powder and CZTSSe film as well as effect of impurity phases on conversion efficiency are discussed in the present paper. The present results suggest that the hybrid ink approach combining with ball milling is a simple, low cost and promising method for preparation of kesterite CZTSSe absorber film and CZTSSe-based solar cell.

  10. Effects of Ni-5%RExOy Composite Additives on Electrochemical Hydrogen Storage Performances of Mg2Ni

    Directory of Open Access Journals (Sweden)

    ZHANG Guo-fang

    2017-11-01

    Full Text Available The Ni-5%RExOy (CeO2, La2O3, Eu2O3 as composite additives, Mg2Ni-Ni-5%RExOy composites were prepared by the ball milling method. The effects of different additives on the structure, morphology, electrochemistry and kinetic properties of Mg2Ni alloy were studied systematically. The results show that composite additives can improve the proportion of amorphous and nanocrystalline structure of Mg2Ni alloy. The particle size is homogeneous but the agglomeration is observed in the sample with Ni-5%CeO2 additives. The composites with additives show higher maximum discharge capacity and better cycle stabilities. All of these three kinds of composite additives can improve the kinetic properties of the composites effectively, including optimizing the charge-transfer ability, the reversibility of the electrochemical reaction on the alloy surface, and enhancing the diffusion coefficients of H atoms in the bulk of alloy. Among these three kinds of additives, Ni-5%CeO2 additive shows the best catalysis effect on promoting the kinetic properties of the composites.

  11. Improved dehydriding property of polyvinylpyrrolidone coated Mg-Ni hydrogen storage nano-composite prepared by hydriding combustion synthesis and wet mechanical milling

    Directory of Open Access Journals (Sweden)

    Linglong Yao

    2018-02-01

    Full Text Available In this work, polyvinylpyrrolidone (PVP coated Mg95Ni5 nano-composites were prepared by hydriding combustion synthesis (HCS plus wet mechanical milling (WM with tetrahydrofuran (THF and donated as WM-x wt% PVP (x = 1, 3, 5 and 7 respectively. The phase compositions, microstructures and dehydriding property, as well as the co-effect of PVP and THF were investigated in detail. XRD results showed that the average crystal size of MgH2 in the milled Mg95Ni5 decreased from 23 nm without PVP to 18 nm with 1 wt% PVP. The peak temperature of dehydrogenation of MgH2 in the milled Mg95Ni5 decreased from 293.0 °C without THF to 250.4 °C with THF. The apparent activation energy for decomposition of MgH2 in WM-7 wt% PVP was estimated to be 66.94 kJ/mol, which is 37.70 kJ/mol lower than that of milled Mg95Ni5 without THF and PVP. PVP and THF can facilitate the refinement of particle size during mechanical milling process. Attributed to small particle sizes and synergistic effect of PVP and THF, the composites exhibit markedly improved dehydriding properties. Keywords: Mg-Ni-PVP, Composite, Mg-based alloy, Wet mechanical milling, Dehydriding temperature

  12. NdFeB nanoparticles prepared by wet-milling

    Energy Technology Data Exchange (ETDEWEB)

    Thielsch, Juliane; Lyubina, Julia; Woodcock, Thomas; Schultz, Ludwig; Gutfleisch, Oliver [IFW Dresden (Germany)

    2010-07-01

    Since the prediction of a giant energy product of textured nanocomposite magnets those materials where believed to be the next generation of permanent magnets. For effective exchange-coupling in such two-phase magnets grain sizes need to be in the range of the domain wall width of the hard magnetic phase. That makes a homogenous phase distribution and a microstructure with nanograins necessary. One option of preparing such materials is the synthesis of magnetic nanoparticles which further could be aligned and compacted to a bulk magnet. For this we performed wet-milling experiments of a NdFeGaNbB alloy. XRD studies revealed that by using a surfactant and a solvent during the high energy ball milling process amorphization sets in later than compared to dry milling experiments under the same conditions. Dynamic Light Scattering investigations showed a Gauss distribution of the particle size with a mean diameter of about 12nm which was also proven by TEM. Magnetic properties were measured with SQUID and showed so far rather poor coercivity values.

  13. Recycling process for recovery of gallium from GaN an e-waste of LED industry through ball milling, annealing and leaching.

    Science.gov (United States)

    Swain, Basudev; Mishra, Chinmayee; Kang, Leeseung; Park, Kyung-Soo; Lee, Chan Gi; Hong, Hyun Seon

    2015-04-01

    Waste dust generated during manufacturing of LED contains significant amounts of gallium and indium, needs suitable treatment and can be an important resource for recovery. The LED industry waste dust contains primarily gallium as GaN. Leaching followed by purification technology is the green and clean technology. To develop treatment and recycling technology of these GaN bearing e-waste, leaching is the primary stage. In our current investigation possible process for treatment and quantitative leaching of gallium and indium from the GaN bearing e-waste or waste of LED industry dust has been developed. To recycle the waste and quantitative leaching of gallium, two different process flow sheets have been proposed. In one, process first the GaN of the waste the LED industry dust was leached at the optimum condition. Subsequently, the leach residue was mixed with Na2CO3, ball milled followed by annealing, again leached to recover gallium. In the second process, the waste LED industry dust was mixed with Na2CO3, after ball milling and annealing, followed acidic leaching. Without pretreatment, the gallium leaching was only 4.91 w/w % using 4M HCl, 100°C and pulp density of 20g/L. After mechano-chemical processing, both these processes achieved 73.68 w/w % of gallium leaching at their optimum condition. The developed process can treat and recycle any e-waste containing GaN through ball milling, annealing and leaching. Copyright © 2015 Elsevier Inc. All rights reserved.

  14. The reduction of optimal heat treatment temperature and critical current density enhancement of ex situ processed MgB2 tapes using ball milled filling powder

    Science.gov (United States)

    Fujii, Hiroki; Iwanade, Akio; Kawada, Satoshi; Kitaguchi, Hitoshi

    2018-01-01

    The optimal heat treatment temperature (Topt) at which best performance in the critical current density (Jc) property at 4.2 K is obtained is influenced by the quality or reactivity of the filling powder in ex situ processed MgB2 tapes. Using a controlled fabrication process, the Topt decreases to 705-735 °C, which is lower than previously reported by more than 50 °C. The Topt decrease is effective to suppress both the decomposition of MgB2 and hence the formation of impurities such as MgB4, and the growth of crystallite size which decreases upper critical filed (Hc2). These bring about the Jc improvement and the Jc value at 4.2 K and 10 T reaches 250 A/mm2. The milling process also decreases the critical temperature (Tc) below 30 K. The milled powder is easily contaminated in air and thus, the Jc property of the contaminated tapes degrades severely. The contamination can raise the Topt by more than 50 °C, which is probably due to the increased sintering temperature required against contaminated surface layer around the grains acting as a barrier.

  15. Influence of spark plasma sintering conditions on the sintering and functional properties of an ultra-fine grained 316L stainless steel obtained from ball-milled powder

    Energy Technology Data Exchange (ETDEWEB)

    Keller, C., E-mail: clement.keller@insa-rouen.fr [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Tabalaiev, K.; Marnier, G. [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Noudem, J. [Laboratoire de Cristallographie des Matériaux, CNRS-UMR 6508, Université de Caen, ENSICAEN, 7 bd du Maréchal Juin, 14050 Caen (France); Sauvage, X. [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Hug, E. [Laboratoire de Cristallographie des Matériaux, CNRS-UMR 6508, Université de Caen, ENSICAEN, 7 bd du Maréchal Juin, 14050 Caen (France)

    2016-05-17

    In this work, 316L samples with submicrometric grain size were sintered by spark plasma sintering. To this aim, 316L powder was first ball-milled with different conditions to obtain nanostructured powder. The process control agent quantity and milling time were varied to check their influence on the crystallite size of milled powder. Samples were then sintered by spark plasma sintering using different sets of sintering parameters (temperature, dwell time and pressure). For each sample, grain size and density were systematically measured in order to investigate the influence of the sintering process on these two key microstructure parameters. Results show that suitable ball-milling and subsequent sintering can be employed to obtain austenitic stainless steel samples with grain sizes in the nanometer range with porosity lower than 3%. However, ball-milling and subsequent sintering enhance chromium carbides formation at the sample surface in addition to intragranular and intergranular oxides in the sample as revealed by X-ray diffraction and transmission electron microscopy. It has been shown that using Boron nitride together with graphite foils to protect the mold from powder welding prevent such carbide formation. For mechanical properties, results show that the grain size refinement strongly increases the hardness of the samples without deviation from Hall-Petch relationship despite the oxides formation. For corrosion resistance, grain sizes lower than a few micrometers involve a strong decrease in the pitting potential and a strong increase in passivation current. As a consequence, spark plasma sintering can be considered as a promising tool for ultra-fine grained austenitic stainless steel.

  16. Improved hydrogen storage properties of MgH2 catalyzed with TiO2

    Science.gov (United States)

    Jangir, Mukesh; Meena, Priyanka; Jain, I. P.

    2018-05-01

    In order to improve the hydrogenation properties of the MgH2, various concentration of rutile Titanium Oxide (TiO2) (X wt%= 5, 10, 15 wt %) is added to MgH2 by ball milling and the catalytic effect of TiO2 on hydriding/dehydriding properties of MgH2 has been investigated. Result shows that the TiO2 significantly reduced onset temperature of desorption. Onset temperature as low as 190 °C were observed for the MgH2-15 wt% TiO2 sample which is 60 °C and 160 °C lower than the as-milled and as-received MgH2. Fromm the Kissinger plot the activation energy of 15 wt% TiO2 added sample is calculated to be -75.48 KJ/mol. These results indicate that the hydrogenation properties of MgH2-TiO2 have been improved compared to the as-milled and as-received MgH2. Furthermore, XRD and XPS were performed to characterize the structural evolution upon milling and dehydrogenation.

  17. Highly Al-doped TiO{sub 2} nanoparticles produced by Ball Mill Method: structural and electronic characterization

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Desireé M. de los, E-mail: desire.delossantos@uca.es; Navas, Javier, E-mail: javier.navas@uca.es; Sánchez-Coronilla, Antonio; Alcántara, Rodrigo; Fernández-Lorenzo, Concha; Martín-Calleja, Joaquín

    2015-10-15

    Highlights: • Highly Al-doped TiO{sub 2} nanoparticles were synthesized using a Ball Mill Method. • Al doping delayed anatase to rutile phase transformation. • Al doping allow controlling the structural and electronic properties of nanoparticles. - Abstract: This study presents an easy method for synthesizing highly doped TiO{sub 2} nanoparticles. The Ball Mill method was used to synthesize pure and Al-doped titanium dioxide, with an atomic percentage up to 15.7 at.% Al/(Al + Ti). The samples were annealed at 773 K, 973 K and 1173 K, and characterized using ICP-AES, XRD, Raman spectroscopy, FT-IR, TG, STEM, XPS, and UV–vis spectroscopy. The effect of doping and the calcination temperature on the structure and properties of the nanoparticles were studied. The results show high levels of internal doping due to the substitution of Ti{sup 4+} ions by Al{sup 3+} in the TiO{sub 2} lattice. Furthermore, anatase to rutile transformation occurs at higher temperatures when the percentage of doping increases. Therefore, Al doping allows us to control the structural and electronic properties of the nanoparticle synthesized. So, it is possible to obtain nanoparticles with anatase as predominant phase in a higher range of temperature.

  18. Synthesis of stoichiometric Ca{sub 2}Fe{sub 2}O{sub 5} nanoparticles by high-energy ball milling and thermal annealing

    Energy Technology Data Exchange (ETDEWEB)

    Amorim, B.F.; Morales, M.A.; Bohn, F.; Carriço, A.S. [Departamento de Física Teórica e Experimental, Universidade Federal do Rio Grande do Norte, 59078-900 Natal, RN (Brazil); Medeiros, S.N. de, E-mail: sndemedeiros@gmail.com [Departamento de Física Teórica e Experimental, Universidade Federal do Rio Grande do Norte, 59078-900 Natal, RN (Brazil); Dantas, A.L. [Departamento de Física, Universidade do Estado do Rio Grande do Norte, 59610-210 Mossoró, RN (Brazil)

    2016-05-01

    We report the synthesis of Ca{sub 2}Fe{sub 2}O{sub 5} nanoparticles by high-energy ball milling and thermal annealing from α-Fe{sub 2}O{sub 3} and CaCO{sub 3}. Magnetization measurements, Mössbauer and X-ray spectra reveal that annealing at high temperatures leads to better quality samples. Our results indicate nanoparticles produced by 10 h high-energy ball milling and thermal annealing for 2 h at 1100 °C achieve improved stoichiometry and the full weak ferromagnetic signal of Ca{sub 2}Fe{sub 2}O{sub 5}. Samples annealed at lower temperatures show departure from stoichiometry, with a higher occupancy of Fe{sup 3+} in octahedral sites, and a reduced magnetization. Thermal relaxation for temperatures in the 700–1100 °C range is well represented by a Néel model, assuming a random orientation of the weak ferromagnetic moment of the Ca{sub 2}Fe{sub 2}O{sub 5} nanoparticles.

  19. The incredible shrinking ball

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Maurice

    2011-12-15

    In the oil and gas industry, the implementation of fracture systems using ball and seat technology helped make multistage fracturing possible. However, frac balls can obstruct later production flow by staying in the well. Baker Hughes Inc. developed a technology to solve this problem: IN-Tallic frac balls. The unique feature of these frac balls is that they are made of an electrolytic metallic nanostructured material which is light and strong and which melts away with salt water or brine through a decomposition process governed by electrochemical reactions controlled by nanoscale coatings. These balls need to be kept away from moisture in order to prevent degradation. This technology is more expensive than traditional frac balls but it prevents the need to mill out obstructions created by the balls. The IN-Tallic frac balls are a new technology which provides operators with peace of mind.

  20. Unraveling the synthesis of homoleptic [Ag(N,N-diaryl-NHC)2]Y (Y = BF4, PF6) complexes by ball-milling.

    Science.gov (United States)

    Beillard, Audrey; Bantreil, Xavier; Métro, Thomas-Xavier; Martinez, Jean; Lamaty, Frédéric

    2016-11-28

    A user-friendly and general mechanochemical method was developed to access rarely described NHC (N-heterocyclic carbene) silver(i) complexes featuring N,N-diarylimidazol(idin)ene ligands and non-coordinating tetrafluoroborate or hexafluorophosphate counter anions. Comparison with syntheses in solution clearly demonstrated the superiority of the ball-milling conditions.

  1. Real/binary co-operative and co-evolving swarms based multivariable PID controller design of ball mill pulverizing system

    International Nuclear Information System (INIS)

    Menhas, Muhammad Ilyas; Fei Minrui; Wang Ling; Qian Lin

    2012-01-01

    Highlights: ► We extend the concept of co-operation and co-evolution in some PSO variants. ► We use developed co-operative PSOs in multivariable PID controller design/tuning. ► We find that co-operative PSOs converge faster and give high quality solutions. ► Dividing the search space among swarms improves search efficiency. ► The proposed methods allow the practitioner for heterogeneous problem formulation. - Abstract: In this paper, multivariable PID controller design based on cooperative and coevolving multiple swarms is demonstrated. A simplified multi-variable MIMO process model of a ball mill pulverizing system with steady state decoupler is considered. In order to formulate computational models of cooperative and coevolving multiple swarms three different algorithms like real coded PSO, discrete binary PSO (DBPSO) and probability based discrete binary PSO (PBPSO) are employed. Simulations are carried out on three composite functions simultaneously considering multiple objectives. The cooperative and coevolving multiple swarms based results are compared with the results obtained through single swarm based methods like real coded particle swarm optimization (PSO), discrete binary PSO (DBPSO), and probability based discrete binary PSO (PBPSO) algorithms. The cooperative and coevolving swarms based techniques outperform the real coded PSO, PBPSO, and the standard discrete binary PSO (DBPSO) algorithm in escaping from local optima. Furthermore, statistical analysis of the simulation results is performed to calculate the comparative reliability of various techniques. All of the techniques employed are suitable for controller tuning, however, the multiple cooperative and coevolving swarms based results are considerably better in terms of mean fitness, variance of fitness, and success rate in finding a feasible solution in comparison to those obtained using single swarm based methods.

  2. Fabrication and characterization of Cu/YSZ cermet high temperature electrolysis cathode material prepared by high-energy ball-milling method

    International Nuclear Information System (INIS)

    Lee, Sungkyu; Kim, Jong-Min; Hong, Hyun Seon; Woo, Sang-Kook

    2009-01-01

    Cu/YSZ cermet (40 and 60 vol.% Cu powder with balance YSZ) is a more economical cathode material than the conventional Ni/YSZ cermet for high temperature electrolysis (HTE) of water vapor and it was successfully fabricated by high-energy ball-milling of Cu and YSZ powders, pressing into pellets (o 13 mm x 2 mm) and subsequent sintering process at 700 deg. C under flowing 5%-H 2 /Ar gas. The Cu/YSZ composite material thus fabricated was characterized using various analytical tools such as XRD, SEM, and laser diffraction and scattering method. Electrical conductivity of sintered Cu/YSZ cermet pellets thus fabricated was measured by using 4-probe technique for comparison with that of conventional Ni/YSZ cermets. The effect of composite composition on the electrical conductivity was investigated and a marked increase in electrical conductivity for copper contents greater than 40 vol.% in the composite was explained by percolation threshold. Also, Cu/YSZ cermet was selected as a candidate for HTE cathode of self-supporting planar unit cell and its electrochemical performance was investigated, paving the way for preliminary correlation of high-energy ball-milling parameters with observed physical and electrochemical performance of Cu/YSZ cermets

  3. Effect of Stiffness of Rolling Joints on the Dynamic Characteristic of Ball Screw Feed Systems in a Milling Machine

    Directory of Open Access Journals (Sweden)

    Dazhong Wang

    2015-01-01

    Full Text Available Dynamic characteristic of ball screw feed system in a milling machine is studied numerically in this work. In order to avoid the difficulty in determining the stiffness of rolling joints theoretically, a dynamic modeling method for analyzing the feed system is discussed, and a stiffness calculation method of the rolling joints is proposed based on the Hertz contact theory. Taking a 3-axis computer numerical control (CNC milling machine set ermined as a research object, the stiffness of its fixed joint between the column and the body together with the stiffness parameters of the rolling joints is evaluated according to the Takashi Yoshimura method. Then, a finite element (FE model is established for the machine tool. The correctness of the FE model and the stiffness calculation method of the rolling joints are validated by theoretical and experimental modal analysis results of the machine tool’s workbench. Under the two modeling methods of joints incorporating the stiffness parameters and rigid connection, a theoretical modal analysis is conducted for the CNC milling machine. The natural frequencies and modal shapes reveal that the joints’ dynamic characteristic has an important influence on the dynamic performance of a whole machine tool, especially for the case with natural frequency and higher modes.

  4. The influence of pressure on the intrinsic dissolution rate of amorphous indomethacin

    DEFF Research Database (Denmark)

    Löbmann, Korbinian; Flouda, Konstantina; Qiu, Danwen

    2014-01-01

    of different compression pressures on the IDR was determined from powder compacts of amorphous (ball-milling) indomethacin (IND), a glass solution of IND and poly(vinylpyrrolidone) (PVP) and crystalline IND. Solid state properties were analyzed with X-ray powder diffraction (XRPD) and the final compacts were...... and to test the potential dissolution advantage of the amorphous form. However, neither the United States Pharmacopeia (USP) nor the European Pharmacopeia (Ph.Eur) state specific limitations for the compression pressure in order to obtain compacts for the IDR determination. In this study, the influence...... visually observed to study the effects of compaction pressure on their surface properties. It was found that there is no significant correlation between IDR and compression pressure for crystalline IND and IND-PVP. This was in line with the observation of similar surface properties of the compacts. However...

  5. Performance enhancement of NdFeB nanoflakes prepared by surfactant-assisted ball milling at low temperature by using different surfactants

    Science.gov (United States)

    An, Xiaoxin; Jin, Kunpeng; Wang, Fang; Fang, Qiuli; Du, Juan; Xia, Weixing; Yan, Aru; Liu, J. Ping; Zhang, Jian

    2017-02-01

    Hard magnetic NdFeB submicron and nanoflakes were successfully prepared by surfactant-assisted ball milling at room temperature (SABMRT) and low temperature (SABMLT) by using oleic acid (OA), oleylamine (OLA) and trioctylamine (TOA) as surfactant, respectively. Among the surfactants used, OA and OLA have similar effects on the morphology of the NdFeB nanoflakes milled at both room and low temperature. In the case of TOA, irregular micron-sized particles and submirco/nanoflakes were obtained for the NdFeB powders prepared by SABMRT and SABMLT, respectively. Samples prepared by SABMLT show better crystallinity and better degree of grain alignment than that prepared by SABMRT with the same surfactant. Comparing with the samples milled at RT, higher coercivity and larger remanence ratio were achieved in the NdFeB samples prepared at LT. The amounts of residual surfactants in final NdFeB powders were also calculated, which reveals that the final NdFeB powders milled at LT possess lower amount of residual surfactants than those milled at RT. It was found that lowering milling temperature of SABM would be a promising way for fabricating permanent magnetic materials with better hard magnetic properties.

  6. Effect of process control agent on the structural and magnetic properties of nano/amorphous Fe0.7Nb0.1Zr0.1Ti0.1 powders prepared by high energy ball milling

    Science.gov (United States)

    Khazaei Feizabad, Mohammad Hossein; Sharafi, Shahriar; Khayati, Gholam Reza; Ranjbar, Mohammad

    2018-03-01

    In this study, amorphous Fe0.7Nb0.1Zr0.1Ti0.1 alloy without metalloids was produced by mechanical alloying of pure mixture elements. Miedema's semi-empirical model was employed to predict the possibility of amorphous phase formation in proposed alloying system. The effect of Hexane as process control agent (PCA) on the structural, magnetic, morphological and thermal properties of the products was investigated. The results showed that the presence of PCA was necessary for the formation of amorphous phase as well as improved its soft magnetic properties. The PCA addition causes an increase of the saturation magnetization (about 43%) and decrease of the coercivity (about 50%). Moreover, the sample milled without PCA, showed a wide particle size distribution as well as relatively spherical geometry. While, in the presence of PCA the powders were aspherical and Polygon. In addition, the crystallization and Curie temperatures were found to be around 800 °C and 650 °C, respectively which are relatively high values for these kinds of alloys.

  7. Surface modification of calcined kaolin with toluene diisocyanate based on high energy ball milling

    International Nuclear Information System (INIS)

    Yuan, Yongbing; Chen, Hongling; Lin, Jinbin; Ji, Yan

    2013-01-01

    The surface of calcined kaolin particle was modified with toluene diisocyanate (TDI) by using high energy ball milling. The prepared hybrids were characterized by FT-IR, MAS NMR, thermal analysis (TGA-DSC), static water contact angle (CA), apparent viscosity and transmission electron microscopy (TEM). FT-IR and MAS NMR spectra demonstrated that TDI molecules were chemically anchored to kaolin surface after modification. The results of thermal analysis showed that the maximum grafting ratio reached up to 446.61% when the mass ratio of TDI/kaolin was 0.5:1.0, and CA measurements revealed that the resultant hybrids exhibited strong hydrophobicity (148.82°). Apparent viscosity and TEM were employed to examine the dispersion properties of blank and modified kaolin particles in poly (dimenthylsiloxane) matrix. The results illustrated that the dispersion stability depended strongly on the grafting ratio of TDI, neither too low nor too high achieved uniform and stable dispersion, and the favorable grafting ratio was obtained when the mass ratio of TDI/kaolin was 0.2:1.0. Further modification of TDI/kaolin (mass ration of TDI/kaolin, 1.0:1.0) particles with bis(aminopropyl)-terminated-poly(dimethylsiloxane) (APS) was also investigated. TEM evidenced that the dispersion properties of the obtained TDI/APS/kaolin particles were remarkably improved in octamethyl cyclotetrasiloxane compared with the original TDI/kaolin particles.

  8. Surface modification of calcined kaolin with toluene diisocyanate based on high energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Yongbing; Chen, Hongling, E-mail: hlchen@njut.edu.cn; Lin, Jinbin; Ji, Yan

    2013-11-01

    The surface of calcined kaolin particle was modified with toluene diisocyanate (TDI) by using high energy ball milling. The prepared hybrids were characterized by FT-IR, MAS NMR, thermal analysis (TGA-DSC), static water contact angle (CA), apparent viscosity and transmission electron microscopy (TEM). FT-IR and MAS NMR spectra demonstrated that TDI molecules were chemically anchored to kaolin surface after modification. The results of thermal analysis showed that the maximum grafting ratio reached up to 446.61% when the mass ratio of TDI/kaolin was 0.5:1.0, and CA measurements revealed that the resultant hybrids exhibited strong hydrophobicity (148.82°). Apparent viscosity and TEM were employed to examine the dispersion properties of blank and modified kaolin particles in poly (dimenthylsiloxane) matrix. The results illustrated that the dispersion stability depended strongly on the grafting ratio of TDI, neither too low nor too high achieved uniform and stable dispersion, and the favorable grafting ratio was obtained when the mass ratio of TDI/kaolin was 0.2:1.0. Further modification of TDI/kaolin (mass ration of TDI/kaolin, 1.0:1.0) particles with bis(aminopropyl)-terminated-poly(dimethylsiloxane) (APS) was also investigated. TEM evidenced that the dispersion properties of the obtained TDI/APS/kaolin particles were remarkably improved in octamethyl cyclotetrasiloxane compared with the original TDI/kaolin particles.

  9. Microstructure and kinetics evolution in MgH2–TiO2 pellets after hydrogen cycling

    International Nuclear Information System (INIS)

    Mirabile Gattia, D.; Di Girolamo, G.; Montone, A.

    2014-01-01

    Highlights: • MgH 2 was ball milled with TiO 2 anatase phase and expanded graphite to prepare pellets. • Different pellets have been prepared at different compression load. • Pellets were repeatedly cycled under hydrogen pressure to simulate tank exercise and verify their stability. • The compression load highly affects the stability of the pellets to cycling. • Microstructural evolution of the particles due to cycling have been observed. - Abstract: The interest in Mg-based hydrides for solid state hydrogen storage is associated to their capability to reversibly absorb and desorb large amounts of hydrogen. In this work MgH 2 powder with 5 wt.% TiO 2 was ball milled for 10 h. The as-milled nanostructured powder was enriched with 5 wt.% of Expanded Natural Graphite (ENG) and then compacted in cylindrical pellets by cold pressing using different loads. Both the powder and the pellets were subjected to kinetic and thermodynamic tests using a Sievert’s type gas reaction controller, in order to study the microstructural and kinetic changes which took place during repeated H 2 absorption and desorption cycles. The pellets exhibited good kinetic performance and durability, even if the pressure of compaction revealed to be an important parameter for their mechanical stability. Scanning Electron Microscopy observations of as-prepared and cycled pellets were carried out to investigate the evolution of their microstructure. In turn the phase composition before and after cycling was analyzed by X-ray diffraction

  10. Mechanism of nanostructure formation in ball-milled Cu and Cu–3wt%Zn studied by X-ray diffraction line profile analysis

    International Nuclear Information System (INIS)

    Khoshkhoo, M. Samadi; Scudino, S.; Bednarcik, J.; Kauffmann, A.; Bahmanpour, H.; Freudenberger, J.; Scattergood, R.; Zehetbauer, M.J.; Koch, C.C.; Eckert, J.

    2014-01-01

    Highlights: • Nanostructured powders of Cu and Cu–3wt%Zn were produced using ball milling. • During cryomilling, nanostructure was formed by structural decomposition. • Dynamic recrystallization happened in room–temperature milling of Cu–3wt%Zn. • Structural decomposition took place during room–temperature milling of Cu. -- Abstract: The mechanism of nanostructure formation during cryogenic and room-temperature milling of Cu and Cu–3wt%Zn was investigated using X-ray diffraction line profile analysis. For that, the whole powder pattern modeling approach (WPPM) was used to analyze the evolution of microstructural features including coherently scattering domain size, dislocation density, and density of planar faults. It was found that for all sets of experiments, structural decomposition is the dominant mechanism of nanostructure formation during cryomilling. During subsequent RT-milling, grain refinement still occurs by structural decomposition for pure copper. On the other hand, discontinuous dynamic recrystallization is responsible for nanostructure formation during RT-milling of Cu–3wt%Zn. This is attributed to lower stacking-fault energy of Cu–3wt%Zn compared to pure copper. Finally, room temperature milling reveals the occurrence of a detwinning phenomenon

  11. Formation of nanocrystalline and amorphous phase of Al-Pb-Si-Sn-Cu powder during mechanical alloying

    International Nuclear Information System (INIS)

    Ran Guang; Zhou Jingen; Xi Shengqi; Li Pengliang

    2006-01-01

    Al-15%Pb-4%Si-1%Sn-1.5%Cu alloys (mass fraction, %) were prepared by mechanical alloying (MA). Phase transformation and microstructure characteristics of the alloy powders were investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the nanocrystalline supersaturated solid solutions and amorphous phase in the powders are obtained during MA. The effect of ball milling is more evident to lead than to aluminum. During MA, the mixture powders are firstly fined, alloyed, nanocrystallized and then the nanocrystalline partly transforms to amorphous phase. A thermodynamic model is developed based on semi-experimental theory of Miedema to calculate the driving force for phase evolution. The thermodynamic analysis shows that there is no chemical driving force to form a crystalline solid solution from the elemental components. But for the amorphous phase, the Gibbs free energy is higher than 0 for the alloy with lead content in the ranges of 0-86.8 at.% and 98.4-100 at.% and lower than 0 in range of 86.8-98.4 at.%. For the Al-2.25 at.%Pb (Al-15%Pb, mass fraction, %), the driving force for formation of amorphization and nanocrystalline supersaturated solid solutions are provided not by the negative heat of mixing but by mechanical work

  12. SnSe/carbon nanocomposite synthesized by high energy ball milling as an anode material for sodium-ion and lithium-ion batteries

    International Nuclear Information System (INIS)

    Zhang, Zhian; Zhao, Xingxing; Li, Jie

    2015-01-01

    Graphical abstract: A homogeneous nanocomposite of SnSe and carbon black was synthesised by high energy ball milling and empolyed as an anode material for sodium-ion batteries (SIBs) and lithium-ion batteries (LIBs). The nanocomposite anode exhibits excellent electrochemical performances in both SIBs and LIBs. - Highlights: • A homogeneous nanocomposite of SnSe and carbon black was fabricated by high energy ball milling. • SnSe and carbon black are homogeneously mixed at the nanoscale level. • The SnSe/C anode exhibits excellent electrochemical performances in both SIBs and LIBs. - Abstract: A homogeneous nanocomposite of SnSe and carbon black, denoted as SnSe/C nanocomposite, was fabricated by high energy ball milling and empolyed as a high performance anode material for both sodium-ion batteries and lithium-ion batteries. The X-ray diffraction patterns, scanning electron microscopy and transmission electron microscopy observations confirmed that SnSe in SnSe/C nanocomposite was homogeneously distributed within carbon black. The nanocomposite anode exhibited enhanced electrochemical performances including a high capacity, long cycling behavior and good rate performance in both sodium-ion batteries (SIBs) and lithium-ion batteries (LIBs). In SIBs, an initial capacitiy of 748.5 mAh g −1 was obtained and was maintained well on cycling (324.9 mAh g −1 at a high current density of 500 mA g −1 in the 200 th cycle) with 72.5% retention of second cycle capacity (447.7 mAh g −1 ). In LIBs, high initial capacities of approximately 1097.6 mAh g −1 was obtained, and this reduced to 633.1 mAh g −1 after 100 cycles at 500 mA g −1

  13. Influence of octanoic acid on SmCo{sub 5} nanoflakes prepared by surfactant-assisted high-energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Zheng Liyun, E-mail: zheng@udel.ed [Department of Physics and Astronomy, University of Delaware, Newark, DE 19716 (United States); College of Electromechanical Engineering, Hebei University of Engineering, Handan, Hebei 056038 (China); Cui Baozhi; Akdogan, Nilay G.; Li Wanfeng; Hadjipanayis, George C. [Department of Physics and Astronomy, University of Delaware, Newark, DE 19716 (United States)

    2010-08-20

    High-energy ball milling (HEBM) of magnetically hard SmCo{sub 5} was conducted in heptane with octanoic acid as the surfactant. The effects of octanoic acid on the morphology and magnetic properties of the powders were investigated by scanning electron microscopy, X-ray diffraction and vibrating sample magnetometry. The results show an interesting unexpected fact that the SmCo{sub 5} powders processed by octanoic acid-assisted HEBM were in form of nanoflakes with aspect-ratio of 10{sup 2}-10{sup 3} without the presence of nanoparticles. The thickness of nanoflakes decreases with increasing milling time. X-ray diffraction patterns did not show the sign of oxidation and the diffraction peaks of SmCo{sub 5} were getting broader with the increase of milling time. The nanoflakes were magnetically anisotropic and had a higher coercivity than the micro-particles prepared by HEBM without surfactant. The coercivity of SmCo{sub 5} increased initially with the milling time and then it decreased after reaching the maximum value of 15.2 kOe. High-resolution transmission electron microscopy image showed that the SmCo{sub 5} nanoflakes are nanocrystalline with an average crystallite size approximately 12 nm.

  14. Continuous amorphization of Cu-Zr studied by positron lifetime

    International Nuclear Information System (INIS)

    Wilde, G.; Wuerschum, R.; Rabitsch, H.; Puff, W.

    2006-01-01

    Full text: Solid state amorphization by cold-rolling represents an attractive alternative to commonly used ball-milling. The present work aimed at a free volume study of the process of amorphization. To study the amorphization process binary Cu-Zr alloys were mechanically intermixed by cold rolling. Foils of pure Cu and Zr were stacked to form arrays of composition Cu 60 Zr 40 and folded four times. The folded samples were rolled at a strain rate of approximately 0.1 s -1 to a thickness of about 80 μm and then folded to double the thickness and rolled again to a minimum thickness of 80 μm. This procedure was repeated until the final material was cold-rolled for up to 80 passes. The microstructural changes during cold-rolling were investigated at different stages of the mechanical intermixing process by positron lifetime and 2-dimensional Doppler broadening measurements. The obtained Doppler results are discussed analysing the S-W-plot as well as a two-component fit and the shape of the ratio curves. Finally the results are compared to the lifetime results. (author)

  15. Easily recycled Bi2O3 photocatalyst coatings prepared via ball milling followed by calcination

    Science.gov (United States)

    Cheng, Lijun; Hu, Xumin; Hao, Liang

    2017-06-01

    Bi2O3 photocatalyst coatings derived from Bi coatings were first prepared by a two-step method, namely ball milling followed by the calcination process. The as-prepared samples were characterized by XRD, SEM, XPS and UV-Vis spectra, respectively. The results showed that monoclinic Bi2O3 coatings were obtained after sintering Bi coatings at 673 or 773 K, while monoclinic and triclinic mixed phase Bi2O3 coatings were obtained at 873 or 973 K. The topographies of the samples were observably different, which varied from flower-like, irregular, polygonal to nanosized particles with the increase in calcination temperature. Photodegradation of malachite green under simulated solar irradiation for 180 min showed that the largest degradation efficiency of 86.2% was achieved over Bi2O3 photocatalyst coatings sintered at 873 K. The Bi2O3 photocatalyst coatings, encapsulated with Al2O3 ball with an average diameter around 1 mm, are quite easily recycled, which provides an alternative visible light-driven photocatalyst suitable for practical water treatment application.

  16. Analysis of isothermal sintering of zinc-titanate doped with MgO

    Directory of Open Access Journals (Sweden)

    Obradović N.

    2007-01-01

    Full Text Available The aim of this work was analysis of isothermal sintering of zinc titanate ceramics doped with MgO obtained by mechanical activation. Mixtures of ZnO, TiO2 and MgO (0, 1.25 and 2.5% were mechanically activated 15 minutes in a planetary ball mill. The powders obtained were pressed under different pressures and the results were fitted with a phenomenological compacting equation. Isothermal sintering was performed in air for 120 minutes at four different temperatures. Structural characterization of ZnO-TiO2-MgO system after milling was performed at room temperature using XRPD measurements. DTA measurements showed different activation energies for pure and doped ZnO-TiO2 systems. Thus addition of MgO stabilizes the crystal structure of zinc titanate.

  17. Characterization of microstructure and mechanical properties of friction stir welded AlMg5- Al{sub 2}O{sub 3} nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Babu, N. Kishore, E-mail: kishorebabu.nagumothu@empa.ch [Empa, Swiss Federal Laboratories for Material Science and Technology, Laboratory for Advanced Materials Processing, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); Kallip, Kaspar; Leparoux, Marc [Empa, Swiss Federal Laboratories for Material Science and Technology, Laboratory for Advanced Materials Processing, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); AlOgab, Khaled A. [King Abdulaziz City for Science and Technology (KACST), National Centers for Advanced Materials, P O Box 6086, Riyadh, 11442 (Saudi Arabia); Reddy, G.M. [Defence Metallurical Research Laboratory, Hyderabad-500 058 (India); Talari, M.K. [Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam (Malaysia)

    2016-03-21

    In the present study, powder metallurgy processed unmilled AlMg5, milled AlMg5 and milled AlMg5-0.5 vol% Al{sub 2}O{sub 3} nanocomposite have been successfully friction stir welded (FSW). The effect of friction stir welding on the evolution of weld microstructures; hardness and tensile properties were studied and discussed in detail. FSW of unmilled AlMg5 resulted in significant grain refinement and strain hardening in the nugget zone induced by the thermo-mechanical processing, thereby increasing the stir zone hardness and tensile strengths to 100 HV and 324 MPa when compared to 80 HV and 300 MPa of base metal, respectively. In contrast, the FSW of milled AlMg5 and milled AlMg5-0.5 vol% Al{sub 2}O{sub 3} samples showed a reduction in UTS values to 375 MPa and 401 MPa in the stir zone compared to 401 MPa and 483 MPa of respective base metal values. Transmission electron microscopic (TEM) investigation of weld stir zones revealed the homogenous distribution of Al{sub 4}C{sub 3} nanophases in milled AlMg5 and Al{sub 2}O{sub 3} nanoparticles in milled AlMg5-0.5 vol% Al{sub 2}O{sub 3} samples throughout the aluminium matrix. It was revealed that the pre-stored energy from the prior ball milling and hot pressing processes, higher deformation energy and grain boundary pinning effect due to the presence of reinforcement particles has resulted in a higher recrystallization tendency and retarded grain growth during FSW of milled samples. The welds prepared with milled AlMg5-0.5 vol% Al{sub 2}O{sub 3} exhibited higher hardness and tensile strength in the stir zone when compared to all other conditions which was attributed to Hall Petch effect due to fine grain size and Orowan strengthening effect due to Al{sub 2}O{sub 3} reinforcements.

  18. Magnetic properties of Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} spinel ferrite nanoparticles synthesized by starch-assisted sol–gel autocombustion method and its ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Yadav, Raghvendra Singh, E-mail: yadav@fch.vutbr.cz [Materials Research Centre, Brno University of Technology, Purkyňova 464/118, 61200 Brno (Czech Republic); Havlica, Jaromir [Materials Research Centre, Brno University of Technology, Purkyňova 464/118, 61200 Brno (Czech Republic); Hnatko, Miroslav; Šajgalík, Pavol [Institute of Inorganic Chemistry, Slovak Academy of Sciences, Dúbravská cesta 9, SK-845 36 Bratislava (Slovakia); Alexander, Cigáň [Institute of Measurement Science, Slovak Academy of Sciences, Dúbravská cesta 9, SK-841 04 Bratislava (Slovakia); Palou, Martin; Bartoníčková, Eva; Boháč, Martin; Frajkorová, Františka; Masilko, Jiri; Zmrzlý, Martin; Kalina, Lukas; Hajdúchová, Miroslava; Enev, Vojtěch [Materials Research Centre, Brno University of Technology, Purkyňova 464/118, 61200 Brno (Czech Republic)

    2015-03-15

    In this article, Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (x=0.0 and 0.5) spinel ferrite nanoparticles were achieved at 800 °C by starch-assisted sol–gel autocombustion method. To further reduce the particle size, these synthesized ferrite nanoparticles were ball-milled for 2 h. X-ray diffraction patterns demonstrated single phase formation of Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (x=0.0 and 0.5) spinel ferrite nanoparticles. FE-SEM analysis indicated the nanosized spherical particles formation with spherical morphology. The change in Raman modes and relative intensity were observed due to ball milling and consequently decrease of particle size and cationic redistribution. An X-ray Photoelectron Spectroscopy (XPS) result indicated that Co{sup 2+}, Zn{sup 2+} and Fe{sup 3+} exist in octahedral and tetrahedral sites. The cationic redistribution of Zn{sup 2+} and consequently Fe{sup 3+} occurred between octahedral and tetrahedral sites after ball-milling. The change in saturation magnetization (M{sub s}) and coercivity (H{sub c}) with decrease of nanocrystalline size and distribution of cations in spinel ferrite were observed. - Highlights: • Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} spinel ferrite nanoparticles. • Starch-assisted sol–gel auto-combustion method. • Effect of ball-milling on particle size and cation distribution. • Magnetic property dependent on cations and particle size.

  19. Air-stable hydrogen generation materials and enhanced hydrolysis performance of MgH2-LiNH2 composites

    Science.gov (United States)

    Ma, Miaolian; Ouyang, Liuzhang; Liu, Jiangwen; Wang, Hui; Shao, Huaiyu; Zhu, Min

    2017-08-01

    Hydrolysis of materials in water can be a promising solution of onsite hydrogen generation for realization of hydrogen economy. In this work, it was the first time that the MgH2-LiNH2 composites were explored as air-stable hydrolysis system for hydrogen generation. The MgH2-LiNH2 composites with different composition ratios were synthesized by ball milling with various durations and the hydrogen generation performances of the composite samples were investigated and compared. X-ray diffraction, X-ray photoelectron spectroscopy and scanning electron microscopy techniques were adopted to elucidate the performance improvement mechanisms. The hydrolysis properties of MgH2 were found to be significantly enhanced by the introduction of LiNH2. The 4MgH2-LiNH2 composite ball milled for 5 h can generate 887.2 mL g-1 hydrogen in 1 min and 1016 mL g-1 in 50 min, one of the best results so far for Mg based hydrolysis materials. The LiOH·H2O and NH4OH phases of hydrolysis products from LiNH2 may prevent formation of Mg(OH)2 passivation layer on the surface and supply enough channels for hydrolysis of MgH2. The MgH2-LiNH2 composites appeared to be very stable in air and no obvious negative effect on kinetics and hydrogen generation yield was observed. These good performances demonstrate that the studied MgH2-LiNH2 composites can be a promising and practicable hydrogen generation system.

  20. Record critical current densities in IG processed bulk YBa{sub 2}Cu{sub 3}O{sub y} fabricated using ball-milled Y{sub 2}Ba{sub 1}Cu{sub 1}O{sub 5} phase

    Energy Technology Data Exchange (ETDEWEB)

    Muralidhar, Miryala; Kenta, Nakazato; Murakami, Masato [Department of Materials Science and Engineering, Superconducting Materials Laboratory, Shibaura Institute of Technology, Tokyo (Japan); Zeng, XianLin; Koblischka, Michael R. [Institute of Experimental Physics, Saarland University, Saarbruecken (Germany); Diko, Pavel [Institute of Experimental Physics, Material Physics Laboratory, Slovak Academy of Sciences, Kosice (Slovakia)

    2016-02-15

    The infiltration-growth (IG) technique enables the uniform and controllable Y{sub 2}BaCuO{sub 5} (Y211) secondary phase particles formation within the YBa{sub 2}Cu{sub 3}O{sub y} (Y123) matrix. Recent results clarified that the flux pinning performance of the Y123 material was dramatically improved by optimizing the processing conditions during the IG process. In this paper, we adapted the IG technique and produced several samples with addition of nanometer-sized Y211 secondary phase particles, which were produced by a ball milling technique. We found that the performance of the IG processed Y123 material dramatically improved in the low field region for a ball milling time of 12 h as compared to the samples without a ball milling step. Magnetization measurements showed a sharp superconducting transition with an onset T{sub c} at around 92 K. The critical current density (J{sub c}) at 77 K and zero field was determined to be 224 022 Acm{sup -2}, which is higher than the not ball-milled sample. Furthermore, microstructural observations exhibited a uniform microstructure with homogenous distribution of nanosized Y-211 inclusions within the Y-123 matrix. The improved performance of the Y-123 material can be understood in terms of fine distribution of the secondary phases. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  1. Low Thermal Conductivity of Bulk Amorphous Si1- x Ge x Containing Nano-Sized Crystalline Particles Synthesized by Ball-Milling Process

    Science.gov (United States)

    Muthusamy, Omprakash; Nishino, Shunsuke; Ghodke, Swapnil; Inukai, Manabu; Sobota, Robert; Adachi, Masahiro; Kiyama, Makato; Yamamoto, Yoshiyuki; Takeuchi, Tsunehiro; Santhanakrishnan, Harish; Ikeda, Hiroya; Hayakawa, Yasuhiro

    2018-06-01

    Amorphous Si0.65Ge0.35 powder containing a small amount of nano-sized crystalline particles was synthesized by means of the mechanical alloying process. Hot pressing for 24 h under the pressure of 400 MPa at 823 K, which is below the crystallization temperature, allowed us to obtain bulk amorphous Si-Ge alloy containing a small amount of nanocrystals. The thermal conductivity of the prepared bulk amorphous Si-Ge alloy was extremely low, showing a magnitude of less than 1.35 Wm-1 K-1 over the entire temperature range from 300 K to 700 K. The sound velocity of longitudinal and transverse waves for the bulk amorphous Si0.65Ge0.35 were measured, and the resulting values were 5841 m/s and 2840 m/s, respectively. The estimated mean free path of phonons was kept at the very small value of ˜ 4.2 nm, which was mainly due to the strong scattering limit of phonons in association with the amorphous structure.

  2. Modeling of Surface Geometric Structure State After Integratedformed Milling and Finish Burnishing

    Science.gov (United States)

    Berczyński, Stefan; Grochała, Daniel; Grządziel, Zenon

    2017-06-01

    The article deals with computer-based modeling of burnishing a surface previously milled with a spherical cutter. This method of milling leaves traces, mainly asperities caused by the cutting crossfeed and cutter diameter. The burnishing process - surface plastic treatment - is accompanied by phenomena that take place right in the burnishing ball-milled surface contact zone. The authors present the method for preparing a finite element model and the methodology of tests for the assessment of height parameters of a surface geometrical structure (SGS). In the physical model the workpieces had a cuboidal shape and these dimensions: (width × height × length) 2×1×4.5 mm. As in the process of burnishing a cuboidal workpiece is affected by plastic deformations, the nonlinearities of the milled item were taken into account. The physical model of the process assumed that the burnishing ball would be rolled perpendicularly to milling cutter linear traces. The model tests included the application of three different burnishing forces: 250 N, 500 N and 1000 N. The process modeling featured the contact and pressing of a ball into the workpiece surface till the desired force was attained, then the burnishing ball was rolled along the surface section of 2 mm, and the burnishing force was gradually reduced till the ball left the contact zone. While rolling, the burnishing ball turned by a 23° angle. The cumulative diagrams depict plastic deformations of the modeled surfaces after milling and burnishing with defined force values. The roughness of idealized milled surface was calculated for the physical model under consideration, i.e. in an elementary section between profile peaks spaced at intervals of crossfeed passes, where the milling feed fwm = 0.5 mm. Also, asperities after burnishing were calculated for the same section. The differences of the obtained values fall below 20% of mean values recorded during empirical experiments. The adopted simplification in after-milling

  3. Correlation of gas sensitivite properties with microstructure of Fe2O3-SnO2 ceramics prepared by high energy ball milling

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Lu, S.W.; Zhou, Y.X.

    1997-01-01

    A remarkable gas sensitivity to ethnaol gas has been observed in nanostructured Fe2O3-SnO2 materials with a composition of 6.4 mol% SnO2 prepared by high energy ball milling. The microstructure of the materials has been examined by x-ray diffraction (XRD) and Mossbauer spectroscopy. It was found...

  4. Influence of emulsifiers on the optimization of processing parameters of refining milk chocolate in the ball mill

    Directory of Open Access Journals (Sweden)

    Pajin Biljana

    2011-01-01

    Full Text Available Chocolate manufacture is a complex process which includes a large number of technology operations. One of the obligatory phases is milling, called refining, which aims at obtaining the appropriate distribution of particle size, resulting in the chocolate with optimal physical and sensory characteristics. The aim of this work was to define and optimize the process parameters for the production of milk chocolate by a non-conventional procedure, using the ball mill. The quality of chocolate mass, produced on this way, is determined by measuring the following parameters: moisture, size of the largest cocoa particle, yield flow, and Casson plastic viscosity. A special consideration of this study is the optimization of the types and amounts of emulsifiers, which are responsible for achieving the appropriate rheological and physical characteristics of the chocolate mass. The obtained parameters are compared with those which are typical for the standard procedure.

  5. The effect of TTNT nanotubes on hydrogen sorption using MgH2

    Directory of Open Access Journals (Sweden)

    Mariana Coutinho Brum

    2013-06-01

    Full Text Available Nanotubes are promising materials to be used with magnesium hydride, as catalysts, in order to enhance hydrogen sorption. A study was performed on the hydrogen absorption/desorption properties of MgH2 with the addition of TTNT (TiTanate NanoTubes. The MgH2-TTNT composite was prepared by ball milling and the influence of the TTNT amount (1.0 and 5.0 wt. (% on the hydrogen capacity was evaluated. The milling of pure MgH2 was performed for 24 hours and afterwards the MgH2-TTNT composite was milled for 20 minutes. Transmission Electronic Microscopy (TEM and Scanning Electron Microscopy (SEM were used to evaluate the nanotube synthesis and show the particle morphology of the MgH2-TTNT composite, respectively. The Differential Scanning Calorimetry (DSC examination provided some evidence with the shifting of the peaks obtained when the amount of TTNT is increased. The hydrogen absorption/desorption kinetics tests showed that the TTNT nanotubes can enhance hydrogen sorption effectively and the total hydrogen capacity obtained was 6.5 wt. (%.

  6. The effect of TTNT nanotubes on hydrogen sorption using MgH2

    International Nuclear Information System (INIS)

    Brum, Mariana Coutinho; Jardim, Paula Mendes; Conceicao, Monique Osorio Talarico da; Santos, Dilson Silva dos

    2013-01-01

    Nanotubes are promising materials to be used with magnesium hydride, as catalysts, in order to enhance hydrogen sorption. A study was performed on the hydrogen absorption/desorption properties of MgH 2 with the addition of TTNT (TiTanate nanotubes). The MgH 2 -TTNT composite was prepared by ball milling and the influence of the TTNT amount (1.0 and 5.0 wt. (%)) on the hydrogen capacity was evaluated. The milling of pure MgH 2 was performed for 24 hours and afterwards the MgH 2 -TTNT composite was milled for 20 minutes. Transmission Electronic Microscopy (TEM) and Scanning Electron Microscopy (SEM) were used to evaluate the nanotube synthesis and show the particle morphology of the MgH 2 -TTNT composite, respectively. The Differential Scanning Calorimetry (DSC) examination provided some evidence with the shifting of the peaks obtained when the amount of TTNT is increased. The hydrogen absorption/desorption kinetics tests showed that the TTNT nanotubes can enhance hydrogen sorption effectively and the total hydrogen capacity obtained was 6.5 wt. (%). (author)

  7. Optical and Acoustic Sensor-Based 3D Ball Motion Estimation for Ball Sport Simulators †

    Directory of Open Access Journals (Sweden)

    Sang-Woo Seo

    2018-04-01

    Full Text Available Estimation of the motion of ball-shaped objects is essential for the operation of ball sport simulators. In this paper, we propose an estimation system for 3D ball motion, including speed and angle of projection, by using acoustic vector and infrared (IR scanning sensors. Our system is comprised of three steps to estimate a ball motion: sound-based ball firing detection, sound source localization, and IR scanning for motion analysis. First, an impulsive sound classification based on the mel-frequency cepstrum and feed-forward neural network is introduced to detect the ball launch sound. An impulsive sound source localization using a 2D microelectromechanical system (MEMS microphones and delay-and-sum beamforming is presented to estimate the firing position. The time and position of a ball in 3D space is determined from a high-speed infrared scanning method. Our experimental results demonstrate that the estimation of ball motion based on sound allows a wider activity area than similar camera-based methods. Thus, it can be practically applied to various simulations in sports such as soccer and baseball.

  8. Phase evolution in Al-Ni-(Ti, Nb, Zr) powder blends by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Samanta, A. [Department of Metallurgy and Materials Engineering, Bengal Engineering and Science University, Shibpur (India); Manna, I. [Metallurgical and Materials Engineering Department, I.I.T., Kharagpur 721302 (India); Chattopadhyay, P.P. [Department of Metallurgy and Materials Engineering, Bengal Engineering and Science University, Shibpur (India)], E-mail: c.partha@mailcity.com

    2007-08-25

    Mechanical alloying of Al-rich Al-Ni-ETM (ETM = Ti, Nb, Zr) elemental powder blends by planetary ball milling yielded amorphous and/or nanocrystalline products after ball milling for suitable duration. Powder samples collected at different stages of ball milling have been examined by X-ray diffraction, differential scanning caloremetry and high-resolution transmission electron microscopy to examine the solid-state phase evolution. Powder blends having nominal composition of Al{sub 80}Ni{sub 10}Ti{sub 10} and Al{sub 80}Ni{sub 10}Nb{sub 10} yielded predominantly amorphous products, while the other alloys formed composite microstructures comprising nanaocrystalline and amorphous solid solutions. The amorphous Al{sub 80}Ni{sub 10}Ti{sub 10} alloy was mixed with different amounts of Al powder, and subjected to warm rolling after consolidation within the Al-cans with or without intermediate annealing for 10 min at 500 K to obtain sheet of 2.5 mm thickness. Notable improvement in mechanical properties has been achieved for the composite sheets in comparison to the pure Al.

  9. Study of the behavior of the compound Mg2Ni0.5Co0.5 front to hydriding process

    International Nuclear Information System (INIS)

    Martinez, C; Ordonez, S; Serafini, D; Guzman, D; Bustos, O

    2012-01-01

    This paper study the behavior of the compound Mg 2 Ni 0,5 Co 0,5 during the hydriding process. Elemental powders of Mg, Ni and Co, with an atomic ratio of 2:0,5:0,5 were mechanically alloyed using a high energy mill SPEX 8000D for 36h. The amorphous and crystalline structure of the samples was characterized through X-ray diffraction The hydriding process was performed by the volumetric technique Sievert at 90 o C and a pressure of 20 bar H 2 . The desorption process was evaluated by differential scanning calorimetry. Based on the results we can conclude that the amorphous structure absorbs more hydrogen, reaching a maximum of 3.6 wt% H2, besides the incorporation of cobalt act as catalyst for the absorption of H2 obtaining values higher than those reported in the Mg-Ni system amorphous state. The desorption process is influenced by the type of structure that presents the alloy

  10. The effect of TTNT nanotubes on hydrogen sorption using MgH{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Brum, Mariana Coutinho; Jardim, Paula Mendes; Conceicao, Monique Osorio Talarico da; Santos, Dilson Silva dos, E-mail: monique@metalmat.ufrj.br [Coordenacao dos Programas de Pos-Graduacao em Engenharia (PEMM/COPPEP/UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Engenharia Metalurgica e de Materiais

    2013-11-01

    Nanotubes are promising materials to be used with magnesium hydride, as catalysts, in order to enhance hydrogen sorption. A study was performed on the hydrogen absorption/desorption properties of MgH{sub 2} with the addition of TTNT (TiTanate nanotubes). The MgH{sub 2} -TTNT composite was prepared by ball milling and the influence of the TTNT amount (1.0 and 5.0 wt. (%)) on the hydrogen capacity was evaluated. The milling of pure MgH{sub 2} was performed for 24 hours and afterwards the MgH{sub 2} -TTNT composite was milled for 20 minutes. Transmission Electronic Microscopy (TEM) and Scanning Electron Microscopy (SEM) were used to evaluate the nanotube synthesis and show the particle morphology of the MgH{sub 2} -TTNT composite, respectively. The Differential Scanning Calorimetry (DSC) examination provided some evidence with the shifting of the peaks obtained when the amount of TTNT is increased. The hydrogen absorption/desorption kinetics tests showed that the TTNT nanotubes can enhance hydrogen sorption effectively and the total hydrogen capacity obtained was 6.5 wt. (%). (author)

  11. Mechanically Strain-Induced Modification of Selenium Powders in the Amorphization Process

    International Nuclear Information System (INIS)

    Fuse, Makoto; Shirakawa, Yoshiyuki; Shimosaka, Atsuko; Hidaka, Jusuke

    2003-01-01

    For the fabrication of particles designed in the nanoscale structure, or the nanostructural modification of particles using mechanical grinding process, selenium powders ground by a planetary ball mill at various rotational speeds have been investigated. Structural analyses, such as particle size distributions, crystallite sizes, lattice strains and nearest neighbour distances were performed using X-ray diffraction, scanning electron microscopy and dynamical light scattering.By grinding powder particles became spherical composites consisting of nanocrystalline and amorphous phase, and had a distribution with the average size of 2.7 μm. Integral intensities of diffraction peaks of annealed crystal selenium decreased with increasing grinding time, and these peaks broadened due to lattice strains and reducing crystallite size during the grinding. The ground powder at 200 rpm did not have the lattice strain and showed amorphization for the present grinding periods. It indicates that the amorphization of Se by grinding accompanies the lattice strain, and the lattice strain arises from a larger energy concerning intermolecular interaction. In this process, the impact energy is spent on thermal and structural changes according to energy accumulation in macroscopic (the particle size distribution) and microscopic (the crystallite size and the lattice strain) range

  12. Effect of milling time on the structure, micro-hardness, and thermal behavior of amorphous/nanocrystalline TiNiCu shape memory alloys developed by mechanical alloying

    International Nuclear Information System (INIS)

    Alijani, Fatemeh; Amini, Rasool; Ghaffari, Mohammad; Alizadeh, Morteza; Okyay, Ali Kemal

    2014-01-01

    Highlights: • Potential to produce B1′ (thermal- and stress-induced) and B2 was established. • Martensitic transformation occurred without the formation of intermediate R-phase. • Formation of unwanted intermetallics during heating was hindered by milling. • During milling, microhardness was increased, then reduced, and afterward re-increased. • By milling evolution, thermal crystallization steps changed from 3 to 2. - Abstract: In the present paper, the effect of milling process on the chemical composition, structure, microhardness, and thermal behavior of Ti–41Ni–9Cu compounds developed by mechanical alloying was evaluated. The structural characteristic of the alloyed powders was evaluated by X-ray diffraction (XRD). The chemical composition homogeneity and the powder morphology and size were studied by scanning electron microscopy coupled with electron dispersive X-ray spectroscopy. Moreover, the Vickers micro-indentation hardness of the powders milled for different milling times was determined. Finally, the thermal behavior of the as-milled powders was studied by differential scanning calorimetery. According to the results, at the initial stages of milling (typically 0–12 h), the structure consisted of a Ni solid solution and amorphous phase, and by the milling evolution, nanocrystalline martensite (B19′) and austenite (B2) phases were initially formed from the initial materials and then from the amorphous phase. It was found that by the milling development, the composition uniformity is increased, the inter-layer thickness is reduced, and the powders microhardness is initially increased, then reduced, and afterward re-increased. It was also realized that the thermal behavior of the alloyed powders and the structure of heat treated samples is considerably affected by the milling time

  13. Recycling process for recovery of gallium from GaN an e-waste of LED industry through ball milling, annealing and leaching

    Energy Technology Data Exchange (ETDEWEB)

    Swain, Basudev, E-mail: swain@iae.re.kr; Mishra, Chinmayee; Kang, Leeseung; Park, Kyung-Soo, E-mail: kspark@iae.re.kr; Lee, Chan Gi; Hong, Hyun Seon, E-mail: hshong@iae.re.kr

    2015-04-15

    Waste dust generated during manufacturing of LED contains significant amounts of gallium and indium, needs suitable treatment and can be an important resource for recovery. The LED industry waste dust contains primarily gallium as GaN. Leaching followed by purification technology is the green and clean technology. To develop treatment and recycling technology of these GaN bearing e-waste, leaching is the primary stage. In our current investigation possible process for treatment and quantitative leaching of gallium and indium from the GaN bearing e-waste or waste of LED industry dust has been developed. To recycle the waste and quantitative leaching of gallium, two different process flow sheets have been proposed. In one, process first the GaN of the waste the LED industry dust was leached at the optimum condition. Subsequently, the leach residue was mixed with Na{sub 2}CO{sub 3}, ball milled followed by annealing, again leached to recover gallium. In the second process, the waste LED industry dust was mixed with Na{sub 2}CO{sub 3}, after ball milling and annealing, followed acidic leaching. Without pretreatment, the gallium leaching was only 4.91 w/w % using 4 M HCl, 100 °C and pulp density of 20 g/L. After mechano-chemical processing, both these processes achieved 73.68 w/w % of gallium leaching at their optimum condition. The developed process can treat and recycle any e-waste containing GaN through ball milling, annealing and leaching. - Highlights: • Simplest process for treatment of GaN an LED industry waste developed. • The process developed recovers gallium from waste LED waste dust. • Thermal analysis and phase properties of GaN to Ga{sub 2}O{sub 3} and GaN to NaGaO{sub 2} revealed. • Solid-state chemistry involved in this process reported. • Quantitative leaching of the GaN was achieved.

  14. Phase transformation and magnetic properties of MnAl powders prepared by elemental-doping and salt-assisted ball milling

    Science.gov (United States)

    Qian, Hui-Dong; Si, Ping-Zhan; Choi, Chul-Jin; Park, Jihoon; Cho, Kyung Mox

    2018-05-01

    The effects of elemental doping of Si and Fe on the ɛ→τ phase transformation and the magnetic properties of MnAl were studied. The magnetic powders of Si- and Fe-doped MnAl were prepared by using induction melting followed by water-quenching, annealing, and salt-assisted ball-milling. The Fe-doped MnAl powders are mainly composed of the L10-structured τ-phase, while the Si-doped MnAl are composed of τ-phase and a small fraction of γ2- and β-phases. A unique thin leaves-like morphology with thickness of several tens of nanometers and diameter size up to 500 nm were observed in the Si-doped MnAl powders. The Fe-doped MnAl powders show irregular shape with much larger dimensions in the range from several to 10 μm. The morphology difference of the samples was ascribed to the variation of the mechanical properties affected by different doping elements. The phase transformation temperatures of the ɛ-phase of the samples were measured. The doping of Fe decreases the onset temperature of the massive phase transformation in MnAl, while the Si-doping increases the massive phase transformation temperature. Both Fe and Si increase the Curie temperature of MnAl. A substantially enhanced coercivity up to 0.45 T and 0.42 T were observed in the ball-milled MnAl powders doped with Si and Fe, respectively.

  15. Preparation of Zn(BH4)2 and diborane and hydrogen release properties of Zn(BH4)2+xMgH2 (x=1, 5, 10, and 15)

    Science.gov (United States)

    Kwak, Young Jun; Kwon, Sung Nam; Song, Myoung Youp

    2015-09-01

    Zn(BH4)2 was prepared by milling ZnCl2 and NaBH4 in a planetary ball mill under Ar atmosphere, and Zn(BH4)2+xMgH2 (x=1, 5, 10, and 15) samples were prepared. Diborane (B2H6) and hydrogen release characteristics of the Zn(BH4)2 and Zn(BH4)2+xMgH2 samples were studied. The samples synthesized by milling ZnCl2 and NaBH4 contained Zn(BH4)2 and NaCl, together with small amounts of ZnCl2 and NaBH4. We designated these samples as Zn(BH4)2(+NaCl). The weight loss up to 400 °C of the Zn(BH4)2(+NaCl) sample synthesized by milling 4 h was 11.2 wt%. FT-IR analysis showed that Zn(BH4)2 was formed in the Zn(BH4)2(+NaCl) samples. MgH2 was also milled in a planetary ball mill, and mixed with the Zn(BH4)2(+NaCl) synthesized by milling for 4 h in a mortar and pestle. The weight loss up to 400 °C of Zn(BH4)2(+NaCl)+MgH2 was 8.2 wt%, corresponding to the weight % of diborane and hydrogen released from the Zn(BH4)2(+NaCl)+MgH2 sample, with respect to the sample weight. DTA results of Zn(BH4)2(+NaCl)+xMgH2 showed that the decomposition peak of Zn(BH4)2 was at about 61 °C, and that of MgH2 was at about 370-389 °C.

  16. The Structure and Mechanical Properties of High-Strength Bulk Ultrafine-Grained Cobalt Prepared Using High-Energy Ball Milling in Combination with Spark Plasma Sintering

    Czech Academy of Sciences Publication Activity Database

    Marek, I.; Vojtěch, D.; Michalcová, A.; Kubatík, Tomáš František

    2016-01-01

    Roč. 9, č. 5 (2016), č. článku 391. ISSN 1996-1944 Institutional support: RVO:61389021 Keywords : ultrafine-grained material * cobalt * ball milling * spark plasma sintering * mechanical properties Subject RIV: JG - Metallurgy Impact factor: 2.654, year: 2016 www.mdpi.com/1996-1944/9/5/391/pdf

  17. Barium Ferrite Ball Milled in Vacuum

    International Nuclear Information System (INIS)

    Campbell, S.J.; Wu, E.; Kaczmarek, W.A.; Wang, G.

    1998-01-01

    The structural and magnetic behaviour of BaFe 12 O 19 subjected to milling in vacuum for 1000 h has been investigated by x-ray powder diffraction and Moessbauer effect spectroscopy techniques. Pronounced structural disorder is obtained along with partial decomposition of BaFe 12 O 19 to α-Fe 2 O 3 and evidence for superparamagnetic relaxation effects due to the fine particles produced on milling. Restoration of the fully crystallised BaFe 12 O 19 structure on annealing at 1000 deg. C is accompanied by a six fold enhancement in the magnetic coercivity. This behaviour is linked with the fine crystallites

  18. Kinetics of hydrogen adsorption on MgH{sub 2}/CNT composite

    Energy Technology Data Exchange (ETDEWEB)

    Rather, Sami ullah, E-mail: rathersami@gmail.com; Taimoor, Aqeel Ahmad; Muhammad, Ayyaz; Alhamed, Yahia Abobakor; Zaman, Sharif Fakhruz; Ali, Arshid Mahmood

    2016-05-15

    Highlights: • Hydrogen adsorption comparisons of commercial, milled, and MgH{sub 2} composite. • Hydrogen adsorption capacity and kinetics improves tremendously by CNT embedding. • Unsteady state modeling and simulation of adsorption kinetics. - Abstract: Magnesium hydride (MgH{sub 2})–carbon nanotubes (CNT) composite has been prepared by high-energy ball milling method and their experimental and kinetic hydrogen adsorption studies was assessed. Hydrogen adsorption studies were performed by Sievert’s volumetric apparatus and kinetic evaluation was conducted by surface chemistry and Langmuir–Hinshelwood–Hougen–Watson (LHHW) type mode. Powder X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) were performed. Hydrogen adsorption capacity of commercial MgH{sub 2}, milled MgH{sub 2}, and MgH{sub 2}/CNT composite are found to be 0.04, 0.057, and 0.059 g (H{sub 2})/g (MgH{sub 2}) at 673 K and hydrogen pressure of 4.6 MPa. Addition of 5 wt% of CNTs to MgH{sub 2} proved to be very critical to enhance hydrogen adsorption as well as to improve its kinetics. It was observed that hydrogen adsorption is not in quasi-state equilibrium and is modeled using kinetic rate laws.

  19. Microstructure and kinetics evolution in MgH{sub 2}–TiO{sub 2} pellets after hydrogen cycling

    Energy Technology Data Exchange (ETDEWEB)

    Mirabile Gattia, D., E-mail: daniele.mirabile@enea.it; Di Girolamo, G.; Montone, A.

    2014-12-05

    Highlights: • MgH{sub 2} was ball milled with TiO{sub 2} anatase phase and expanded graphite to prepare pellets. • Different pellets have been prepared at different compression load. • Pellets were repeatedly cycled under hydrogen pressure to simulate tank exercise and verify their stability. • The compression load highly affects the stability of the pellets to cycling. • Microstructural evolution of the particles due to cycling have been observed. - Abstract: The interest in Mg-based hydrides for solid state hydrogen storage is associated to their capability to reversibly absorb and desorb large amounts of hydrogen. In this work MgH{sub 2} powder with 5 wt.% TiO{sub 2} was ball milled for 10 h. The as-milled nanostructured powder was enriched with 5 wt.% of Expanded Natural Graphite (ENG) and then compacted in cylindrical pellets by cold pressing using different loads. Both the powder and the pellets were subjected to kinetic and thermodynamic tests using a Sievert’s type gas reaction controller, in order to study the microstructural and kinetic changes which took place during repeated H{sub 2} absorption and desorption cycles. The pellets exhibited good kinetic performance and durability, even if the pressure of compaction revealed to be an important parameter for their mechanical stability. Scanning Electron Microscopy observations of as-prepared and cycled pellets were carried out to investigate the evolution of their microstructure. In turn the phase composition before and after cycling was analyzed by X-ray diffraction.

  20. Morphology and magnetic properties of CeCo5 submicron flakes prepared by surfactant-assisted high-energy ball milling

    Science.gov (United States)

    Zhang, J. J.; Gao, H. M.; Yan, Y.; Bai, X.; Su, F.; Wang, W. Q.; Du, X. B.

    2012-10-01

    CeCo5 permanent magnetic alloy has been processed by surfactant assisted high energy ball milling. Heptane and oleic acid were used as the solvent and surfactant, respectively. The amount of surfactant used was 50% by weight of the starting powder. The produced particles were deposited on a piece of copper (4 mm in length and width) under a magnetic field of 27 kOe applied along the copper surface and immobilized by ethyl α-cyanoacrylate. Scanning electron microscope pictures show that the particles are flakes, several μm in length and width and tens of nm in thickness. X-ray diffraction patterns and magnetic measurements prove that the flakes are crystalline with c-axes magnetic anisotropy. The easy magnetization axis is oriented perpendicular to the surface of the flake. A maximum coercivity of 3.3 kOe was obtained for the sample milled for 40 min.

  1. Lignocellulose fermentation and residual solids characterization for senescent switchgrass fermentation by Clostridium thermocellum in the presence and absence of continuous in situ ball-milling

    Energy Technology Data Exchange (ETDEWEB)

    Balch, Michael L.; Holwerda, Evert K.; Davis, Mark F.; Sykes, Robert W.; Happs, Renee M.; Kumar, Rajeev; Wyman, Charles E.; Lynd, Lee R.

    2017-04-12

    Milling during lignocellulosic fermentation, henceforth referred to as cotreatment, is investigated as an alternative to thermochemical pretreatment as a means of enhancing biological solubilization of lignocellulose. We investigate the impact of milling on soluble substrate fermentation by Clostridium thermocellum with comparison to yeast, document solubilization for fermentation of senescent switchgrass with and without ball milling, and characterize residual solids. Soluble substrate fermentation by C. thermocellum proceeded readily in the presence of continuous ball milling but was completely arrested for yeast. Total fractional carbohydrate solubilization achieved after fermentation of senescent switchgrass by C. thermocellum for 5 days was 0.45 without cotreatment or pretreatment, 0.81 with hydrothermal pretreatment (200 degrees C, 15 minutes, severity 4.2), and 0.88 with cotreatment. Acetate and ethanol were the main fermentation products, and were produced at similar ratios with and without cotreatment. Analysis of solid residues was undertaken using molecular beam mass spectrometry (PyMBMS) and solid-state nuclear magnetic resonance spectroscopy (NMR) in order to provide insight into changes in plant cell walls during processing via various modes. The structure of lignin present in residual solids remaining after fermentation with cotreatment appeared to change little, with substantially greater changes observed for hydrothermal pretreatment - particularly with respect to formation of C-C bonds. The observation of high solubilization with little apparent modification of the residue is consistent with cotreatment enhancing solubilization primarily by increasing the access of saccharolytic enzymes to the feedstock, and C. thermocellum being able to attack all the major linkages in cellulosic biomass provided that these linkages are accessible.

  2. Mg amorphous alloys for biodegradable implants; Ligas amorfas de magnesio utilizadas em implantes consumiveis

    Energy Technology Data Exchange (ETDEWEB)

    Danez, G.P., E-mail: gabidanez@hotmail.co [Universidade Federal de Sao Carlos (PPG-CEMUFSCar), SP (Brazil). Programa de Pos-Graduacao em Ciencia e Engenharia de Materiais; Koga, G.Y.; Tonucci, S.; Bolfarini, C.; Kiminami, C.S.; Botta Filho, W.J. [Universidade Federal de Sao Carlos (DEMa/UFSCar), SP (Brazil). Dept. de Engenharia de Materiais

    2010-07-01

    The use of implants made from amorphous alloys magnesium-based with additions of zinc and calcium are promising. Properties such as biocompatibility, low density, high mechanical strength, low modulus (as compared to alloys such as stainless steel and titanium), corrosion resistance and wear resistance make it attractive for use in implants. Moreover, the by-products of corrosion and wear are not toxic and may contribute to fixation. Aiming to understand the tendency of this amorphous ternary (Mg-Zn-Ca) and expand the information about this system, this work involved the use of the topological criterion of instability ({lambda}) and the criterion of electronegativity ({Delta}e) to the choice of compositions. The alloys were processed into wedge-shaped and analyzed structurally and in X-ray diffraction and scanning electron microscopy. (author)

  3. Potential sustainable slow release fertilizers obtained by mechanochemical activation of layered double hydroxides and K{sub 2}HPO{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Roger; Wypych, Fernando, E-mail: 1roger.borges@gmail.com [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil); Prevot, Vanessa; Forano, Claude [Universite Blaise Pascal, Clermont-Ferrand (France)

    2016-07-01

    Full text: This study describes the preliminary results on the development of potential sustainable slow-release fertilizer (SSRF), obtained by mechanochemical activation of mixtures of calcined layered double hydroxides (LDH) Mg{sub 2}Al-CO{sub 3} and Mg{sub 2}Fe-CO{sub 3} and K{sub 2}HPO{sub 4}. The effect of LDH temperature of calcination, milling time (using a high-energy balls mill) and LDH:K{sub 2}HPO{sub 4} molar were investigated. The samples were characterized by XRD and FTIR. Phosphate release essays shown that its solubility is reduced, while the solubility of amorphous structures from LDH can be increased, which characterize the expected slow release behavior of a SSRF. (author)

  4. Formation of ultra-fine grained TiC-dispersed SUS316L by ball-milling and their consolidation by hot isostatic pressing

    International Nuclear Information System (INIS)

    Zheng, Yongjia; Yamasaki, Tohru; Fukami, Takeshi; Mitamura, Tohru; Terasawa, Mititaka

    2003-01-01

    In order to overcome the irradiation embrittlement in austenitic stainless steels, ultra-fine grained SUS316L steels with very fine TiC particles have been developed. The SUS316-TiC nanocomposite powders having 1.0 to 2.0 mass%TiC were prepared by ball-milling SUS316-TiC powder mixtures for 125h in an argon gas atmosphere. The milled powders were consolidated by hot isostatic pressing (HIP) under a pressure of 200 MPa at temperature between 700-1000degC, and the bulk materials with crystallite size ranging between 100-400 nm have been produced. The possibility of using fine-grained TiC particles for pinning grain boundaries and thereby to maintain the ultra-fine grained structures has been discussed. (author)

  5. Hot Melt Extrusion and Spray Drying of Co-amorphous Indomethacin-Arginine With Polymers.

    Science.gov (United States)

    Lenz, Elisabeth; Löbmann, Korbinian; Rades, Thomas; Knop, Klaus; Kleinebudde, Peter

    2017-01-01

    Co-amorphous drug-amino acid systems have gained growing interest as an alternative to common amorphous formulations which contain polymers as stabilizers. Several preparation methods have recently been investigated, including vibrational ball milling on a laboratory scale or spray drying in a larger scale. In this study, the feasibility of hot melt extrusion for continuous manufacturing of co-amorphous drug-amino acid formulations was examined, challenging the fact that amino acids melt with degradation at high temperatures. Furthermore, the need for an addition of a polymer in this process was evaluated. After a polymer screening via the solvent evaporation method, co-amorphous indomethacin-arginine was prepared by a melting-solvent extrusion process without and with copovidone. The obtained products were characterized with respect to their solid-state properties, non-sink dissolution behavior, and stability. Results were compared to those of spray-dried formulations with the same compositions and to spray-dried indomethacin-copovidone. Overall, stable co-amorphous systems could be prepared by extrusion without or with copovidone, which exhibited comparable molecular interaction properties to the respective spray-dried products, while phase separation was detected by differential scanning calorimetry in several cases. The formulations containing indomethacin in combination with arginine and copovidone showed enhanced dissolution behavior over the formulations with only copovidone or arginine. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  6. Characterization of the hidden glass transition of amorphous cyclomaltoheptaose.

    Science.gov (United States)

    Tabary, Nicolas; Mahieu, Aurélien; Willart, Jean-François; Dudognon, Emeline; Danède, Florence; Descamps, Marc; Bacquet, Maryse; Martel, Bernard

    2011-10-18

    An amorphous solid of cyclomaltoheptaose (β-cyclodextrin, β-CD) was formed by milling its crystalline form using a high-energy planetary mill at room temperature. The glass transition of this amorphous solid was found to occur above the thermal degradation point of the material preventing its direct observation and thus its full characterization. The corresponding glass transition temperature (T(g)) and the ΔC(p) at T(g) have, however, been estimated by extrapolation of T(g) and ΔC(p) of closely related amorphous compounds. These compounds include methylated β-CD with different degrees of substitution and molecular alloys obtained by co-milling β-CD and methylated β-CD (DS 1.8) at different ratios. The physical characterization of the amorphous states have been performed by powder X-ray diffraction and differential scanning calorimetry, while the chemical integrity of β-CD upon milling was checked by NMR spectroscopy and mass spectrometry. Copyright © 2011 Elsevier Ltd. All rights reserved.

  7. Focused ion beam milling of carbon fibres

    International Nuclear Information System (INIS)

    Huson, Mickey G.; Church, Jeffrey S.; Hillbrick, Linda K.; Woodhead, Andrea L.; Sridhar, Manoj; Van De Meene, Allison M.L.

    2015-01-01

    A focused ion beam has been used to mill both individual carbon fibres as well as fibres in an epoxy composite, with a view to preparing flat surfaces for nano-indentation. The milled surfaces have been assessed for damage using scanning probe microscopy nano-indentation and Raman micro-probe analysis, revealing that FIB milling damages the carbon fibre surface and covers surrounding areas with debris of disordered carbon. The debris is detected as far as 100 μm from the milling site. The energy of milling as well as the orientation of the beam was varied and shown to have an effect when assessed by Raman spectroscopy. - Highlights: • Focused ion beam (FIB) milling was used to mill flat surfaces on carbon fibres. • Raman spectroscopy showed amorphous carbon was generated during FIB milling. • The amorphous debris is detected as far as 100 μm from the milling site. • This surface degradation was confirmed by nano-indentation experiments.

  8. Electrochemical performance of Si-CeMg{sub 12} composites as anode materials for Li-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Z.W. [Institute of New Energy Material Chemistry, Nankai University, Tianjin 300071 (China); Tianjin Institute of Power Sources, Tianjin 300381 (China); Wang, G.; Gao, X.P. [Institute of New Energy Material Chemistry, Nankai University, Tianjin 300071 (China); Liu, X.J.; Wang, J.Q. [Tianjin Institute of Power Sources, Tianjin 300381 (China)

    2009-04-01

    The Si-CeMg{sub 12} composites with 30 wt.%, 40 wt.% and 50 wt.% Si, were synthesized by directly ball milling Si and CeMg{sub 12} alloy. The microstructure of the Si-CeMg{sub 12} composites is confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. It is demonstrated from TEM images that active Si nanoparticles are distributed in the inactive CeMg{sub 12} matrix. The electrochemical performance of the Si-CeMg{sub 12} composites as a function of Si content is investigated. The maximum reversible (charge) capacities of the ball-milled Si-CeMg{sub 12} composites with 30 wt.%, 40 wt.% and 50 wt.% Si reach 470, 690 and 1080 mAh g{sup -1}, respectively, after full activations. It is found that the Si-CeMg{sub 12} composite with 40 wt.% Si delivers a larger reversible capacity and better cycle ability because the uniform distribution of active Si nanoparticles embedded in the CeMg{sub 12} matrix, which can accommodate the volume expansion of the composite during Li-alloying/dealloying processes. After subsequent cycles, the recrystallization of Si with lattice shrinkage is observed, which is unfavorable to the Li-alloying/dealloying reaction. The degeneration of CeMg{sub 12}-Si composites during repeated cycling is attributed not only to the Si pulverization led by the volume change, but partially also to the irreversible phase transformation of Si. (author)

  9. Effective utilizations of palm oil mill fly ash for synthetic amorphous silica and carbon zeolite composite synthesis

    Science.gov (United States)

    Utama, P. S.; Saputra, E.; Khairat

    2018-04-01

    Palm Oil Mill Fly Ash (POMFA) the solid waste of palm oil industry was used as a raw material for synthetic amorphous silica and carbon zeolite composite synthesis in order to minimize the wastes of palm oil industry. The alkaline extraction combine with the sol-gel precipitation and mechanical fragmentation was applied to produce synthetic amorphous silica. The byproduct, extracted POMFA was rich in carbon and silica content in a significant amount. The microwave heated hydrothermal process used to synthesize carbon zeolite composite from the byproduct. The obtained silica had chemical composition, specific surface area and the micrograph similar to commercial precipitated silica for rubber filler. The microwave heated hydrothermal process has a great potential for synthesizing carbon zeolite composite. The process only needs one-step and shorter time compare to conventional hydrothermal process.

  10. Optimization of chemical composition in the manufacturing process of flotation balls based on intelligent soft sensing

    Directory of Open Access Journals (Sweden)

    Dučić Nedeljko

    2016-01-01

    Full Text Available This paper presents an application of computational intelligence in modeling and optimization of parameters of two related production processes - ore flotation and production of balls for ore flotation. It is proposed that desired chemical composition of flotation balls (Mn=0.69%; Cr=2.247%; C=3.79%; Si=0.5%, which ensures minimum wear rate (0.47 g/kg during copper milling is determined by combining artificial neural network (ANN and genetic algorithm (GA. Based on the results provided by neuro-genetic combination, a second neural network was derived as an ‘intelligent soft sensor’ in the process of white cast iron production. The proposed ANN 12-16-12-4 model demonstrated favourable prediction capacity, and can be recommended as a ‘intelligent soft sensor’ in the alloying process intended for obtaining favourable chemical composition of white cast iron for production of flotation balls. In the development of intelligent soft sensor data from the two real production processes was used. [Projekat Ministarstva nauke Republike Srbije, br. TR35037 i br. TR35015

  11. EFFECT OF CUP AND BALL TYPES ON MECHANO-CHEMICAL SYNTHES IS OF Al2O3–TiC NANOCOMPOSITE POWDER

    Directory of Open Access Journals (Sweden)

    M. Zakeri

    2012-07-01

    Full Text Available Al2O3–TiC nanocomposite powder was successfully synthesized by ball milling TiO2, Al and graphite powders. Effects of cup and ball type, milling time and annealing were investigated. XRD was used to characterize milled and annealed powders. The morphological and microstructural evolutions were studied by SEM and TEM. Results showed that the formation of this composite begins after 20 h and completes after 35 h of milling with stainless steel cup and balls. In contrast, there is no reaction during milling (up to 80 h with ZrO2 cup and balls. Fe and ZrO2 were the major impurities introduced during milling with stainless steel and ZrO2 cups, respectively. The Fe impurity was removed by leaching in 3HCl·HNO3 solution for 4 days. Mean grain size less than 7 nm was achieved at the end of milling. In spite of grain growth, this composite maintained its nanocrystalline nature after annealing at 1000°C.

  12. Pseudocapacitance of amorphous TiO2@nitrogen doped graphene composite for high rate lithium storage

    International Nuclear Information System (INIS)

    Li, Sheng; Xue, Pan; Lai, Chao; Qiu, Jingxia; Ling, Min; Zhang, Shanqing

    2015-01-01

    The high rate applications such as electric vehicles of the traditional lithium ion batteries (LIBs) are commonly limited by their insufficient electron conductivity and slow mass transport of lithium ions in bulk electrode materials. In order to address these issues, in this work, a simple and up-scalable wet-mechanochemical (wet-ball milling) route has been developed for fabrication of amorphous porous TiO 2 @nitrogen doped graphene (TiO 2 @N-G) nanocomposites. The amorphous phase, unique porous structure of TiO 2 and the surface defects from nitrogen doping to graphene planes have incurred surface controlled reactions, contributing pseudocapacitance to the total capacity of the battery. It plays a dominant role in producing outstanding high rate electrochemical performance, e.g., 182.7 mAh/g (at 3.36 A/g) after 100 cycles. The design and synthesis of electrode materials with enhanced conductivity and surface pseudocapacitance can be a promising way for high rate LIBs.

  13. Investigation of different carbon nanotube reinforcements for fabricating bulk AlMg5 matrix nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Kallip, Kaspar, E-mail: kaspar.kallip@empa.ch [Empa, Swiss Federal Laboratories for Material Science and Technology, Laboratory for Advanced Materials Processing, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); Leparoux, Marc [Empa, Swiss Federal Laboratories for Material Science and Technology, Laboratory for Advanced Materials Processing, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); AlOgab, Khaled A. [King Abdulaziz City for Science and Technology (KACST), National Centers for Advanced Materials, P O Box 6086, Riyadh, 11442 (Saudi Arabia); Clerc, Steve; Deguilhem, Guillaume [Empa, Swiss Federal Laboratories for Material Science and Technology, Laboratory for Advanced Materials Processing, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); Arroyo, Yadira [Empa, Swiss Federal Laboratories for Material Science and Technology, Electron Microscopy Center, Ueberlandstrasse 129, CH-8600 Dübendorf (Switzerland); Kwon, Hansang [Empa, Swiss Federal Laboratories for Material Science and Technology, Laboratory for Advanced Materials Processing, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); Pukyong National University, Department of Materials System Engineering, 365 Sinseon-ro, Busan 608-739 (Korea, Republic of)

    2015-10-15

    AlMg5-based metal matrix composites were successfully fabricated using high energy planetary ball-milling and hot pressing. The influence of 6 types of carbon nanotubes (CNTs) with different properties was investigated for reinforcement. Over 3 fold increase in hardness and ultimate tensile strength was achieved with maximum values of 200 HV{sub 20} and 720 MPa respectively by varying CNT content from 0.5 to 5 vol%. The state, the dispersion as well as the reactivity of the different CNTs were investigated by Raman spectroscopy, X-Ray diffraction and microscopy. The CNTs were considered to be dispersed homogeneously, but were shortened due to high energy milling. No significant differences in mechanical performances could be observed depending either on the nature or on the agglomeration initial state of the investigated CNTs. The milling time has to be however adjusted to the CNT content as higher concentrations require a longer milling time for achieving dispersion of the nano-reinforcement. - Highlights: • CNTs sustained the milling process and became homogeneously dispersed. • 3 times strengthening over unreinforced alloy achieved. • Flexible processing route for dispersing wide range of nanoparticulate materials.

  14. Tratamiento mecanoquímico de la ferrita MgFe2O4

    Directory of Open Access Journals (Sweden)

    Torralba, J. M.

    2000-06-01

    Full Text Available Powder of MgFe2O4, previously prepared by solid state reaction, was mechanochemically treated in a centrifugal ball mill in air atmosphere. Different milling conditions has been employed varying ball/powder mass ratio. After low milling time a strong reduction on crystallite size has been detected while the strain lattice increase slowly. The presence of α-Fe2O3 was also observed at different milling time, depending on milling conditions, by means of X-Ray diffraction experiments. Magnetic transition temperatures were evaluated using a thermogravimetric analyser, equipped with a small permanent magnet. An attempt of dependence of magnetic properties with crystallite size has been established.La ferrita MgFe2O4, en forma de polvo y previamente preparada por reacción en estado sólido, se ha sometido a un proceso de molienda mecánica en atmósfera de aire usando un molino centrífugo. Se emplearon diferentes condiciones de molienda variando la relación de peso bolas/ferrita. La variación del tamaño de dominio cristalino o de cristalita y lamicrodeformaciones de red a escala de celda unidad se evaluaron mediante difracción de rayos-X de polvo. Para bajos tiempos de molienda se observó una acusada disminución del tamaño de dominio cristalino, mientras que las microdeformaciones de la red experimentaron un ligero aumento. Así mismo, a partir de determinados tiempos de molienda, se detectó la presencia de α-Fe2O3. Las temperaturas de transición magnética fueron evaluadas a partir de un analizador termogravimétrico equipado con un pequeño imán permanente y se estableció un correlación entre la temperatura de Curie y el tamaño de dominio cristalino.

  15. Analytical Prediction of Three Dimensional Chatter Stability in Milling

    Science.gov (United States)

    Altintas, Yusuf

    The chip regeneration mechanism during chatter is influenced by vibrations in three directions when milling cutters with ball end, bull nose, or inclined cutting edges are used. A three dimensional chatter stability is modeled analytically in this article. The dynamic milling system is formulated as a function of cutter geometry, the frequency response of the machine tool structure at the cutting zone in three Cartesian directions, cutter engagement conditions and material property. The dynamic milling system with nonlinearities and periodic delayed differential equations is reduced to a three dimensional linear stability problem by approximations based on the physics of milling. The chatter stability lobes are predicted in the frequency domain using the proposed analytical solution, and verified experimentally in milling a Titanium alloy with a face milling cutter having circular inserts.

  16. Investigation of Catalytic Effects and Compositional Variations in Desorption Characteristics of LiNH2-nanoMgH2

    Directory of Open Access Journals (Sweden)

    Sesha S. Srinivasan

    2017-07-01

    Full Text Available LiNH2 and a pre-processed nanoMgH2 with 1:1 and 2:1 molar ratios were mechano-chemically milled in a high-energy planetary ball mill under inert atmosphere, and at room temperature and atmospheric pressure. Based on the thermogravimetric analysis (TGA experiments, 2LiNH2-nanoMgH2 demonstrated superior desorption characteristics when compared to the LiNH2-nanoMgH2. The TGA studies also revealed that doping 2LiNH2-nanoMgH2 base material with 2 wt. % nanoNi catalyst enhances the sorption kinetics at lower temperatures. Additional investigation of different catalysts showed improved reaction kinetics (weight percentage of H2 released per minute of the order TiF3 > nanoNi > nanoTi > nanoCo > nanoFe > multiwall carbon nanotube (MWCNT, and reduction in the on-set decomposition temperatures of the order nanoCo > TiF3 > nanoTi > nanoFe > nanoNi > MWCNT for the base material 2LiNH2-nanoMgH2. Pristine and catalyst-doped 2LiNH2-nanoMgH2 samples were further probed by X-ray diffraction, Fourier transform infrared spectroscopy, transmission and scanning electron microscopies, thermal programmed desorption and pressure-composition-temperature measurements to better understand the improved performance of the catalyst-doped samples, and the results are discussed.

  17. Mechanical alloying and reactive milling in a high energy planetary mill

    International Nuclear Information System (INIS)

    Jiang Xianjin; Trunov, Mikhaylo A.; Schoenitz, Mirko; Dave, Rajesh N.; Dreizin, Edward L.

    2009-01-01

    Powder refinement in a planetary mill (Retsch PM 400-MA) is investigated experimentally and analyzed using discrete element modeling (DEM). Refinement is defined as the average size of the individual components in a composite powder. The specific milling dose, defined as the product of charge ratio and milling time, is used as an experimental parameter tracking the progress of the material refinement. This parameter is determined experimentally for milling of boron and titanium powders, for which the time of initiation of a self-sustained reaction is measured under different milling conditions. It is assumed that the reaction becomes self-sustaining when the same powder refinement is achieved. The DEM calculations established that the milling balls primarily roll along the milling container's perimeter. The inverse of the rate of energy dissipation resulting from this rolling motion is used as the DEM analog of the specific milling dose. The results correlate well with experimental observations.

  18. Silicon/Wolfram Carbide@Graphene composite: enhancing conductivity and structure stability in amorphous-silicon for high lithium storage performance

    International Nuclear Information System (INIS)

    Sun, Wei; Hu, Renzong; Liu, Hui; Zhang, Hanying; Liu, Jiangwen; Yang, Lichun; Wang, Haihui; Zhu, Min

    2016-01-01

    Highlights: • Two-step ball milling was used to produce an amorphous-Si/WC@Graphene(SW@G) composite. • Concrete-like core-shell structure with high stability was designed. • Multiscale WC particle strengthen the inside structure. • Graphene coating outside much enhanced the cycling stability and conductivity. • The SW@G anode exhibited long cycle life and superior volumetric capacity. - Abstract: Improving the electron conductivity and lithiated structure stability for Si anodes can result in high stable capacity in cells. A Silicon/Wolfram Carbide@Graphene (SW@G) composite anode is designed and produced by a simple two-step ball milling the mixture of coarse-grained Si with good conductive wolfram carbide (WC) and graphite. The SW@G composite consists of multiple-scale WC particles, which are uniformly distributed in amorphous Si matrices, and wrapped by graphene nanosheets (GNs) on the outside. Owing to the unique concrete-like core-shell structure, the wrapping of GNs on the Si improves the conductivity and structural stability of the composite. The inner WC particles which tightly connect the Si and graphene act as the cornerstone to resist large volumetric expansion of Si during charge/discharge, and in particular serve as the high-speed channels of electrons as well as provide more interface paths for Li + to accelerate their transfer inside the Si. These contribute to the excellent electrochemical properties of SW@G composite anode, including high volumetric capacity (three times higher than that of graphite), superior rate capability, and long-life stable cycleability. The synthetic method developed in this work paves the way for large-scale manufacturing of high performance Li storage anodes using commercially available materials and technologies.

  19. Effect of milling variables on powder character and sintering behaviour of 434L ferritic stainless steel-Al2O3 composites

    International Nuclear Information System (INIS)

    Mukherjee, S.K.; Upadhyaya, G.S.

    1985-01-01

    Ball milling of ferritic stainless steel-4 vol% Al 2 O 3 powder was carried out for the duration up to 222 ks. Attritor milling of ferritic stainless steel-6 vol% Al 2 O 3 were also carried out for the duration up to 32.4 ks. The characterization of the milled powders were performed. The sintering of ball milled powders was carried out at 1623 K for 10.8 ks in hydrogen. The premix of as received stainless steel powder and the attritor milled powder was also sintered at 1623 K for 3.6 ks in hydrogen. The results showed that an optimum ball milling period in between 58 and 173 ks was required to achieve better sintered properties. The attritor milling was more effective in grinding the powders as compared to ball milling, and the sinterability was also higher for such powders. (author)

  20. Bulk superhard B-C-N nanocomposite compact and method for preparing thereof

    Science.gov (United States)

    Zhao, Yusheng; He, Duanwei

    2004-07-06

    Bulk, superhard, B-C-N nanocomposite compact and method for preparing thereof. The bulk, superhard, nanocomposite compact is a well-sintered compact and includes nanocrystalline grains of at least one high-pressure phase of B-C-N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compact has a Vicker's hardness of about 41-68 GPa. It is prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture, and sintering the encapsulated ball-milled mixture at a pressure of about 5-25 GPa and at a temperature of about 1000-2500 K.

  1. Superthermostability of nanoscale TIC-reinforced copper alloys manufactured by a two-step ball-milling process

    Science.gov (United States)

    Wang, Fenglin; Li, Yunping; Xu, Xiandong; Koizumi, Yuichiro; Yamanaka, Kenta; Bian, Huakang; Chiba, Akihiko

    2015-12-01

    A Cu-TiC alloy, with nanoscale TiC particles highly dispersed in the submicron-grained Cu matrix, was manufactured by a self-developed two-step ball-milling process on Cu, Ti and C powders. The thermostability of the composite was evaluated by high-temperature isothermal annealing treatments, with temperatures ranging from 727 to 1273 K. The semicoherent nanoscale TiC particles with Cu matrix, mainly located along the grain boundaries, were found to exhibit the promising trait of blocking grain boundary migrations, which leads to a super-stabilized microstructures up to approximately the melting point of copper (1223 K). Furthermore, the Cu-TiC alloys after annealing at 1323 K showed a slight decrease in Vickers hardness as well as the duplex microstructure due to selective grain growth, which were discussed in terms of hardness contributions from various mechanisms.

  2. Research Progress on Fe-based Amorphous Coatings

    Directory of Open Access Journals (Sweden)

    LIANG Xiu-bing

    2017-09-01

    Full Text Available The latest research progresses on Fe-based amorphous coatings were reviewed. The typical alloy system and the classification of Fe-based amorphous coatings were clarified. The status, progress and development of the Fe-based amorphous coatings prepared by thermal spray processing and laser cladding process were discussed. The main mechanical properties and potential applications of the Fe-based amorphous coatings were also described. Furthermore, based on the main problems mentioned above, the future development of the Fe-based amorphous coatings was discussed, including the exploitation preparation technologies of high amorphous content of the Fe-based coatings, the development of the low cost and high performance Fe-based coating alloys system, the broadening application of Fe-based amorphous coatings, and so on.

  3. N-type nano-silicon powders with ultra-low electrical resistivity as anode materials in lithium ion batteries

    Science.gov (United States)

    Yue, Zhihao; Zhou, Lang; Jin, Chenxin; Xu, Guojun; Liu, Liekai; Tang, Hao; Li, Xiaomin; Sun, Fugen; Huang, Haibin; Yuan, Jiren

    2017-06-01

    N-type silicon wafers with electrical resistivity of 0.001 Ω cm were ball-milled to powders and part of them was further mechanically crushed by sand-milling to smaller particles of nano-size. Both the sand-milled and ball-milled silicon powders were, respectively, mixed with graphite powder (silicon:graphite = 5:95, weight ratio) as anode materials for lithium ion batteries. Electrochemical measurements, including cycle and rate tests, present that anode using sand-milled silicon powder performed much better. The first discharge capacity of sand-milled silicon anode is 549.7 mAh/g and it is still up to 420.4 mAh/g after 100 cycles. Besides, the D50 of sand-milled silicon powder shows ten times smaller in particle size than that of ball-milled silicon powder, and they are 276 nm and 2.6 μm, respectively. In addition, there exist some amorphous silicon components in the sand-milled silicon powder excepting the multi-crystalline silicon, which is very different from the ball-milled silicon powder made up of multi-crystalline silicon only.

  4. Comparison of particle sizes between 238PuO2 before aqueous processing, after aqueous processing, and after ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Mulford, Roberta Nancy [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-02-06

    Particle sizes determined for a single lot of incoming Russian fuel and for a lot of fuel after aqueous processing are compared with particle sizes measured on fuel after ball-milling. The single samples of each type are believed to have particle size distributions typical of oxide from similar lots, as the processing of fuel lots is fairly uniform. Variation between lots is, as yet, uncharacterized. Sampling and particle size measurement methods are discussed elsewhere.

  5. Investigation of planetary milling for nano-silicon carbide reinforced aluminium metal matrix composites

    Energy Technology Data Exchange (ETDEWEB)

    Kollo, Lauri, E-mail: lauri.kollo@staff.ttu.e [Laboratory of Advanced Materials Processing, EMPA, Feuerwerkerstrasse 39, 3602 Thun (Switzerland); Department of Materials Engineering, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Leparoux, Marc; Bradbury, Christopher R.; Jaeggi, Christian [Laboratory of Advanced Materials Processing, EMPA, Feuerwerkerstrasse 39, 3602 Thun (Switzerland); Carreno-Morelli, Efrain; Rodriguez-Arbaizar, Mikel [University of Applied Sciences of Western Switzerland, Design and Materials Unit, 1950 Sion (Switzerland)

    2010-01-21

    High-energy planetary milling was used for mixing aluminium powders with 1 vol.% of silicon carbide (SiC) nanoparticles. A number of milling parameters were modified for constituting the relationship between the energy input from the balls and the hardness of the bulk nanocomposite materials. It was shown that mixing characteristics and reaction kinetics with stearic acid as process control agent can be estimated by normalised input energy from the milling bodies. For this, the additional parameter characterising the vial filling was determined experimentally. Depending on the ball size, a local minimum in filling parameter was found, laying at 25 or 42% filling of the vial volume for the balls with diameter of 10 and 20 mm, respectively. These regions should be avoided to achieve the highest milling efficiency.After a hot compaction, fourfold difference of hardness for different milling conditions was detected. Therewith the hardness of the Al-1 vol.% nanoSiC composite could be increased from 47 HV{sub 0.5} of pure aluminium to 163 HV{sub 0.5} when milling at the highest input energy levels.

  6. Characterization of BaBi2Ta2O9 prepared through amorphous precursor

    International Nuclear Information System (INIS)

    Maczka, M.; Kepinski, L.; Hermanowicz, K.; Dacko, S.; Czapla, Z.; Hanuza, J.

    2011-01-01

    Research highlights: → Formation of Bi-layered BaBi 2 Ta 2 O 9 proceeds via an intermediate fluorite phase. → Mechanochemical activation lowers the synthesis temperature by 150-200 deg. C. → The lateral size of the synthesized plate-like crystallites is about 100-200 nm. → Properties of the synthesized crystallites are different from the bulk material. - Abstract: Formation of ferroelectric BaBi 2 Ta 2 O 9 by annealing of an amorphous precursor prepared by high energy milling in ball mill has been studied by X-ray, scanning electron microscopy (SEM), Raman, infrared spectroscopy (IR), diffuse reflectivity and dielectric measurements. Our results show that formation of Bi-layered BaBi 2 Ta 2 O 9 proceeds via an intermediate fluorite phase. Mechanochemical activation allows obtaining BaBi 2 Ta 2 O 9 at short time and much lower temperatures than those required in a conventional solid state reaction. The lateral size of the plate-like crystallites is about 100-200 nm and properties of the synthesized particles are different compared to the bulk material.

  7. Ball-milling effect on Indonesian natural bentonite for manganese removal from acid mine drainage

    Directory of Open Access Journals (Sweden)

    Prastistho Widyawanto

    2018-01-01

    Full Text Available The influences of mechanical milling on Indonesian Natural Bentonite (INB characteristics and manganese (Mn removal from acid mine drainage (AMD were investigated. The INB characteristics were observed by scanning electron microscope (SEM, X-ray diffraction (XRD, nitrogen adsorption-desorption for specific surface area (SSA and microporosity measurement, cation exchange capacity (CEC and particle size distribution (PSD analyzer. Four minutes milling with frequency 20 Hz on INB caused morphological change which showed more crumbled and destructed particle, lost the (001 peak but still retained the (100 peak that indicated delamination of montmorillonite mineral without breaking the tetrahedral-octahedral-tetrahedral (T-O-T structure, rose the CEC from 28.49 meq/100g to 35.51 meq/100g, increase in the SSA from 60.63 m2/g to 104.88 m2/g, significant increase in microporosity which described in the t plots and decrease in the mean particle size distribution peak from 49.28 μm to 38.84 μm. The effect of contact time and effect of adsorbent dosage on Mn sorption was studied. Both unmilled and milled samples reached equilibrium at 24 hours and the pH rose from 4 to 7 in first 30 minutes. The Mn removal percentage increased significantly after milling. Using Langmuir isotherm, the maximum adsorbed metals (qmax also increased from 0.570 to 4.219 mg/g.

  8. The Influence of Milling on the Dissolution Performance of Simvastatin

    Directory of Open Access Journals (Sweden)

    Thomas Rades

    2010-12-01

    Full Text Available Particle size reduction is a simple means to enhance the dissolution rate of poorly water soluble BCS-class II and IV drugs. However, the major drawback of this process is the possible introduction of process induced disorder. Drugs with different molecular arrangements may exhibit altered properties such as solubility and dissolution rate and, therefore, process induced solid state modifications need to be monitored. The aim of this study was two-fold: firstly, to investigate the dissolution rates of milled and unmilled simvastatin; and secondly, to screen for the main milling factors, as well as factor interactions in a dry ball milling process using simvastatin as model drug, and to optimize the milling procedure with regard to the opposing responses particle size and process induced disorder by application of a central composite face centered design. Particle size was assessed by scanning electron microscopy (SEM and image analysis. Process induced disorder was determined by partial least squares (PLS regression modeling of respective X-ray powder diffractograms (XRPD and Raman spectra. Valid and significant quadratic models were built. The investigated milling factors were milling frequency, milling time and ball quantity at a set drug load, out of which milling frequency was found to be the most important factor for particle size as well as process induced disorder. Milling frequency and milling time exhibited an interaction effect on the responses. The optimum milling settings using the maximum number of milling balls (60 balls with 4 mm diameter was determined to be at a milling frequency of 21 Hz and a milling time of 36 min with a resulting primary particle size of 1.4 μm and a process induced disorder of 6.1% (assessed by Raman spectroscopy and 8.4% (assessed by XRPD, at a set optimization limit of < 2 μm for particle size and < 10% for process induced disorder. This optimum was tested experimentally and the process induced disorder

  9. Solvent-Free Biginelli Reactions Catalyzed by Hierarchical Zeolite Utilizing a Ball Mill Technique: A Green Sustainable Process

    Directory of Open Access Journals (Sweden)

    Ameen Shahid

    2017-03-01

    Full Text Available A sustainable, green one-pot process for the synthesis of dihydropyrimidinones (DHPMs derivatives by a three-component reaction of β-ketoester derivatives, aldehyde and urea or thiourea over the alkali-treated H-ZSM-5 zeolite under ball-milling was developed. Isolation of the product with ethyl acetate shadowed by vanishing of solvent was applied. The hierachical zeolite catalyst (MFI27_6 showed high yield (86%–96% of DHPMs in a very short time (10–30 min. The recyclability of the catalyst for the subsequent reactions was examined in four subsequent runs. The catalyst was shown to be robust without a detectable reduction in catalytic activity, and high yields of products showed the efficient protocol of the Biginelli reactions.

  10. Effect of ball milling and dynamic compaction on magnetic properties of Al{sub 2}O{sub 3}/Co(P) composite particles

    Energy Technology Data Exchange (ETDEWEB)

    Denisova, E. A. [Kirensky Institute of Physics SB RAS, Krasnoyarsk (Russian Federation); Krasnoyarsk Institute of Railways Transport, Krasnoyarsk (Russian Federation); Kuzovnikova, L. A. [Krasnoyarsk Institute of Railways Transport, Krasnoyarsk (Russian Federation); Iskhakov, R. S., E-mail: rauf@iph.krasn.ru; Eremin, E. V. [Kirensky Institute of Physics SB RAS, Krasnoyarsk (Russian Federation); Bukaemskiy, A. A. [Institut fur Sicherheitsforschung und Reaktortechnik, D-52425 Juelich (Germany); Nemtsev, I. V. [Krasnoyarsk Scientific Center SB RAS, Krasnoyarsk (Russian Federation)

    2014-05-07

    The evolution of the magnetic properties of composite Al{sub 2}O{sub 3}/Co(P) particles during ball milling and dynamic compaction is investigated. To prepare starting composite particles, the Al{sub 2}O{sub 3} granules were coated with a Co{sub 95}P{sub 5} shell by electroless plating. The magnetic and structural properties of the composite particles are characterized by scanning electron microscopy, X-ray diffraction, and the use of the Physical Property Measurement System. The use of composite core-shell particles as starting powder for mechanoactivation allows to decrease treatment duration to 1 h and to produce a more homogeneous bulk sample than in the case of the mixture of Co and Al{sub 2}O{sub 3} powders. The magnetic properties of the milled composite particles are correlated with changes in the microstructure. Reduction in grain size of Co during milling leads to an increase of the volume fraction of superparamagnetic particles and to a decrease of the saturation magnetization. The local magnetic anisotropy field depends on the amount of hcp-Co phase in sample. The anisotropy field value decreases from 8.4 kOe to 3.8 kOe with an increase in milling duration up to 75 min. The regimes of dynamic compaction were selected so that the magnetic characteristics—saturation magnetization and coercive field—remained unchanged.

  11. Enhancing the Hardness and Compressive Response of Magnesium Using Complex Composition Alloy Reinforcement

    Directory of Open Access Journals (Sweden)

    Khin Sandar Tun

    2018-04-01

    Full Text Available The present study reports the development of new magnesium composites containing complex composition alloy (CCA particles. Materials were synthesized using a powder metallurgy route incorporating hybrid microwave sintering and hot extrusion. The presence and variation in the amount of ball-milled CCA particles (2.5 wt %, 5 wt %, and 7.5 wt % in a magnesium matrix and their effect on the microstructure and mechanical properties of Mg-CCA composites were investigated. The use of CCA particle reinforcement effectively led to a significant matrix grain refinement. Uniformly distributed CCA particles were observed in the microstructure of the composites. The refined microstructure coupled with the intrinsically high hardness of CCA particles (406 HV contributed to the superior mechanical properties of the Mg-CCA composites. A microhardness of 80 HV was achieved in a Mg-7.5HEA (high entropy alloy composite, which is 1.7 times higher than that of pure Mg. A significant improvement in compressive yield strength (63% and ultimate compressive strength (79% in the Mg-7.5CCA composite was achieved when compared to that of pure Mg while maintaining the same ductility level. When compared to ball-milled amorphous particle-reinforced and ceramic-particle-reinforced Mg composites, higher yield and compressive strengths in Mg-CCA composites were achieved at a similar ductility level.

  12. Magneto-optical properties of α-Fe2O3@ZnO nanocomposites prepared by the high energy ball-milling technique

    Science.gov (United States)

    Chaudhury, Chandana Roy; Roychowdhury, Anirban; Das, Anusree; Das, Dipankar

    2016-05-01

    Magnetic-fluorescent nanocomposites (NCs) with 10 wt% of α-Fe2O3 in ZnO have been prepared by the high energy ball-milling. The crystallite sizes of α-Fe2O3 and ZnO in the NCs are found to vary from 65 nm to 20 nm and 47 nm to 15 nm respectively as milling time is increased from 2 to 30 h. XRD analysis confirms presence of α-Fe2O3 and ZnO in pure form in all the NCs. UV-vis study of the NCs shows a continuous blue-shift of the absorption peak and a steady increase of band gap of ZnO with increasing milling duration that are assigned to decreasing particle size of ZnO in the NCs. Photoluminescence (PL) spectra of the NCs reveal three weak emission bands in the visible region at 421, 445 and 485 nm along with the strong near band edge emission at 391 nm. These weak emission bands are attributed to different defect - related energy levels e.g. Zn-vacancy, Zn interstitial and oxygen vacancy. Dc and ac magnetization measurements show presence of weakly interacting superparamagnetic (SPM) α-Fe2O3 particles in the NCs. 57Fe-Mössbauer study confirms presence of SPM hematite in the sample milled for 30 h. Positron annihilation lifetime measurements indicate presence of cation vacancies in ZnO nanostructures confirming results of PL studies.

  13. The Influence of Pressure on the Intrinsic Dissolution Rate of Amorphous Indomethacin

    Directory of Open Access Journals (Sweden)

    Korbinian Löbmann

    2014-08-01

    Full Text Available New drug candidates increasingly tend to be poorly water soluble. One approach to increase their solubility is to convert the crystalline form of a drug into the amorphous form. Intrinsic dissolution testing is an efficient standard method to determine the intrinsic dissolution rate (IDR of a drug and to test the potential dissolution advantage of the amorphous form. However, neither the United States Pharmacopeia (USP nor the European Pharmacopeia (Ph.Eur state specific limitations for the compression pressure in order to obtain compacts for the IDR determination. In this study, the influence of different compression pressures on the IDR was determined from powder compacts of amorphous (ball-milling indomethacin (IND, a glass solution of IND and poly(vinylpyrrolidone (PVP and crystalline IND. Solid state properties were analyzed with X-ray powder diffraction (XRPD and the final compacts were visually observed to study the effects of compaction pressure on their surface properties. It was found that there is no significant correlation between IDR and compression pressure for crystalline IND and IND–PVP. This was in line with the observation of similar surface properties of the compacts. However, compression pressure had an impact on the IDR of pure amorphous IND compacts. Above a critical compression pressure, amorphous particles sintered to form a single compact with dissolution properties similar to quench-cooled disc and crystalline IND compacts. In such a case, the apparent dissolution advantage of the amorphous form might be underestimated. It is thus suggested that for a reasonable interpretation of the IDR, surface properties of the different analyzed samples should be investigated and for amorphous samples the IDR should be measured also as a function of the compression pressure used to prepare the solid sample for IDR testing.

  14. Pseudobrookite-type MgTi2O5 water purification filter with controlled particle morphology

    Directory of Open Access Journals (Sweden)

    Yuta Nakagoshi

    2015-09-01

    Full Text Available Pseudobrookite-type oxide-based ceramics, such as Al2TiO5 and MgTi2O5, have recently been studied as porous ceramic membranes. Here, the effect of LiF doping on the morphology of MgTi2O5 particles is presented in detail. Water purification filters were produced using porous MgTi2O5, with different particle morphologies. MgCO3 (basic and TiO2 powders with various LiF contents were wet-ball milled, dried, and then, calcined in air at 1100 °C to obtain the MgTi2O5 powders. The powder compacts were sintered at 1000–1200 °C to produce the MgTi2O5 disk filters. The 0.5 wt.% LiF-doped MgTi2O5 disk filter, with elongated grains, showed well-balanced performance removing boehmite particles with diameter of 0.7 μm. Non-doped MgTi2O5 disk filter with equiaxed grains was suitable for precise filtration.

  15. Ball-milling synthesis of ZnO@sulphur/carbon nanotubes and Ni(OH)_2@sulphur/carbon nanotubes composites for high-performance lithium-sulphur batteries

    International Nuclear Information System (INIS)

    Gu, Xingxing; Tong, Chuan-jia; Wen, Bo; Liu, Li-min; Lai, Chao; Zhang, Shanqing

    2016-01-01

    Highlights: • Metal oxides or hydroxides coating sulfur-based composite are successfully prepared. • Large-scale synthesis can be realized via the facile wet ball-milling strategy. • Density functional theory (DFT) calculation is applied to calculate adsorption energy. • ZnO exhibits a higher adsorption energy for Li_2S_8 than that Ni(OH)_2. • ZnO@sulphur/carbon nanotubes composite show excellent cycle and discharge performance. - Abstract: Zinc oxide wrapped sulphur/carbon nanotubes (ZnO@S/CNT) and nickel hydroxide wrapped sulphur/carbon nanotubes (Ni(OH)_2@S/CNT) nanocomposites are prepared using a simple, low cost and scalable ball-milling method. As the cathodes in Li-S batteries, the as-prepared ZnO@S/CNT composite illustrates a superior high initial capacity of 1663 mAh g"−"1 at a charge/discharge rate of 160 mA g"−"1, and maintains a reversible capacity at approximately 942 mAh g"−"1 after 70 cycles. While for Ni(OH)_2@S/CNT composites, its initial capacity is also as high as 1331 mAh g"−"1, but a poorer cycling stability is presented. When the charge/discharge current is increased to 1600 mA g"−"1, a high reversible capacity of 698 mAh g"−"1 after 200 cycles still can be obtained for the ZnO@S/CNT composite, far better than that of Ni(OH)_2@S/CNT composites. The better cycling performance and high discharge capacity can be attributed to the strong interactions between ZnO and S_x"2"− species, which is verified by the density functional theory (DFT) calculation result that the ZnO exhibits a higher adsorption energy for Li_2S_8 than the Ni(OH)_2.

  16. Formation mechanism of coamorphous drug−amino acid mixtures

    DEFF Research Database (Denmark)

    Jensen, Katrine Birgitte Tarp; Larsen, Flemming Hofmann; Cornett, Claus

    2015-01-01

    Two coamorphous drug−amino acid systems, indomethacin−tryptophan (Ind−Trp) and furosemide−tryptophan Fur−Trp), were analyzed toward their ease of amorphization and mechanism of coamorphization during ball milling. The two mixtures were compared to the corresponding amorphization of the pure drug...

  17. DEM modeling of ball mills with experimental validation: influence of contact parameters on charge motion and power draw

    Science.gov (United States)

    Boemer, Dominik; Ponthot, Jean-Philippe

    2017-01-01

    Discrete element method simulations of a 1:5-scale laboratory ball mill are presented in this paper to study the influence of the contact parameters on the charge motion and the power draw. The position density limit is introduced as an efficient mathematical tool to describe and to compare the macroscopic charge motion in different scenarios, i.a. with different values of the contact parameters. While the charge motion and the power draw are relatively insensitive to the stiffness and the damping coefficient of the linear spring-slider-damper contact law, the coefficient of friction has a strong influence since it controls the sliding propensity of the charge. Based on the experimental calibration and validation by charge motion photographs and power draw measurements, the descriptive and predictive capabilities of the position density limit and the discrete element method are demonstrated, i.e. the real position of the charge is precisely delimited by the respective position density limit and the power draw can be predicted with an accuracy of about 5 %.

  18. Effect of zirconium on grain growth and mechanical properties of a ball-milled nanocrystalline FeNi alloy

    Energy Technology Data Exchange (ETDEWEB)

    Kotan, Hasan, E-mail: hkotan@ncsu.edu [Department of Materials Science and Engineering, NC State University, 911 Partners Way, Room 3078, Raleigh, NC 27606-7907 (United States); Darling, Kris A. [U.S. Army Research Laboratory, Weapons and Materials Research Directorate, RDRL-WMM-F, Aberdeen Proving Ground, MD 21005-5069 (United States); Saber, Mostafa; Koch, Carl C.; Scattergood, Ronald O. [Department of Materials Science and Engineering, NC State University, 911 Partners Way, Room 3078, Raleigh, NC 27606-7907 (United States)

    2013-02-25

    Highlights: Black-Right-Pointing-Pointer Pure Fe, Fe{sub 92}Ni{sub 8}, and Fe{sub 91}Ni{sub 8}Zr{sub 1} powders were hardened up to 10 GPa by ball milling. Black-Right-Pointing-Pointer Annealing of Fe and Fe{sub 92}Ni{sub 8} leads to reduced hardness and extensive grain growth. Black-Right-Pointing-Pointer The addition of Zr to Fe{sub 92}Ni{sub 8} increases its stability and strength by second phases. Black-Right-Pointing-Pointer The second phases are found to promote the stability of Fe{sub 91}Ni{sub 8}Zr{sub 1} by Zener pinning. Black-Right-Pointing-Pointer The Zr-containing precipitates contribute to the overall strength of the material. - Abstract: Grain growth of ball-milled pure Fe, Fe{sub 92}Ni{sub 8}, and Fe{sub 91}Ni{sub 8}Zr{sub 1} alloys has been studied using X-ray diffractometry (XRD), focused ion beam (FIB) microscopy and transmission electron microscopy (TEM). Mechanical properties with respect to compositional changes and annealing temperatures have been investigated using microhardness and shear punch tests. We found the rate of grain growth of the Fe{sub 91}Ni{sub 8}Zr{sub 1} alloy to be much less than that of pure Fe and the Fe{sub 92}Ni{sub 8} alloy at elevated temperatures. The microstructure of the ternary Fe{sub 91}Ni{sub 8}Zr{sub 1} alloy remains nanoscale up to 700 Degree-Sign C where only a few grains grow abnormally whereas annealing of pure iron and the Fe{sub 92}Ni{sub 8} alloy leads to extensive grain growth. The grain growth of the ternary alloy at high annealing temperatures is coupled with precipitation of Fe{sub 2}Zr. A fine dispersion of precipitated second phase is found to promote the microstructural stability at high annealing temperatures and to increase the hardness and ultimate shear strength of ternary Fe{sub 91}Ni{sub 8}Zr{sub 1} alloy drastically when the grain size is above nanoscale.

  19. Mechanical and Microstructure Study of Nickel-Based ODS Alloys Processed by Mechano-Chemical Bonding and Ball Milling

    Science.gov (United States)

    Amare, Belachew N.

    Due to the need to increase the efficiency of modern power plants, land-based gas turbines are designed to operate at high temperature creating harsh environments for structural materials. The elevated turbine inlet temperature directly affects the materials at the hottest sections, which includes combustion chamber, blades, and vanes. Therefore, the hottest sections should satisfy a number of material requirements such as high creep strength, ductility at low temperature, high temperature oxidation and corrosion resistance. Such requirements are nowadays satisfied by implementing superalloys coated by high temperature thermal barrier coating (TBC) systems to protect from high operating temperature required to obtain an increased efficiency. Oxide dispersive strengthened (ODS) alloys are being considered due to their high temperature creep strength, good oxidation and corrosion resistance for high temperature applications in advanced power plants. These alloys operating at high temperature are subjected to different loading systems such as thermal, mechanical, and thermo-mechanical combined loads at operation. Thus, it is critical to study the high temperature mechanical and microstructure properties of such alloys for their structural integrity. The primary objective of this research work is to investigate the mechanical and microstructure properties of nickel-based ODS alloys produced by combined mechano-chemical bonding (MCB) and ball milling subjected to high temperature oxidation, which are expected to be applied for high temperature turbine coating with micro-channel cooling system. Stiffness response and microstructure evaluation of such alloy systems was studied along with their oxidation mechanism and structural integrity through thermal cyclic exposure. Another objective is to analyze the heat transfer of ODS alloy coatings with micro-channel cooling system using finite element analysis (FEA) to determine their feasibility as a stand-alone structural

  20. Structure and soft magnetic properties of the bulk samples prepared by compaction of the mixtures of Co-based and Fe-based powders

    International Nuclear Information System (INIS)

    Fuezer, J.; Bednarcik, J.; Kollar, P.; Roth, S.

    2007-01-01

    Ball milling of CoFeZrB ribbons and subsequent compaction of the resulting powders were used to prepare bulk amorphous samples. Further, two sets of powder samples were prepared by cryomilling of FeCuNbMoSiB alloy in amorphous and nanocrystalline state. Amorphous and nanocrystalline FeCuNbMoSiB powders were blended with CoFeZrB powder at different concentrations. Such powder mixtures were consolidated and several bulk nanocomposites have been synthesized. An addition of nanocrystalline or amorphous FeCuNbMoSiB powder to amorphous CoFeZrB powder caused a decrease of the magnetostriction of the resultant bulk samples, while the coercivity shows an opposite behavior. Our results show that the powder consolidation by hot pressing is an alternative method for the preparation of bulk metallic glasses, which are difficult to prepare by casting methods

  1. Efek Waktu Wet Milling dan Suhu Annealing Terhadap Sifat Fisis, Mikrostruktur dan Magnet dari Flakes NdFeB

    OpenAIRE

    Sipahutar, Wahyu Solafide

    2015-01-01

    Had made research manufacture NdFeB magnets of flakes of wet milling process using a ball mill to the physic properties, microstructure, and magnetic properties with variations milling time is 16 hours, 24 hours, 48 hours, 72 hours. Powder result of mechanical milling using a ball mill and then analyzed the resulting particle size by using PSA and XRD. Then do the manufacture of test samples in the form of pellets by compaction process through print isotropy. Having obtained a sample of pelle...

  2. A comparison of amorphous calcium carbonate crystallization in aqueous solutions of MgCl2 and MgSO4: implications for paleo-ocean chemistry

    Science.gov (United States)

    Han, Mei; Zhao, Yanyang; Zhao, Hui; Han, Zuozhen; Yan, Huaxiao; Sun, Bin; Meng, Ruirui; Zhuang, Dingxiang; Li, Dan; Liu, Binwei

    2018-04-01

    Based on the terminology of "aragonite seas" and "calcite seas", whether different Mg sources could affect the mineralogy of carbonate sediments at the same Mg/Ca ratio was explored, which was expected to provide a qualitative assessment of the chemistry of the paleo-ocean. In this work, amorphous calcium carbonate (ACC) was prepared by direct precipitation in anhydrous ethanol and used as a precursor to study crystallization processes in MgSO4 and MgCl2 solutions having different concentrations at 60 °C (reaction times 240 and 2880 min). Based on the morphology of the aragonite crystals, as well as mineral saturation indices and kinetic analysis of geochemical processes, it was found that these crystals formed with a spherulitic texture in 4 steps. First, ACC crystallized into columnar Mg calcite by nearly oriented attachment. Second, the Mg calcite changed from columnar shapes into smooth dumbbell forms. Third, the Mg calcite transformed into rough dumbbell or cauliflower-shaped aragonite forms by local dissolution and precipitation. Finally, the aragonite transformed further into spherulitic radial and irregular aggregate forms. The increase in Ca2+ in the MgSO4 solutions compared with the MgCl2 solutions indicates the fast dissolution and slow precipitation of ACC in the former solutions. The phase transition was more complete in the 0.005 M MgCl2 solution, whereas Mg calcite crystallized from the 0.005 M MgSO4 solution, indicating that Mg calcite could be formed more easily in an MgSO4 solution. Based on these findings, aragonite and Mg calcite relative to ACC could be used to provide a qualitative assessment of the chemistry of the paleo-ocean. Therefore, calcite seas relative to high-Mg calcite could reflect a low concentration MgSO4 paleo-ocean, while aragonite seas could be related to an MgCl2 or high concentration of MgSO4 paleo-ocean.

  3. Mechanical Properties and Fabrication of Nanostructured Mg_2SiO_4-MgAl_2O_4 Composites by High-Frequency Induction Heated Combustion

    International Nuclear Information System (INIS)

    Shon, In-Jin; Kang, Hyun-Su; Hong, Kyung-Tae; Doh, Jung-Mann; Yoon, Jin-Kook

    2011-01-01

    Nanopowders of MgO, Al_2O_3 and SiO_2 were made by high energy ball milling. The rapid sintering of nanostructured MgAl_2O_4-Mg_2SiO_4 composites was investigated by a high-frequency induction heating sintering process. The advantage of this process is that it allows very quick densification to near theoretical density and inhibition of grain growth. Nanocrystalline materials have received much attention as advanced engineering materials with improved physical and mechanical properties. As nanomaterials possess high strength, high hardness, excellent ductility and toughness, undoubtedly, more attention has been paid for the application of nanomaterials. Highly dense nanostructured MgAl_2O_4-Mg_2SiO_4 composites were produced with simultaneous application of 80 MPa pressure and induced output current of total power capacity (15 kW) within 2 min. The sintering behavior, gain size and mechanical properties of MgAl_2O_4-Mg_2SiO_4 composites were investigated.

  4. Pengaruh Penambahan Ni, Cu, dan Al dan Waktu Milling pada Mechanical Alloying Terhadap Sifat Absorpsi dan Desorpsi Mg sebagai Material Penyimpan Hidrogen

    Directory of Open Access Journals (Sweden)

    Febrian Budi Pratama

    2012-09-01

    Full Text Available Mg merupakan salah satu material yang digunakan sebagai material penyimpan hidrogen dengan membentuk MgH2. Sifat absorpsi dan desorpsi hidrogen dari suatu metal hidrida salah satunya tergantung  pada bahan, unsur penambah, dan metode pembuatannya. Pada penelitian kali ini Mg sebagai material penyimpan hidrogen dihasilkan melalui metode mechanical alloying dengan unsur penambah Ni, Cu, dan Al dan variasi waktu milling 10, 20, 30 jam. Selanjutnya sampel dilakukan pengujian SEM, XRD, DSC, dan Uji hidrogenisasi. Dari data uji diperoleh bahwa meningkatnya waktu milling menurunkan ukuran partikel sehingga meningkatkan wt% hidrogen terabsorb dan menurunkan temperatur onset desorpsi. Namun efek aglomerasi dan coldwelding yang berlebih pada proses mechanical alloying mengakibatkan ukuran partikel menjadi lebih besar. Unsur pemadu Al dan Cu berfungsi sebagai katalis, sedangkan Ni berfungsi sebagai pemadu yang ikut bereaksi dengan hidrogen. Mg10wt%Al dengan waktu milling 20 jam mempunyai nilai weight percent terbaik H2 yaitu 0.38% dalam temperatur hidrogenisasi 2500C, tekanan 3 atm, dan waktu tahan 1 jam. Sedangkan Mg10wt%Al dengan waktu milling 30 jam memiliki temperatur onset paling rendah yaitu 341.490C Kata Kunci— Absorpsi, Desorpsi, Material Penyimpan Hidrogen, Mechanical Alloying, Mg

  5. In vitro metal ion release and biocompatibility of amorphous Mg67Zn28Ca5 alloy with/without gelatin coating

    International Nuclear Information System (INIS)

    Chan, W.Y.; Chian, K.S.; Tan, M.J.

    2013-01-01

    Amorphous zinc-rich Mg–Zn–Ca alloys have exhibited good tissue compatibility and low hydrogen evolution in vivo. However, suboptimal cell–surface interaction on magnesium alloy surface observed in vitro could lead to reduced integration with host tissue for regenerative purpose. This study aims to improve cell–surface interaction of amorphous Mg 67 Zn 28 Ca 5 alloy by coating a gelatin layer by electrospinning. Coated/uncoated alloys were immersed and extracted for 3 days under different CO 2 . The immersion results showed that pH and metal ion release in the alloy extracts were affected by gelatin coating and CO 2 , suggesting their roles in alloy biocorrosion and a mechanism has been proposed for the alloy–CO 2 system with/without coating. Cytotoxicity results are evident that gelatin-coated alloy with 2-day crosslinking not only exhibited no indirect cytotoxicity, but also supported attachment of L929 and MG63 cell lines around/on the alloy with high viability. Therefore, amorphous Mg 67 Zn 28 Ca 5 alloy coated with gelatin by electrospinning technique provides a useful method to improve alloy biocompatibility. - Highlights: • Electrospinning is a new method to coat amorphous Mg 67 Zn 28 Ca 5 alloy with gelatin. • Gelatin-coated alloy has differential effect on pH and ion release at various CO 2 . • L929 cell proliferation correlates with Mg 2+ level in alloy extracts. • Biomimetic gelatin coating significantly improves cell–surface interaction

  6. Quantification of process induced disorder in milled samples using different analytical techniques

    DEFF Research Database (Denmark)

    Zimper, Ulrike; Aaltonen, Jaakko; McGoverin, Cushla M.

    2012-01-01

    The aim of this study was to compare three different analytical methods to detect and quantify the amount of crystalline disorder/ amorphousness in two milled model drugs. X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Raman spectroscopy were used as analytical methods...... and indomethacin and simvastatin were chosen as the model compounds. These compounds partly converted from crystalline to disordered forms by milling. Partial least squares regression (PLS) was used to create calibration models for the XRPD and Raman data, which were subsequently used to quantify the milling......-induced crystalline disorder/ amorphousness under different process conditions. In the DSC measurements the change in heat capacity at the glass transition was used for quantification. Differently prepared amorphous indomethacin standards (prepared by either melt quench cooling or cryo milling) were compared...

  7. Coordination of arsenic and nickel to aluminum and magnesium phases in uranium mill raffinate precipitates

    International Nuclear Information System (INIS)

    Robertson, Jared; Essilfie-Dughan, J.; Lin, J.; Hendry, M. Jim

    2017-01-01

    The Key Lake U mill uses a stepwise neutralization process (pH 4.0, 6.5, 9.5, and 10.5) to treat raffinate (acidic, metal-rich wastewater) prior to safely releasing effluent to the environment. This process generates a complex mixture of precipitates that are deposited to a tailings facility. In this study, the coordination environments of As and Ni with respect to Al-Mg phases precipitated in the presence and absence of Fe in mill-generated and synthetic precipitates were defined using bulk X-ray absorption spectroscopy complemented with bulk X-ray diffraction. In low pH (pH 4.0–4.6) samples, As(V) precipitates as ferric arsenate and adsorbs to AlOHSO_4 (an amorphous hydrobasaluminite-like phase) and ferrihydrite via bidentate-binuclear complexes. Nickel(II) predominantly adsorbs to amorphous Al(OH)_3 via edge-sharing bidentate-mononuclear complexes. In high pH (pH 9.5–9.9) samples, As(V) adsorbs to amorphous Al(OH)_3_, ferrihydrite, and MgAlFe-hydrotalcite (bidentate complex). Nickel(II) octahedra adsorb to amorphous Al(OH)_3 and likely form a Ni-Al layered double hydroxide (LDH) surface precipitate on MgAlFe-hydrotalcite via Al dissolution-precipitation. In the final solids (blended low and high pH precipitates) discharged at ∼ pH 10.5, As(V) adsorbs to amorphous Al(OH)_3_, ferrihydrite, and MgAlFe-hydrotalcite. Nickel(II) adsorbs to amorphous Al(OH)_3 and forms Ni-Al LDH surface precipitates on hydrotalcite. This study demonstrates that neutralization of chemically complex wastewater precipitates multiple phases capable of controlling dissolved As and Ni concentrations. Knowledge gained from this study will aid investigations in understanding the long-term fate of these potential contaminants in the environment and can be applied to other industries and environmental systems with similar conditions. - Highlights: • Adds to the current model of aqueous contaminant control in U tailings. • As(V) adsorbs to Al(OH)_3/hydrotalcite/ferrihydrite via

  8. Preparation of bulk superhard B-C-N nanocomposite compact

    Science.gov (United States)

    Zhao, Yusheng [Los Alamos, NM; He, Duanwei [Sichuan, CN

    2011-05-10

    Bulk, superhard, B--C--N nanocomposite compacts were prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture at a pressure in a range of from about 15 GPa to about 25 GPa, and sintering the pressurized encapsulated ball-milled mixture at a temperature in a range of from about 1800-2500 K. The product bulk, superhard, nanocomposite compacts were well sintered compacts with nanocrystalline grains of at least one high-pressure phase of B--C--N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compacts had a measured Vicker's hardness in a range of from about 41 GPa to about 68 GPa.

  9. Dependence of rates of breakage on fines content in wet ball mill grinding

    Science.gov (United States)

    Bhattacharyya, Anirban

    The following research fundamentally deals with the cause and implications of nonlinearities in breakage rates of materials in wet grinding systems. The innate dependence of such nonlinearities on fines content and the milling environment during wet grinding operations is also tested and observed. Preferential breakage of coarser size fractions as compared to the finer size fractions in a particle population were observed and discussed. The classification action of the pulp was deemed to be the probable cause for such a peculiarity. Ores with varying degrees of hardness and brittleness were used for wet grinding experiments, primarily to test the variations in specific breakage rates as a function of varying hardness. For this research, limestone, quartzite, and gold ore were used. The degree of hardness is of the order of: limestone, quartzite, gold ore. Selection and breakage function parameters were determined in the course of this research. Functional forms of these expressions were used to compare experimentally derived parameter estimates. Force-fitting of parameters was not done in order to examine the realtime behavior of particle populations in wet grinding systems. Breakage functions were established as being invariant with respect to such operating variables like ball load, mill speed, particle load, and particle size distribution of the mill. It was also determined that specific selection functions were inherently dependent on the particle size distribution in wet grinding systems. Also, they were consistent with inputs of specific energy, according to grind time. Nonlinearity trends were observed for 1st order specific selection functions which illustrated variations in breakage rates with incremental inputs of grind time and specific energy. A mean particle size called the fulcrum was noted below which the nonlinearities in the breakage trends were observed. This magnitude of the fulcrum value varied with percent solids and slurry filling, indicating

  10. Enhanced hydrogen generation by hydrolysis of Mg doped with flower-like MoS2 for fuel cell applications

    Science.gov (United States)

    Huang, Minghong; Ouyang, Liuzhang; Liu, Jiangwen; Wang, Hui; Shao, Huaiyu; Zhu, Min

    2017-10-01

    In this work, flower-like MoS2 spheres are synthesized via a hydrothermal method and the catalytic activity of the as-prepared and bulk MoS2 on hydrolysis of Mg is systematically investigated for the first time. The Mg-MoS2 composites are prepared by ball milling and the hydrogen generation performances of the composites are investigated in 3.5% NaCl solution. The experimental results suggest that the as-prepared MoS2 exhibits better catalytic effect on hydrolysis of Mg compared to bulk MoS2. In particular, Mg-10 wt% MoS2 (as-prepared) composite milled for 1 h shows the best hydrogen generation properties and releases 90.4% of theoretical hydrogen generation capacity within 1 min at room temperature. The excellent catalytic effect of as-prepared MoS2 may be attributed to the following aspects: three-dimensional flower-like MoS2 architectures improve its dispersibility on Mg particles; make the composite more reactive; hamper the generated Mg(OH)2 from adhering to the surface of Mg; and increase the galvanic corrosion of Mg. In addition, a hydrogen generator based on the hydrolysis reaction of Mg-0.2 wt% MoS2 composite is manufactured and it can supply a maximum hydrogen flow rate of 2.5 L/min. The findings here demonstrate the as-prepared flower-like MoS2 can be a promising catalyst for hydrogen generation from Mg.

  11. Mechanical properties and fracture mechanism of as-cast Mg77TM12Zn5Y6 (TM = Cu, Ni) bulk amorphous matrix composites

    International Nuclear Information System (INIS)

    Qiu, K.Q.; Hu, N.N.; Zhang, H.B.; Jiang, W.H.; Ren, Y.L.; Liaw, P.K.

    2009-01-01

    Comparative investigations on the microstructures, thermal stability and mechanical properties of Mg 77 Cu 12 Zn 5 Y 6 and Mg 77 Ni 12 Zn 5 Y 6 bulk metallic glass matrix composites were carried out by using scanning electron microscopy (SEM), DSC and compressive tester. The results show that the microstructure of as-cast samples with 3 mm in diameter for Cu-containing alloy is consisted of Mg flakes and dotted Mg 2 Cu phase in the amorphous matrix, while the as-cast Ni-containing alloy with the same diameter is mainly consisted of Mg flakes in the amorphous matrix. The glass transition temperature and supercooled liquid region are 413 K and 27 K for the Cu-containing, 443 K and 32 K for the Ni-containing amorphous matrix composites, respectively. The fracture strength, yield strength and plastic strain are 532 MPa, 390 MPa and 2.4% for the Cu-containing alloy, 667 MPa, 412 MPa and 7% for the Ni-containing alloy, respectively. Furthermore, the fracture mechanism for the amorphous matrix composites was discussed according to both the fracture surfaces and the stress-strain curves.

  12. CONDENSED MATTER: STRUCTURE, MECHANICAL AND THERMAL PROPERTIES: Molecular Dynamics Study of Stability of Solid Solutions and Amorphous Phase in the Cu-Al System

    Science.gov (United States)

    Yang, Bin; Lai, Wen-Sheng

    2009-06-01

    The relative stability of fcc and bcc solid solutions and amorphous phase with different compositions in the Cu-Al system is studied by molecular dynamics simulations with n-body potentials. For Cu1-xAlx alloys, the calculations show that the fcc solid solution has the lowest energies in the composition region with x 0.72, while the bee solid solution has the lowest energies in the central composition range, in agreement with the ball-milling experiments that a single bcc solid solution with 0.30 < x < 0.70 is obtained. The evolution of structures in solid solutions and amorphous phase is studied by the coordination number (CN) and bond-length analysis so as to unveil the underlying physics. It is found that the energy sequence among three phases is determined by the competition in energy change originating from the bond length and CNs (or the number of bonds).

  13. Transport properties and exponential n-values of Fe/MgB2 tapes with various MgB2 particle sizes

    International Nuclear Information System (INIS)

    Lezza, P.; Abaecherli, V.; Clayton, N.; Senatore, C.; Uglietti, D.; Suo, H.L.; Fluekiger, R.

    2004-01-01

    Fe/MgB 2 tapes have been prepared starting with pre-reacted binary MgB 2 powders. As shown by resistive and inductive measurements, the reduction of particle size to a few microns by ball milling has little influence on B c2 , while the superconducting properties of the individual MgB 2 grains are essentially unchanged. Reducing the particle size causes an enhancement of B irr from 14 to 16 T, while J c has considerably increased at high fields, its slope J c (B) being reduced. At 4.2 K, values of 5.3 x 10 4 and 1.2 x 10 3 A/cm 2 were measured at 3.5 and 10 T, respectively, suggesting a dominant role of the conditions at the grain interfaces. A systematic variation of these conditions at the interfaces is undertaken in order to determine the limit of transport properties for Fe/MgB 2 tapes. The addition of 5% Mg to MgB 2 powder was found to affect neither J c nor B c2 . For the tapes with the highest J c values, very high exponential n factors were measured: n=148, 89 and 17 at 3.5, 5 and 10 T, respectively and measurements of critical current versus applied strain have been performed. The mechanism leading to high transport critical current densities of filamentary Fe/MgB 2 tapes based on MgB 2 particles is discussed

  14. Dual-tuning effects of In, Al, and Ti on the thermodynamics and kinetics of Mg85In5Al5Ti5 alloy synthesized by plasma milling

    International Nuclear Information System (INIS)

    Cao, Zhijie; Ouyang, Liuzhang; Wu, Yuyu; Wang, Hui; Liu, Jiangwen; Fang, Fang; Sun, Dalin; Zhang, Qingan; Zhu, Min

    2015-01-01

    Highlights: • Mg 85 In 5 Al 5 Ti 5 alloy catalyzed with in-situ formed MgF 2 was prepared by P-milling. • Reaction mechanism of Mg 85 In 5 Al 5 Ti 5 alloy was presented. • Further destabilization of Mg was realized (65.2 kJ/mol H 2 ). • Dual tuning of the thermodynamic and kinetic properties of MgH 2 was realized. - Abstract: The dehydrogenation enthalpy change of MgH 2 by reversibly forming an Mg 0.95 In 0.05 solid solution offers a new method for tuning the thermodynamics of Mg-based alloys. In order to further lower the stability of MgH 2 , Al has been introduced into Mg(In) solid solution. At the same time, to solve the problem of sluggish kinetic properties of Mg–In solid–solution systems and to lower the dehydrogenation activation energy, Ti has also been added. It has been demonstrated that the Mg 85 In 5 Al 5 Ti 5 alloy synthesized by plasma milling (P-milling) shows both enhanced dehydriding thermodynamics and kinetics. This technique could be used to synthesize Mg(In, Al) ternary solid solution incorporating the Ti catalyst in only one step, making it much more efficient than the two-step method. Compared with Mg-based solid solutions, the addition of Ti and in-situ synthesized MgF 2 improved the kinetics and the introduction of In as well as Al imparted enhanced thermodynamics to the Mg 85 In 5 Al 5 Ti 5 system. The dehydrogenation enthalpy change and activation energy were lowered to 65.2 kJ/(mol H 2 ) and 125.2 kJ/mol, respectively, for the Mg 85 In 5 Al 5 Ti 5 alloy

  15. Investigation of nanostructured Al-10 wt.% Zr material prepared by ball milling for high temperature applications

    International Nuclear Information System (INIS)

    Prosviryakov, A.S.; Shcherbachev, K.D.; Tabachkova, N.Yu.

    2017-01-01

    Ground chips of as-cast Al-10 wt.% Zr alloy were subjected to mechanical alloying (MA) with 5 vol.% of nanodiamond addition in a high energy planetary ball-mill. The aim of this work was to investigate the microstructure, phase transformation and mechanical properties of the material both after MA and after subsequent annealing. Optical and transmission electron microscopes were used for morphological and microstructural analysis. The effect of milling time on powder microhardness, Al lattice parameter, lattice microstrain and crystallite size was determined. It was shown that mechanical alloying of as-cast Al-10wt.%Zr alloy during 20 h leads to a complete dissolution of the primary tetragonal Al 3 Zr crystals in aluminum. At the same time, the powder microhardness increases to 370 HV. Metastable cubic Al 3 Zr phase nanoparticles precipitate from the Al solution due to its decomposition after annealing, however, the Al solid solution remains supersaturated and nanocrystalline. Compression tests at room temperature and at 300 °C showed that the strength values of the hot-pressed samples reach 822 MPa and 344 MPa, respectively. - Highlights: •As-cast Al-10 wt.% Zr alloy was mechanically alloyed with 5 vol.% nanodiamond. •The primary tetragonal Al 3 Zr crystals were completely dissolved in Al after 20 h. •Cubic Al 3 Zr phase nanoparticles precipitated from Al solution after aging. •The aged bulk material showed a high strength at room and elevated temperatures.

  16. Investigation of nanostructured Al-10 wt.% Zr material prepared by ball milling for high temperature applications

    Energy Technology Data Exchange (ETDEWEB)

    Prosviryakov, A.S., E-mail: pro.alex@mail.ru; Shcherbachev, K.D.; Tabachkova, N.Yu.

    2017-01-15

    Ground chips of as-cast Al-10 wt.% Zr alloy were subjected to mechanical alloying (MA) with 5 vol.% of nanodiamond addition in a high energy planetary ball-mill. The aim of this work was to investigate the microstructure, phase transformation and mechanical properties of the material both after MA and after subsequent annealing. Optical and transmission electron microscopes were used for morphological and microstructural analysis. The effect of milling time on powder microhardness, Al lattice parameter, lattice microstrain and crystallite size was determined. It was shown that mechanical alloying of as-cast Al-10wt.%Zr alloy during 20 h leads to a complete dissolution of the primary tetragonal Al{sub 3}Zr crystals in aluminum. At the same time, the powder microhardness increases to 370 HV. Metastable cubic Al{sub 3}Zr phase nanoparticles precipitate from the Al solution due to its decomposition after annealing, however, the Al solid solution remains supersaturated and nanocrystalline. Compression tests at room temperature and at 300 °C showed that the strength values of the hot-pressed samples reach 822 MPa and 344 MPa, respectively. - Highlights: •As-cast Al-10 wt.% Zr alloy was mechanically alloyed with 5 vol.% nanodiamond. •The primary tetragonal Al{sub 3}Zr crystals were completely dissolved in Al after 20 h. •Cubic Al{sub 3}Zr phase nanoparticles precipitated from Al solution after aging. •The aged bulk material showed a high strength at room and elevated temperatures.

  17. Structural and hydration properties of amorphous tricalcium silicate

    International Nuclear Information System (INIS)

    Mori, K.; Fukunaga, T.; Shiraishi, Y.; Iwase, K.; Xu, Q.; Oishi, K.; Yatsuyanagi, K.; Yonemura, M.; Itoh, K.; Sugiyama, M.; Ishigaki, T.; Kamiyama, T.; Kawai, M.

    2006-01-01

    Mechanical milling was carried out to synthesize amorphous tricalcium silicate (Ca 3 SiO 5 ) sample, where Ca 3 SiO 5 is the most principal component of Portland cement. The partial phase transformation from the crystalline to the amorphous state was observed by X-ray and neutron diffractions. Moreover, it was found that the structural distortion on the Ca-O correlation exists in the milled Ca 3 SiO 5 . The hydration of the milled Ca 3 SiO 5 with D 2 O proceeds as follows: the formation of hydration products such as Ca(OD) 2 rapidly occurs in the early hydration stage, and then proceeds slowly after about 15 h. The induction time for the hydration of the milled Ca 3 SiO 5 is approximately one half shorter than that for the hydration of the unmilled one. This result means that the mechanical milling brings about the chemical activity of Ca 3 SiO 5 for hydration, and may be particularly useful for increasing the reactivity in the early hydration stage

  18. C, N co-doped TiO_2/TiC_0_._7N_0_._3 composite coatings prepared from TiC_0_._7N_0_._3 powder using ball milling followed by oxidation

    International Nuclear Information System (INIS)

    Hao, Liang; Wang, Zhenwei; Zheng, Yaoqing; Li, Qianqian; Guan, Sujun; Zhao, Qian; Cheng, Lijun; Lu, Yun; Liu, Jizi

    2017-01-01

    Highlights: • TiO_2/TiC_0_._7N_0_._3 coatings were prepared by ball milling followed by oxidation. • In situ co-doping of C and N with simultaneous TiO_2 formation was observed. • Improved photocatalytic activity under UV/visible light was noticed. • Synergism in co-doping and heterojunction formation promoted carrier separation. - Abstract: Ball milling followed by heat oxidation was used to prepared C, N co-doped TiO_2 coatings on the surfaces of Al_2O_3 balls from TiC_0_._7N_0_._3 powder. The as-prepared coatings were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and ultraviolet-visible spectrophotometer (UV–vis). The results show that continuous TiC_0_._7N_0_._3 coatings were formed after ball milling. C, N co-doped TiO_2/TiC_0_._7N_0_._3 composite coatings were prepared after the direct oxidization of TiC_0_._7N_0_._3 coatings in the atmosphere. However, TiO_2 was hardly formed in the surface layer of TiC_0_._7N_0_._3 coatings within a depth less than 10 nm during the heat oxidation of TiC_0_._7N_0_._3 coatings in carbon powder. Meanwhile, the photocatalytic activity evaluation of these coatings was conducted under the irradiation of UV and visible light. All the coatings showed photocatalytic activity in the degradation of MB no matter under the irradiation of UV or visible light. The C, N co-doped TiO_2/TiC_0_._7N_0_._3 composite coatings showed the most excellent performance. The enhancement under visible light irradiation should attribute to the co-doping of carbon and nitrogen, which enhances the absorption of visible light. The improvement of photocatalytic activity under UV irradiation should attribute to the synergistic effect of C, N co-doping, the formation of rutile-anatase mixed phases and the TiO_2/TiC_0_._7N_0_._3 composite microstructure.

  19. Effect of grain size on structural and dielectric properties of barium titanate piezoceramics synthesized by high energy ball milling

    Science.gov (United States)

    Verma, Narendra Kumar; Patel, Sandeep Kumar Singh; Kumar, Dinesh; Singh, Chandra Bhal; Singh, Akhilesh Kumar

    2018-05-01

    We have investigated the effect of sintering temperature on the densification behaviour, grain size, structural and dielectric properties of BaTiO3 ceramics, prepared by high energy ball milling method. The Powder x-ray diffraction reveals the tetragonal structure with space group P4mm for all the samples. The samples were sintered at four different temperatures, (T = 900°C, 1000°C, 1100°C, 1200°C and 1300°C). Density increased with increasing sintering temperature, reaching up to 97% at 1300°C. A grain growth was observed with increasing sintering temperature. Impedance analyses of the sintered samples at various temperatures were performed. Increase in dielectric constant and Curie temperature is observed with increasing sintering temperature.

  20. Precipitation of aluminum and magnesium secondary minerals from uranium mill raffinate (pH 1.0–10.5) and their controls on aqueous contaminants

    International Nuclear Information System (INIS)

    Robertson, Jared; Hendry, M. Jim; Essilfie-Dughan, J.; Chen, J.

    2016-01-01

    Models of geochemical controls on elements of concern (EOCs; e.g., As, Se, Mo, Ni) in U tailings are dominated by ferrihydrite. However, the evolution of aqueous concentrations of Al and Mg through the Key Lake (KL) U mill bulk neutralization process indicates that secondary Al and Mg minerals comprise a large portion of the tailings solids. X-ray diffraction, Al K-edge XAS, and TEM elemental mapping of solid samples collected from a pilot-scale continuous-flow synthetic raffinate neutralization system of the KL mill indicate the secondary Al–Mg minerals present include Mg–Al hydrotalcite, amorphous Al(OH)_3, and an amorphous hydrobasaluminite-type phase. The ferrihydrite present contains Al and may be more accurately described as Al–Fe(OH)_3. In the final combined tailings sample (pH 10.5) collected from the model experiments using raffinate with Al, Mg, and Fe, solid phase EOCs were associated with Al–Fe(OH)_3 and Mg–Al hydrotalcite. In model experiments using raffinate devoid of Fe, aqueous EOC concentrations decreased greatly at pH 4.0 (i.e., where ferrihydrite would precipitate) and largely remained in the solid phase when increased to the terminal pH of 10.5; this suggests Al–Mg minerals can control aqueous concentrations of EOCs in the raffinate in the absence of Fe. Maximum adsorption capacities for individual and mixtures of adsorbates by Mg–Al hydrotalcite were determined. A revised model of the geochemical controls in U mill tailings is presented in which Al and Mg minerals co-exist with Fe minerals to control EOC concentrations. - Highlights: • Simulated a U mill neutralization process to identify Al–Mg secondary mineralogy. • Identified AlOHSO_4, Al–Fe(OH)_3, Al(OH)_3, and Mg–Al hydrotalcite as precipitates. • Aqueous As, Ni, Mo, and Se concentrations controlled by Al–Mg minerals. • Experimental hydrotalcite uptake of As, Mo, and Se was comparable to ferrihydrite. • Updates the current model of aqueous contaminant

  1. Comparison of mechanical and friction properties of composite materials based on AlMg2 containing nano-dimensional particles of crystalline graphite and nanofibers of gamma oxide of aluminum

    Science.gov (United States)

    Aborkin, A. V.; Babin, D. M.; Soboĺkov, A. V.

    2018-04-01

    The method of mechanical synthesis in a planetary ball mill was used for production of composite powders based on the AlMg2 alloy containing 1 wt. % of nanosized particles of crystalline graphite or γ-Al2O3. The resulting powders are consolidated by the sintering under pressure. Using the methods of X-ray diffraction analysis, scanning and transmission electron microscopy, the structural-phase composition of bulk composite materials was studied. Comparative analysis of the microhardness, the conditional yield stress at compression, and the friction coefficient of bulk composite materials is carried out. It has been found out that the mechanical properties of composites reinforced with γ-Al2O3 nanofibers are higher than when reinforcing with nanoscale particles of crystalline graphite.

  2. Comparison of various milling modes combined to the enzymatic hydrolysis of lignocellulosic biomass for bioenergy production: Glucose yield and energy efficiency

    International Nuclear Information System (INIS)

    Licari, A.; Monlau, F.; Solhy, A.; Buche, P.; Barakat, A.

    2016-01-01

    Bagasse is an abundant by-product from sugarcane production that can be used for conversion into biofuels. Nonetheless, the recalcitrant structures of lignocellulosic fibers required a pretreatment prior conversion into biofuels. In this study, four mechanical deconstruction methods were compared in terms of energy demand and energy efficiency at lab scale: BM (ball mill), VBM (vibratory ball mill), CM (centrifugal mill) and JM (jet mill). Results indicate that VBM was more effective compared to BM, JM and CM in enzymatic accessibility and sugars solubilization: VBM-3h > BM-72 h > JM-5000 rpm > CM-0.12 mm. However, preliminary energetic assessment showed that at lab scale, the CM (centrifugal mill) as mechanical fractionation process appears to be the most efficient in terms of energy-efficiency (kg glucose/kWh) compared to BM, VBM and JM. A comparison with literature pretreatments data highlighted that fine and/or ultrafine milling process (BM, VBM, CM) are simpler saccharification technologies, which not required any chemical or water inputs, thus minimizing waste generation and treatment. - Highlights: • VBM (vibro ball milling) was the most effective in decreasing of cellulose crystallinity. • BM (ball milling) was the most effective in increasing surface area. • The highest energy efficiency was obtained with CM (centrifugal milling).

  3. Amorphous silicon based particle detectors

    OpenAIRE

    Wyrsch, N.; Franco, A.; Riesen, Y.; Despeisse, M.; Dunand, S.; Powolny, F.; Jarron, P.; Ballif, C.

    2012-01-01

    Radiation hard monolithic particle sensors can be fabricated by a vertical integration of amorphous silicon particle sensors on top of CMOS readout chip. Two types of such particle sensors are presented here using either thick diodes or microchannel plates. The first type based on amorphous silicon diodes exhibits high spatial resolution due to the short lateral carrier collection. Combination of an amorphous silicon thick diode with microstrip detector geometries permits to achieve micromete...

  4. The development of cobalt-base alloy ball bearing

    International Nuclear Information System (INIS)

    Yu Xinshui; Chen Jianting; Wang Zaishu; Wang Ximei; Huang Chongming.

    1986-01-01

    The main technologies and experiences in developing a Cobalt-base alloy ball bearing are described. In the hardfacing of bearing races, a lower-hardness alloy of type St-6 is used rather than an alloy with hardness similar to that of the ball and finally the hardness of race is increased to match that of the ball by heat treatment. This improvement has certain advantages. The experience of whole developing technology indicates that strict control of the technology in the bearing-race hardfacing is the key problem in the quality assurance of bearings

  5. Effect of carbons (G and CFs), TM (Ni, Fe and Al) and oxides (Nb_2O_5 and V_2O_5) on hydrogen generation from ball milled Mg-based hydrolysis reaction for fuel cell

    International Nuclear Information System (INIS)

    Awad, A.S.; El-Asmar, E.; Tayeh, T.; Mauvy, F.; Nakhl, M.; Zakhour, M.; Bobet, J.-L.

    2016-01-01

    This paper dedicated to investigation the effect of carbons (graphite and carbon fibers), transition metals (TM = Ni, Fe and Al) and oxides (Nb_2O_5 and V_2O_5) on Mg–H hydrolysis reaction in aqueous media (3.5 wt% NaCl). Mg – 10 wt% X (X = C, TM and oxides) mixtures were prepared by mechanical milling (1, 3 and 5 h). Mg – 10 wt% G mixtures show the best hydrolysis performance (95% of theoretical hydrogen generation yield in almost 3 min) in comparison to Mg – oxide and Mg – TM mixtures. In addition to the presence of micro-galvanic cells, particle size, MgH_2 content, density defects, fractures and cracking have an important influence on the hydrolysis reaction. Synergetic effect of carbons and transition metals has been studied for Mg – 5 wt% G – 5 wt% Ni mixture. Activation energies were calculated using Avrami–Erofeev model. An activation energy of 14.34 kJ/mol was found for Mg/G/Ni mixture which demonstrates the best hydrolysis behavior (95% of theoretical hydrogen generation yield within 2 min). Hydrogen generated from Mg–H hydrolysis reaction was fed directly to a single Proton Exchange Membrane Fuel Cell (PEMFC). At 0.15 A, the cell voltage exhibited a stable value of approximately 0.52 V for roughly 35 min. - Highlights: • The presence of carbon and transition metals enhance the hydrolysis reaction of magnesium. • The synergetic effect of graphite and Ni leads to the best hydrolysis kinetics. • Cl"− ions replace OH"− ions to destabilize the Mg(OH)_2 passivation layer. • Production of electricity is feasible from hydrogen generated from Mg.

  6. Solid solution and amorphous phase in Ti–Nb–Ta–Mn systems synthesized by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Aguilar, C., E-mail: claudio.aguilar@usm.cl [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Guzman, P. [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Lascano, S. [Departamento de Ingeniería Mecánica, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Parra, C. [Departamento de Física, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Bejar, L. [Instituto de Investigaciones Metalúrgicas, Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, Morelia C.P. 58000, Michoacán (Mexico); Medina, A. [Facultad de Ingeniería Mecánica, Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, C.P. 58000, Michoacán (Mexico); Guzman, D. [Departamento de Metalurgia, Universidad de Atacama, Av. España 485, Copiapó (Chile)

    2016-06-15

    This work discusses the formation of Ti–30Nb–13Ta–xMn (x: 2, 4 and 6 wt%) solid solution by mechanical alloying using a shaker mill. A solid solution was formed after 15 h of milling and an amorphous phase was formed after 30 h of milling, according to X-ray diffraction results. Disappearance of strongest X-ray diffraction peaks of Nb, Ta and Mn indicated the formation of solid solution, while, X-ray diffraction patterns of powders milled for 30 h showed an amorphous hump with crystalline peaks in the angular range of 35–45° in 2θ. TEM image analysis showed the presence of nanocrystalline intermetallic compounds embedded in an amorphous matrix. Mn{sub 2}Ti, MnTi and NbTi{sub 4} intermetallic compounds were detected and revealed crystallites with size ranging from 3 to 20 nm. The Gibbs free energy for the formation of solid solution and amorphous phase of three ternary systems (Ti–Nb–Ta, Ti–Nb–Mn and Ti–Ta–Mn) was calculated using extended Miedema's model. Experimental and thermodynamic data confirmed that solid solution was first formed in the alloy with 6wt% Mn followed by the formation of an amorphous phase as milling time increases. The presence of Mn promoted the formation of amorphous phase because the atomic radius difference between Mn with Ti, Nb and Ta. - Highlights: • Thermodynamics analysis of extension of solid solution of the Ti–Nb–Ta–Mn system. • Formation of amorphous phase and intermetallic compounds were observed. • Nanocrystalline intermetallic compounds were formed with the sizes between 3 and 20 nm.

  7. Use of high energy ball milling to study the role of graphene nanoplatelets and carbon nanotubes reinforced magnesium alloy

    Energy Technology Data Exchange (ETDEWEB)

    Rashad, Muhammad, E-mail: rashadphy87@gmail.com [College of Materials Science and Engineering, Chongqing University, Chongqing 400044 (China); National Engineering Research Center for Magnesium Alloys, Chongqing University, Chongqing 400044 (China); Pan, Fusheng, E-mail: fspan@cqu.edu.cn [College of Materials Science and Engineering, Chongqing University, Chongqing 400044 (China); National Engineering Research Center for Magnesium Alloys, Chongqing University, Chongqing 400044 (China); Chongqing Academy of Science and Technology, Chongqing, Chongqing 401123 (China); Zhang, Jianyue [College of Materials Science and Engineering, Chongqing University, Chongqing 400044 (China); National Engineering Research Center for Magnesium Alloys, Chongqing University, Chongqing 400044 (China); Asif, Muhammad [School of Materials Science and Engineering, Dalian University of Technology, Dalian 116024 (China)

    2015-10-15

    Graphene nanoplatelets (few layer graphene) and carbon nanotubes were used as reinforcement fillers to enhance the mechanical properties of AZ31 magnesium alloy through high energy ball milling, sintering, and hot extrusion techniques. Experimental results revealed that tensile fracture strain of AZ31 magnesium alloy was enhanced by +49.6% with 0.3 wt.% graphene nanoplatelets compared to −8.3% regression for 0.3 wt.% carbon nanotubes. The tensile strength of AZ31 magnesium alloy was decreased (−11.2%) with graphene nanoplatelets addition, while increased (+7.7%) with carbon nanotubes addition. Unlike tensile test, compression tests showed different trend. The compression strength of carbon nanotubes-AZ31 composite was +51.2% greater than AZ31 magnesium alloy as compared to +0.6% increase for graphene nanoplatelets. The compressive fracture strain of carbon nanotubes-AZ31 composite was decreased (−14.1%) while no significant change in fracture strain of graphene nanoplatelets-AZ31 composite was observed. The X-ray diffraction results revealed that addition of reinforcement particles weaken the basal textures which affect the composite's yield asymmetry. Microstructure evaluation revealed the absence of intermetallic phase formation between reinforcements and matrix. The carbon reinforcements in AZ31 magnesium alloy dissolve and isolate β phases throughout the matrix. The increased fracture strain and mechanical strength of graphene nanoplatelets and carbon nanotubes-AZ31 composites are attributed to large specific surface area of graphene nanoplatelets and stiffer nature of carbon nanotubes respectively. - Highlights: • Powder metallurgy method was used to fabricate magnesium composites. • The AZ31-carbon materials composite were blended using ball milling. • The reinforcement particles weaken the basal texture which affects yield asymmetry of composites. • AZ31-graphene nanoplatelets composite exhibited impressive increase in tensile elongation

  8. Use of high energy ball milling to study the role of graphene nanoplatelets and carbon nanotubes reinforced magnesium alloy

    International Nuclear Information System (INIS)

    Rashad, Muhammad; Pan, Fusheng; Zhang, Jianyue; Asif, Muhammad

    2015-01-01

    Graphene nanoplatelets (few layer graphene) and carbon nanotubes were used as reinforcement fillers to enhance the mechanical properties of AZ31 magnesium alloy through high energy ball milling, sintering, and hot extrusion techniques. Experimental results revealed that tensile fracture strain of AZ31 magnesium alloy was enhanced by +49.6% with 0.3 wt.% graphene nanoplatelets compared to −8.3% regression for 0.3 wt.% carbon nanotubes. The tensile strength of AZ31 magnesium alloy was decreased (−11.2%) with graphene nanoplatelets addition, while increased (+7.7%) with carbon nanotubes addition. Unlike tensile test, compression tests showed different trend. The compression strength of carbon nanotubes-AZ31 composite was +51.2% greater than AZ31 magnesium alloy as compared to +0.6% increase for graphene nanoplatelets. The compressive fracture strain of carbon nanotubes-AZ31 composite was decreased (−14.1%) while no significant change in fracture strain of graphene nanoplatelets-AZ31 composite was observed. The X-ray diffraction results revealed that addition of reinforcement particles weaken the basal textures which affect the composite's yield asymmetry. Microstructure evaluation revealed the absence of intermetallic phase formation between reinforcements and matrix. The carbon reinforcements in AZ31 magnesium alloy dissolve and isolate β phases throughout the matrix. The increased fracture strain and mechanical strength of graphene nanoplatelets and carbon nanotubes-AZ31 composites are attributed to large specific surface area of graphene nanoplatelets and stiffer nature of carbon nanotubes respectively. - Highlights: • Powder metallurgy method was used to fabricate magnesium composites. • The AZ31-carbon materials composite were blended using ball milling. • The reinforcement particles weaken the basal texture which affects yield asymmetry of composites. • AZ31-graphene nanoplatelets composite exhibited impressive increase in tensile elongation

  9. Rock Characteristics and Ball Mill Energy Requirements at ...

    African Journals Online (AJOL)

    These changes can have great impact on milling operations. ... Goldfields Ghana Limited, Tarkwa Gold Mine (TGM), processes ores which occur in ... The parameters examined had deviated from the design; Work Index (WI) for example was ...

  10. Effects of surfactant addition and high-speed ball milling on magnetic powders based on Pr-Fe-B obtained by HDDR

    International Nuclear Information System (INIS)

    Santos, Patricia Brissi

    2011-01-01

    This work verified the effect caused by adding the surfactant in the high speed/energy milling in order to obtain Pr 12 Fe 65.9 Co 16 B 6 Nb 0.1 magnetic nano powders. The first part of this work involved the magnetic powder obtainment through the process of hydrogenation, disproportionation, desorption and recombination (HDDR). The pressure of H2 during the hydrogenation and disproportion steps was 930 mbar and the temperature of desorption and recombination was 840 deg C. Initially, the HDDR powders were subjected a high speed milling process at 900 rpm, with quantity variations of the milling medium (cyclohexane) and without the addition of oleic acid. Then, the HDDR powders were subjected to the milling process with the addition of oleic acid and with milling time variations. After the milling process, heat treatments of the powder were carried out at 700 deg C or 800 deg C for 30 minutes in order to obtain the crystallization of the powder. By performing the procedures, it was verified that the milling efficiency improved with the addition of 6.6 ml of cyclohexane as the milling medium and with the addition of oleic acid. It was determined that for the surfactant additions of 0.02 ml to 0.05 ml, with a milling time of up to 360 minutes, powder agglomeration does not occur in the milling pot and the milling efficiency is higher than 90%. The second stage of this work involved the magnetic powder's characterization obtained by using vibrating sample magnetometer, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. Through the characterizations it was found that the powder's magnetic properties improved when the addition of oleic acid in a high-speed /energy milling occurred. It was also verified that the α-Fe phase, present in the powder, shows a crystallite size decrease (from 35 nm to ∼ 10 nm) when the time milling variation occurred; meanwhile, the crystallinity degree was lower in the Pr 2 Fe 14 B phase when the time

  11. Nanostructured Layered Cathode for Rechargeable Mg-Ion Batteries.

    Science.gov (United States)

    Tepavcevic, Sanja; Liu, Yuzi; Zhou, Dehua; Lai, Barry; Maser, Jorg; Zuo, Xiaobing; Chan, Henry; Král, Petr; Johnson, Christopher S; Stamenkovic, Vojislav; Markovic, Nenad M; Rajh, Tijana

    2015-08-25

    Nanostructured bilayered V2O5 was electrochemically deposited within a carbon nanofoam conductive support. As-prepared electrochemically synthesized bilayered V2O5 incorporates structural water and hydroxyl groups, which effectively stabilizes the interlayers and provides coordinative preference to the Mg(2+) cation in reversible cycling. This open-framework electrode shows reversible intercalation/deintercalation of Mg(2+) ions in common electrolytes such as acetonitrile. Using a scanning transmission electron microscope we demonstrate that Mg(2+) ions can be effectively intercalated into the interlayer spacing of nanostructured V2O5, enabling electrochemical magnesiation against a Mg anode with a specific capacity of 240 mAh/g. We employ HRTEM and X-ray fluorescence (XRF) imaging to understand the role of environment in the intercalation processes. A rebuilt full cell was tested by employing a high-energy ball-milled Sn alloy anode in acetonitrile with Mg(ClO4)2 salt. XRF microscopy reveals effective insertion of Mg ions throughout the V2O5 structure during discharge and removal of Mg ions during electrode charging, in agreement with the electrode capacity. We show using XANES and XRF microscopy that reversible Mg intercalation is limited by the anode capacity.

  12. Structural evolution and formation mechanisms of TiC/Ti nanocomposites prepared by high-energy mechanical alloying

    International Nuclear Information System (INIS)

    Gu Dongdong; Meiners, Wilhelm; Hagedorn, Yves-christian; Wissenbach, Konrad; Poprawe, Reinhart

    2010-01-01

    In this work, high-energy ball milling of a micrometre-scaled Ti and TiC powder mixture was performed to prepare TiC/Ti nanocomposites. The constituent phases and microstructural characteristics of the milled powders were studied by an x-ray diffractometer, a scanning electron microscope, an energy dispersive x-ray spectroscope and a transmission electron microscope. Formation mechanisms and theoretical basis of the microstructural development were elucidated. It showed that on increasing the applied milling time, the structures of the Ti constituent experienced a successive change from hcp (5 h) to fcc (10 h) and finally to an amorphous state (≥15 h). The hydrostatic stresses caused by the excess free volume at grain boundaries were calculated to be 3.96 and 5.59 GPa for the Ti constituent in 5 and 10 h milled powders, which was responsible for the hcp to fcc polymorphic change. The amorphization of Ti constituent was due to the large defect concentration induced by severe plastic deformation during milling. The milled powder particles underwent two stages of significant refinement at 10 and 20 h during milling. For a higher milling time above 25 h, powder characteristics and chemical compositions became stable. The competitive action and the final equilibrium between the mechanisms of fracturing and cold welding accounted for the microstructural evolution. The ball milled products were typically nanocomposite powders featured by a nanocrystalline/amorphous Ti matrix reinforced with uniformly dispersed TiC nanoparticles. The finest crystalline sizes of the Ti and TiC constituents were 17.2 nm (after 10 h milling) and 13.5 nm (after 20 h milling), respectively.

  13. Effect of mechanical milling on barium titanate (BaTiO3) perovskite

    Science.gov (United States)

    Singh, Rajan Kumar; Sanodia, Sagar; Jain, Neha; Kumar, Ranveer

    2018-05-01

    Commercial Barium Titanate BaTiO3 (BT) is milled by planetary ball mill in acetone medium using stainless steel bowl & ball for different hours. BT is an important perovskite oxide with structure ABO3. BT has applications in electro-optic devices, energy storing devices such as photovoltaic cells, thermistors, multiceramic capacitors & DRAMs etc. BT is non-toxic & environment friendly ceramic with high dielectric and piezoelectric property so it can be used as the substitute of PZT & PbTiO3. Here, we have investigated the effect of milling time and temperature on particle size and phase transition of BT powder. We used use Raman spectroscopy for studying the spectra of BT; XRD is used for structural study. Intensity (height) of Raman spectra and XRD spectra continuously decrease with increasing the milling hours and width if these spectra increases which indicates, decrease in BT size.

  14. Microstructural characterization of Mg-based bulk metallic glass and nanocomposite

    Energy Technology Data Exchange (ETDEWEB)

    Babilas, Rafał, E-mail: rafal.babilas@polsl.pl [Institute of Engineering Materials and Biomaterials, Silesian University of Technology, Konarskiego 18a St., 44-100 Gliwice (Poland); Nowosielski, Ryszard; Pawlyta, Mirosława [Institute of Engineering Materials and Biomaterials, Silesian University of Technology, Konarskiego 18a St., 44-100 Gliwice (Poland); Fitch, Andy [European Synchrotron Radiation Facility, CS40220, 38043 Grenoble (France); Burian, Andrzej [A. Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4 St., 40-007 Katowice (Poland)

    2015-04-15

    New magnesium-based bulk metallic glasses Mg{sub 60}Cu{sub 30}Y{sub 10} have been prepared by pressure casting. Glassy alloys were successfully annealed to become nanocomposite containing 200 nm crystallites in an amorphous matrix. The microstructure of bulk glassy alloy and nanocomposite obtained during heat treatment was examined by X-ray diffraction and scanning and high-resolution electron microscopy. Metallic glass has been also studied to explain the structural characteristics by the reverse Monte Carlo (RMC) modeling based on the diffraction data. The HRTEM images allow to indicate some medium-range order (MRO) regions about 2–3 nm in size and formation of local atomic clusters. The RMC modeling results confirmed some kinds of short range order (SRO) structures. It was found that the structure of bulk metallic glass formed by the pressure casting is homogeneous. The composite material contained very small particles in the amorphous matrix. Homogeneous glassy alloy had better corrosion resistance than a composite containing nanocrystalline particles in a glassy matrix. - Highlights: • RMC modeling demonstrates some kinds of SRO structures in Mg-based BMGs. • HRTEM indicated MRO regions about 2–3 nm and SRO regions about 0.5 nm in size. • Mg-based glassy alloys were successfully annealed to become nanocomposite material. • Crystalline particles have spherical morphology with an average diameter of 200 nm. • Glassy alloy had higher corrosion resistance than a nanocomposite sample.

  15. Indications of the formation of an oversaturated solid solution during hydrogenation of Mg-Ni based nanocomposite produced by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Guzman, D. [Departamento de Ingenieria en Metalurgia, Facultad de Ingenieria, Universidad de Atacama y Centro Regional de Investigacion y Desarrollo Sustentable de Atacama, CRIDESAT, Av. Copayapu 485, Copiapo (Chile); Ordonez, S. [Departamento de Ingenieria Metalurgica, Facultad de Ingenieria, Universidad de Santiago de Chile, Av. Lib. Bernardo O' Higgins 3363, Santiago (Chile); Fernandez, J.F.; Sanchez, C. [Departamento de Fisica de Materiales, Facultad de Ciencias, Universidad Autonoma de Madrid, Cantoblanco 28049, Madrid (Spain); Serafini, D. [Departamento de Fisica, Facultad de Ciencias, Universidad de Santiago de Chile and Center for Interdisciplinary Research in Materials, CIMAT, Av. Lib. Bernardo O' Higgins 3363, Santiago (Chile); Rojas, P.A. [Escuela de Ingenieria Mecanica, Facultad de Ingenieria, Av. Los Carrera 01567, Quilpue, Pontificia Universidad Catolica de Valparaiso, PUCV (Chile); Aguilar, C. [Instituto de Materiales y Procesos Termomecanicos, Facultad de Ciencias de la Ingenieria, Universidad Austral de Chile, Av. General Lagos 2086, Valdivia (Chile)

    2009-07-15

    An oversaturated solid solution of H in a nanocomposite material formed mainly by nanocrystalline Mg{sub 2}Ni, some residual nanocrystalline Ni and an Mg rich amorphous phase has been found for the first time. The nanocomposite was produced by mechanical alloying starting from Mg and Ni elemental powders, using a SPEX 8000D mill. The hydriding characterization of the nanocomposite was carried out by solid-gas reaction method in a Sievert's type apparatus. The maximum hydrogen content reached in a period of 21 Ks without prior activation was 2.00 wt.% H under hydrogen pressure of 2 MPa at 363 K. The X-ray diffraction analysis showed the presence of an oversaturated solid solution between nanocrystalline Mg{sub 2}Ni and H without any sign of Mg{sub 2}NiH{sub 4} hydride formation. The dehydriding behaviour was studied by differential scanning calorimetry and thermogravimetry. The results showed the existence of two desorption peaks, the first one associated with the transformation of the oversaturated solid solution into Mg{sub 2}NiH{sub 4}, and the second one with the Mg{sub 2}NiH{sub 4} desorption. (author)

  16. Micro-scale prediction method for API-solubility in polymeric matrices and process model for forming amorphous solid dispersion by hot-melt extrusion.

    Science.gov (United States)

    Bochmann, Esther S; Neumann, Dirk; Gryczke, Andreas; Wagner, Karl G

    2016-10-01

    A new predictive micro-scale solubility and process model for amorphous solid dispersions (ASDs) by hot-melt extrusion (HME) is presented. It is based on DSC measurements consisting of an annealing step and a subsequent analysis of the glass transition temperature (Tg). The application of a complex mathematical model (BCKV-equation) to describe the dependency of Tg on the active pharmaceutical ingredient (API)/polymer ratio, enables the prediction of API solubility at ambient conditions (25°C). Furthermore, estimation of the minimal processing temperature for forming ASDs during HME trials could be defined and was additionally confirmed by X-ray powder diffraction data. The suitability of the DSC method was confirmed with melt rheological trials (small amplitude oscillatory system). As an example, ball milled physical mixtures of dipyridamole, indomethacin, itraconazole and nifedipine in poly(vinylpyrrolidone-co-vinylacetate) (copovidone) and polyvinyl caprolactam-polyvinyl acetate-polyethylene glycol graft copolymer (Soluplus®) were used. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Influence of milling process on efavirenz solubility

    Directory of Open Access Journals (Sweden)

    Erizal Zaini

    2017-01-01

    Full Text Available Introduction: The aim of this study was to investigate the influence of the milling process on the solubility of efavirenz. Materials and Methods: Milling process was done using Nanomilling for 30, 60, and 180 min. Intact and milled efavirenz were characterized by powder X-ray diffraction, scanning electron microscopy (SEM, spectroscopy infrared (IR, differential scanning calorimetry (DSC, and solubility test. Results: The X-ray diffractogram showed a decline on peak intensity of milled efavirenz compared to intact efavirenz. The SEM graph depicted the change from crystalline to amorphous habit after milling process. The IR spectrum showed there was no difference between intact and milled efavirenz. Thermal analysis which performed by DSC showed a reduction on endothermic peak after milling process which related to decreasing of crystallinity. Solubility test of intact and milled efavirenz was conducted in distilled water free CO2with 0.25% sodium lauryl sulfate media and measured using high-performance liquid chromatography method with acetonitrile: distilled water (80:20 as mobile phases. The solubility was significantly increased (P < 0.05 after milling processes, which the intact efavirenz was 27.12 ± 2.05, while the milled efavirenz for 30, 60, and 180 min were 75.53 ± 1.59, 82.34 ± 1.23, and 104.75 ± 0.96 μg/mL, respectively. Conclusions: Based on the results, the solubility of efavirenz improved after milling process.

  18. Bulk amorphous alloys: Preparation and properties of (Mg0.98Al0.02)x(Cu0.75Y0.25)100

    DEFF Research Database (Denmark)

    Eldrup, Morten Mostgaard; Pedersen, Allan Schrøder; Ohnuma, M.

    2000-01-01

    New bulk amorphous quaternary alloys of the composition (Mg1-xAlx)(60)Cu30Y10 (x = 0 - 0.17) were recently reported by the authors and preliminary results of the influence of Al content on the ability to form a bulk amorphous phase were presented. In the present note we extend this work to look...... for the influence of the Mg-Al content on the glass forming ability by studying a range of compositions, (Mg0.98Al0.02)(x)(Cu0.75Y0.25)(100-x) for x = 60 - 80 at.%. As previously, the alloys were prepared by a relatively simple technique, i.e. rapid cooling of the melt in a wedge-shaped copper mould. This method...... provides a range of cooling rates within a single ingot during the solidification that link the slowly and rapidly cooled microstructure for each alloy composition. Hence, the maximum thickness of the amorphous part of the cast material will be a measure of the glass forming ability (GFA) of the particular...

  19. Ab initio molecular dynamics simulation of the liquid and amorphous structure of Mg65Cu25Gd10 alloy

    International Nuclear Information System (INIS)

    Gao, R.; Zhao, Y.F.; Liu, X.J.; Liu, Z.K.; Hui, X.

    2013-01-01

    The liquid and amorphous structures of Mg 65 Cu 25 Gd 10 alloy were studied by using molecular dynamics methods within the frame of density functional theory. The generalized and partial pair correlation functions, structure factors, coordination numbers and bond pairs for this alloy were analyzed. It is shown that this alloy exhibit typical characterization of liquid structure at the temperature higher than 750 K, and of amorphous structure with shoulders on the second diffuse peaks of the pair correlation functions curves at room temperature. The local short and medium range ordering tends to be increased with the decrease of temperature. Both the liquid and the amorphous structures are mainly composed of icosahedral type of bond pairs. Perfect and distorted icosahedra can be differentiated from the atomic configuration of the amorphous alloy

  20. Texture formation in iron particles using mechanical milling with graphite as a milling aid

    Energy Technology Data Exchange (ETDEWEB)

    Motozuka, S.; Hayashi, K. [Department of Mechanical Engineering, Gifu National College of Technology, 2236-2 Kamimakuwa, Motosu, Gifu 501-0495 (Japan); Tagaya, M. [Department of Materials Science and Technology, Nagaoka University of Technology, 1603-1 Kamitomioka, Nagaoka, Niigata 940-2188 (Japan); Morinaga, M. [Toyota Physical and Chemical Research Institute, 41-1, Yokomichi, Nagakute, Aichi 480-1192 (Japan)

    2015-09-15

    Crystallographically anisotropic platelet iron particles were successfully prepared using a conventional ball mill with addition of graphite (Gp) particles. The morphological and structural changes resulting from the milling were investigated using scanning electron microscopy and X-ray diffraction. The spherical iron particles were plastically deformed into platelet shapes during the milling. Simultaneously, it is suggested that the size of the Gp particles decreased and adhered as nanoparticles on the surface of the iron particles. The adhered Gp particles affected the plastic deformation behavior of the iron particles: the (001) planes of α-iron were oriented parallel to the particle face, and no preferred in-plane orientation was observed. This study not only details the preparation of soft magnetic metal particles that crystallographically oriented to enhance their magnetic properties but also provides new insight into the activities of the well-established and extensively studied mechanical milling method.

  1. Texture formation in iron particles using mechanical milling with graphite as a milling aid

    International Nuclear Information System (INIS)

    Motozuka, S.; Hayashi, K.; Tagaya, M.; Morinaga, M.

    2015-01-01

    Crystallographically anisotropic platelet iron particles were successfully prepared using a conventional ball mill with addition of graphite (Gp) particles. The morphological and structural changes resulting from the milling were investigated using scanning electron microscopy and X-ray diffraction. The spherical iron particles were plastically deformed into platelet shapes during the milling. Simultaneously, it is suggested that the size of the Gp particles decreased and adhered as nanoparticles on the surface of the iron particles. The adhered Gp particles affected the plastic deformation behavior of the iron particles: the (001) planes of α-iron were oriented parallel to the particle face, and no preferred in-plane orientation was observed. This study not only details the preparation of soft magnetic metal particles that crystallographically oriented to enhance their magnetic properties but also provides new insight into the activities of the well-established and extensively studied mechanical milling method

  2. Fabrication of Fe1.1Se0.5Te0.5 bulk by a high energy ball milling technique

    Science.gov (United States)

    Liu, Jixing; Li, Chengshan; Zhang, Shengnan; Feng, Jianqing; Zhang, Pingxiang; Zhou, Lian

    2017-11-01

    Fe1.1Se0.5Te0.5 superconducting bulks were successfully synthesized by a high energy ball milling (HEBM) aided sintering technique. Two advantages of this new technique have been revealed compared with traditional solid state sintering method. One is greatly increased the density of sintered bulks. It is because the precursor powders with β-Fe(Se, Te) and δ-Fe(Se, Te) were obtained directly by the HEBM process and without formation of liquid Se (and Te), which could avoid the huge volume expansion. The other is the obvious decrease of sintering temperature and dwell time due to the effective shortened length of diffusion paths. The superconducting critical temperature Tc of 14.2 K in our sample is comparable with those in previous reports, and further optimization of chemical composition is on the way.

  3. Synthesis of Zn(BH{sub 4}){sub 2} and Gas Absorption and Release Characteristics of Zn(BH{sub 4}){sub 2}, Ni, or Ti-Added MgH{sub 2}–Based Alloys

    Energy Technology Data Exchange (ETDEWEB)

    Kwak, Young Jun; Lee, Seong Ho; Kwon, Sung Nam; Park Il Woo; Song, Myoung Youp [Chonbuk National University, Jeonju (Korea, Republic of)

    2015-07-15

    A sample [named Zn(BH{sub 4}){sub 2}(+NaCl)] was synthesized by milling ZnCl{sub 2} and NaBH{sub 4} at 400 rpm under argon gas for 2 h. And Zn(BH{sub 4}){sub 2}(+NaCl)+MgH{sub 2} sample was prepared by milling MgH{sub 2} in a planetary ball mill and mixing with the Zn(BH{sub 4}){sub 2}(+NaCl) synthesized by milling for 4 h in a mortar with a pestle. Then the gas-release characteristics of the two samples were investrigated. Analyses of XRD patterns and FT-IR spectra, as well as TGA, DTA, and SEM observations, were also performed. After heating the samples to 400 ℃, the weight losses of Zn(BH{sub 4}){sub 2}(+NaCl) and Zn(BH{sub 4}){sub 2}(+NaCl)+MgH{sub 2} were 11.2 and 8.2 wt%, respectively, with respect to the sample weight. The DTA results for the two samples showed a decomposition peak for Zn(BH{sub 4}){sub 2} at about 61 ℃. The DTA result of Zn(BH{sub 4}){sub 2}(+NaCl) + MgH{sub 2} showed a decomposition peak for MgH{sub 2} at about 374 ℃. A sample of Zn(BH{sub 4}){sub 2}(+NaCl)+MgH{sub 2} to which Ni, and Ti were added, with a composition of 90 wt% MgH{sub 2}-5 wt% Zn(BH{sub 4}){sub 2}(+NaCl)-2.5 wt% Ni-2.5 wt% Ti, in which a large amount of MgH2 is contained in order to make a large quantity of hydrogen be absorbed and released reversibly, was also prepared. The experimental results showed that addition of Zn(BH{sub 4}){sub 2}(+NaCl), Ni, or Ti increased the dehydriding rate of MgH{sub 2}, while decreased its initial hydriding rate.

  4. Structural and magnetic properties of Fe60Al40 alloys prepared by means of a magnetic mill

    International Nuclear Information System (INIS)

    Bernal-Correa, R.; Rosales-Rivera, A.; Pineda-Gomez, P.; Salazar, N.A.

    2010-01-01

    A study on synthesis, structural and magnetic characterization of Fe 60 Al 40 (at.%) alloys prepared by means of mechanical alloying process is presented. The mechanical alloying was performed using a milling device with magnetically controlled ball movement (Uni-Ball-Mill 5 equipment) at several milling times. The characterization was carried out via X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The effects of milling time on the structural state, morphological evolution and magnetic behaviour of the Fe 60 Al 40 (at.%) alloys are discussed. Besides, in this current study we emphasize the result that indicating a ferro-para-ferromagnetic transition from a correlation between X-ray diffraction and magnetization data.

  5. The influence of mineralogical, chemical and physical properties on grindability of commercial clinkers with high MgO level

    International Nuclear Information System (INIS)

    Souza, Vladia Cristina G. de; Koppe, Jair Carlos; Costa, Joao F.C.L.; Vargas, Andre Luis Marin; Blando, Eduardo; Huebler, Roberto

    2008-01-01

    This research investigates various methods able to identify possible mineralogical, physical and chemical influences on the grindability of commercial clinkers with high MgO level. The aim of the study is to evaluate the hardness and elastic modulus of the clinker mineral phases and their fracture strength during the comminution processes, comparing samples from clinkers with low MgO level (0.5%) and clinkers with elevated MgO levels (> 5.0%). The study of the influence of mineralogical, chemical and physical properties was carried out using several analytical techniques, such as: optical microscopy, X-ray diffraction with Rietveld refinement (XRD) and X-ray fluorescence (XRF). These techniques were useful in qualifying the different clinker samples. The drop weight test (DWT) and the Bond ball mill grindability test were performed to characterize the mechanical properties of clinkers. Nanoindentation tests were also carried out. Results from the Bond ball mill grindability test were found to be related to the hardness of the mineral phase and to mineralogical characteristics, such as type and amount of inclusions in silicates, belite and alite crystals shape, or microcracked alites. In contrast, the results obtained by the DWT were associated to the macro characteristics of clinkers, such as porosity, as well as to the hardness and mineralogical characteristics of belite crystals in clusters. Hardness instrumented tests helped to determine the Vickers hardness and elastic modulus from the mineral phases in commercial clinkers and produced different values for the pure phases compared to previous publications

  6. In situ Fabrication of Fe-TiB{sub 2} Nanocomposite Powder by Planetary Ball Milling and Subsequent Heat-treatment of FeB and TiH{sub 2} Powder Mixture

    Energy Technology Data Exchange (ETDEWEB)

    Huynh, Xuan-Khoa [Hanoi Uneversity of Science and Technology, Hanoi (Viet Nam); Bae, Sun-Woo; Kim, Ji Soon [University of Ulsan, Ulsan (Korea, Republic of)

    2017-01-15

    Fe-TiB{sub 2} powder was synthesized in-situ by the planetary ball milling and subsequent heat-treatment of an iron boride (FeB) and titanium hydride (TiH{sub 2}) powder mixture. Mechanical activation of the (FeB+TiH{sub 2}) powder mixtures was observed after a milling time of 3 hours at 700 rpm of rotation speed, but activation was not the same after 1 hour milling time. The particle size of the (FeB+ TiH{sub 2}) powder mixture was reduced to the nanometer scale, and each constituent was homogeneously distributed. A sharp exothermic peak was observed at a lower temperature (749 ℃) on the DSC curves for the (FeB+TiH{sub 2}) powder mixture milled for 3 hours, compared to the one milled for 1 hour (774 ℃). These peaks were confirmed to have resulted from the formation reaction of the TiB{sub 2} phase, from Ti and B elements in the FeB. The Fe-TiB{sub 2} composite powder fabricated in situ exhibited only two phases of Fe and TiB{sub 2} with homogeneous distribution. The size of the TiB{sub 2} particulates in the Fe matrix was less than 5 nm.

  7. Processing of Polysulfone to Free Flowing Powder by Mechanical Milling and Spray Drying Techniques for Use in Selective Laser Sintering

    Directory of Open Access Journals (Sweden)

    Nicolas Mys

    2016-04-01

    Full Text Available Polysulfone (PSU has been processed into powder form by ball milling, rotor milling, and spray drying technique in an attempt to produce new materials for Selective Laser Sintering purposes. Both rotor milling and spray drying were adept to make spherical particles that can be used for this aim. Processing PSU pellets by rotor milling in a three-step process resulted in particles of 51.8 μm mean diameter, whereas spray drying could only manage a mean diameter of 26.1 μm. The resulting powders were characterized using Differential Scanning Calorimetry (DSC, Gel Permeation Chromatography (GPC and X-ray Diffraction measurements (XRD. DSC measurements revealed an influence of all processing techniques on the thermal behavior of the material. Glass transitions remained unaffected by spray drying and rotor milling, yet a clear shift was observed for ball milling, along with a large endothermic peak in the high temperature region. This was ascribed to the imparting of an orientation into the polymer chains due to the processing method and was confirmed by XRD measurements. Of all processed powder samples, the ball milled sample was unable to dissolve for GPC measurements, suggesting degradation by chain scission and subsequent crosslinking. Spray drying and rotor milling did not cause significant degradation.

  8. PAC study in the HfO2-SiO2 system

    International Nuclear Information System (INIS)

    Chain, C.Y.; Damonte, L.C.; Ferrari, S.; Munoz, E.; Torres, C. Rodriguez; Pasquevich, A.F.

    2010-01-01

    A high-k HfO 2 /SiO 2 gate stack is taking the place of SiO 2 as a gate dielectric in field effect transistors. This fact makes the study of the solid-state reaction between these oxides very important. Nanostructure characterization of a high-energy ball milled and post-annealed equimolar HfO 2 and amorphous SiO 2 powder mixture has been carried out by perturbed angular correlations (PAC) technique. The study was complemented with X-ray diffraction and positron annihilation lifetime spectroscopy (PALS). The experimental results revealed that the ball milling of equimolar mixtures increases the defects concentration in hafnium oxide. No solid-state reaction occurred even after 8 h of milling. The formation of HfSiO 4 (hafnon) was observed in the milled blends annealed at high temperatures.The PAC results of the milled samples are compared with those obtained for pure m-ZrO 2 subjected to high-energy ball milling and with reported microstructure data for the system ZrO 2 -SiO 2 .

  9. The coercivity mechanism of Pr–Fe–B nanoflakes prepared by surfactant-assisted ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Zuo, Wen-Liang, E-mail: wlzuo@iphy.ac.cn; Zhang, Ming; Niu, E.; Shao, Xiao-Ping; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen, E-mail: shenbg@aphy.iphy.ac.cn

    2015-09-15

    The strong (00l) textured Pr{sub 12+x}Fe{sub 82−x}B{sub 6} (x=0, 1, 2, 3, 4) nanoflakes with high coercivity were prepared by surfactant-assisted ball milling (SABM). The thickness and length of the flakes are mainly in the range of 50−200 nm and 0.5−2 μm, respectively. A coercivity of 4.16 kOe for Pr{sub 15}Fe{sub 79}B{sub 6} nanoflakes was obtained, which is the maximum coercivity of R{sub 2}Fe{sub 14}B (R=Pr, Nd) nanoflakes or nanoparticles reported up to now. The results of XRD and SEM for the aligned Pr{sub 15}Fe{sub 79}B{sub 6} nanoflakes indicate that a strong (00l) texture is obtained and the easy magnetization direction is parallel to the surface of the flakes. The angular dependence of coercivity for aligned sample indicates that the coercivity mechanism of the as-milled nanoflakes is mainly dominated by domain wall pinning. Meanwhile, the field dependence of coercivity, isothermal (IRM) and dc demagnetizing (DCD) remanence curves also indicate that the coercivity is mainly determined by domain wall pinning, and nucleation also has an important effect. In addition, the mainly interaction of flakes is dipolar coupling. The research of coercivity mechanism for Pr{sub 15}Fe{sub 79}B{sub 6} nanoflakes is important for guidance the further increase its value, and is useful for the future development of the high performance nanocomposite magnets and soft/hard exchange spring magnets. - Highlights: • A coercivity of 4.16 kOe for Pr{sub 15}Fe{sub 79}B{sub 6} nanoflakes was obtained. • The strong (00l) textured is obtained for Pr{sub 15}Fe{sub 79}B{sub 6} nanoflakes. • The interaction of nanoflakes is mainly dipolar coupling. • Domain wall pinning is the mainly coercivity mechanism.

  10. The microstructure of mechanically alloyed nanocrystalline aluminium-magnesium

    Energy Technology Data Exchange (ETDEWEB)

    Gubicza, J. [Dept. of General Physics, Eoetvoes Univ., Budapest (Hungary); Dept. of Solid State Physics, Eoetvoes Univ., Budapest (Hungary); Kassem, M. [Dept. of Materials Science and Engineering, Faculty of Petroleum and Mining, Suez Canal Univ., Suez (Egypt); Ungar, T. [Dept. of General Physics, Eoetvoes Univ., Budapest (Hungary)

    2004-07-01

    The effect of the nominal Mg content and the milling time on the microstructure of mechanically alloyed Al(Mg) solid solutions is studied. The crystallite size distribution and the dislocation structure are determined by X-ray diffraction peak profile analysis. Magnesium gradually goes into solid solution during ball milling and after 3 h almost all of the Mg atoms are soluted into the Al matrix. With increasing milling time the Mg content in solid solution, the dislocation density as well as the hardness are increasing, whereas the crystallite size is decreasing. A similar tendency of these parameters is observed at a particular duration of ball milling with increasing of the nominal Mg content. At the same time for a long milling period the dislocation density slightly decreases together with a slight reduction of the hardness. (orig.)

  11. Formation of ultra-fine grained SUS316L steels by ball-milling and their mechanical properties after neutron irradiation

    International Nuclear Information System (INIS)

    Zheng, Y.J.; Yamasaki, T.; Fukami, T.; Terasawa, M.; Mitamura, T.

    2003-01-01

    In order to overcome the irradiation embrittlement in austenitic stainless steels, ultra-fine grained SUS316L steels with very fine TiC particles have been developed. The SUS316L-TiC nanocomposite powders having 1.0 to 2.0 mass% TiC were prepared by ball-milling SUS316L-TiC powder mixtures for 125 h in an argon gas atmosphere. The milled powders were consolidated by hot isostatic pressing (HIP) under a pressure of 200 MPa at temperatures between 700 and 1000 C, and the bulk materials with grain sizes between 100 and 400 nm have been produced. The possibility of using fine-grained TiC particles to pin grain boundaries and thereby maintain the ultra-fine grained structures has been discussed. In order to clarify the effects of the neutron irradiation on mechanical properties of the ultra-fine grained SUS316L steels, Vickers microhardness measurements were performed before and after the irradiation of 1.14 x 10 23 n/m 2 and 1.14 x 10 24 n/m 2 . The hardness increased with increasing the dose of the irradiation. However, these increasing rates of the ultra-fine grained steels were much smaller than those of the coarse-grained SUS316L steels having grain sizes between 13 and 50 μm. (orig.)

  12. The use of one-dimensional Niobate to improve MgH{sub 2} hydrogen sorption

    Energy Technology Data Exchange (ETDEWEB)

    Brum, M.C., E-mail: mbrum@metalmat.ufrj.br; Conceição, M.O.T. da; Jardim, P.M.; Santos, D.S. dos

    2014-12-05

    Highlights: • The 1-D Niobate W and Niobate C catalysts were synthesized. • The composites MgH{sub 2} + 5 wt.% catalysts were obtained by 20 min of mechanical milling. • The synthesized wired-like material 1-D Niobate W showed to be a promising catalyst. • A desorption capacity of 6.0 wt.%. of H{sub 2} was attained in 10 min with MgH{sub 2} + 5 wt.% 1-D Niobate W. - Abstract: A study was performed on the hydrogen absorption/desorption properties of MgH{sub 2} with the addition of Niobates synthesized by hydrothermal treatment of Nb{sub 2}O{sub 5} in 10 M NaOH. Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD) were used to evaluate their synthesis and show the morphological and crystallographic differences between Nb{sub 2}O{sub 5} used as a precursor and the Niobates produced, the one-dimensional wired type, 1-D Niobate W and the cuboid one, Niobate C. The ball milling of MgH{sub 2} with the Niobates was performed within only 20 min and afterwards the Differential Scanning Calorimetry (DSC) examination of MgH{sub 2} + 1-D Niobate W and MgH{sub 2} + Niobate C showed the shifting of the peaks for both composites in comparison to pure MgH{sub 2}. The influence of the two different types of Niobates and also the Nb{sub 2}O{sub 5} on the hydrogen absorption/desorption capacity was evaluated at 350 °C. The higher absorption and desorption values were attained by the MgH{sub 2} + 5 wt.% 1-D Niobate W composite, reaching, in 10 min, approximately 5.0 wt.% and 6.0 wt.%, respectively. The possible mechanism involved in such property improvement upon adding niobium based catalysts with different morphology and structure was discussed.

  13. Ball Nut Preload Diagnosis of the Hollow Ball Screw through Support Vector Machine

    Directory of Open Access Journals (Sweden)

    Yi-Cheng Huang

    2018-01-01

    Full Text Available This paper studies the diagnostic results of hollow ball screws with different ball nut preload through the support vector machine (SVM process. The method is testified by considering the use of ball screw pretension and different ball nut preload. SVM was used to discriminate the hollow ball screw preload status through the vibration signals and servo motor current signals. Maximum dynamic preloads of 2%, 4%, and 6% ball screws were predesigned, manufactured, and conducted experimentally. Signal patterns with different preload features are separatedby SVM. The irregularity development of the ball screw driving motion current and rolling balls vibration of the ball screw can be discriminated via SVM based on complexity perception. The experimental results successfully show that the prognostic status of ball nut preload can be envisaged by the proposed methodology. The smart reasoning for the health of the ball screw is available based on classification of SVM. This diagnostic method satisfies the purposes of prognostic effectiveness on knowing the ball nut preload status

  14. Producing a particle-reinforced AlCuMgMn alloy by means of mechanical alloying; Herstellung einer partikelverstaerkten AlCuMgMn-Legierung durch mechanisches Legieren

    Energy Technology Data Exchange (ETDEWEB)

    Nestler, D.; Wielage, B. [TU Chemnitz, Institut fuer Werkstoffwissenschaft und Werkstofftechnik (Germany); Siebeck, S.

    2012-07-15

    High-energy ball milling (HEM) with subsequent consolidation is a suitable method to produce particle-reinforced aluminium materials. The task of HEM is to distribute the reinforcement particles as homogeneously as possible. A further application of HEM is mechanical alloying (MA). This paper deals with the combination of both applications. Pure metallic powders (Al, Cu, Mg, Mn) were milled together with SiC particles up to 10 h. The composition of the metallic powder corresponds to that of the alloy AA2017 (3.9% Cu, 0.7% Mg, 0.6% Mn). In previous experiments [1], this alloy was used in the form of atomized powder. The changes in microstructure during the formation of the composite powder have been studied by light microscopy, SEM, EDXS and XRD. The results show that the production of composite powders in a single step is possible. This not only allows the economical production of such powders, but also facilitates the use of alloy compositions that are not producible via the melting route, or only producible with difficulty via the melting route. It's possible to produce tailor-made-alloys. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  15. An example of how to handle amorphous fractions in API during early pharmaceutical development: SAR114137--a successful approach.

    Science.gov (United States)

    Petzoldt, Christine; Bley, Oliver; Byard, Stephen J; Andert, Doris; Baumgartner, Bruno; Nagel, Norbert; Tappertzhofen, Christoph; Feth, Martin Philipp

    2014-04-01

    The so-called pharmaceutical solid chain, which encompasses drug substance micronisation to the final tablet production, at pilot plant scale is presented as a case study for a novel, highly potent, pharmaceutical compound: SAR114137. Various solid-state analytical methods, such as solid-state Nuclear Magnetic Resonance (ssNMR), Differential Scanning Calorimetry (DSC), Dynamic Water Vapour Sorption Gravimetry (DWVSG), hot-stage Raman spectroscopy and X-ray Powder Diffraction (XRPD) were applied and evaluated to characterise and quantify amorphous content during the course of the physical treatment of crystalline active pharmaceutical ingredient (API). DSC was successfully used to monitor the changes in amorphous content during micronisation of the API, as well as during stability studies. (19)F solid-state NMR was found to be the method of choice for the detection and quantification of low levels of amorphous API, even in the final drug product (DP), since compaction during tablet manufacture was identified as a further source for the formation of amorphous API. The application of different jet milling techniques was a critical factor with respect to amorphous content formation. In the present case, the change from spiral jet milling to loop jet milling led to a decrease in amorphous API content from 20-30 w/w% to nearly 0 w/w% respectively. The use of loop jet milling also improved the processability of the API. Stability investigations on both the milled API and the DP showed a marked tendency for recrystallisation of the amorphous API content on exposure to elevated levels of relative humidity. No significant impact of amorphous API on either the chemical stability or the dissolution rate of the API in drug formulation was observed. Therefore, the presence of amorphous content in the oral formulation was of no consequence for the clinical trial phases I and II. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. MgB2 ultrathin films fabricated by hybrid physical chemical vapor deposition and ion milling

    Directory of Open Access Journals (Sweden)

    Narendra Acharya

    2016-08-01

    Full Text Available In this letter, we report on the structural and transport measurements of ultrathin MgB2 films grown by hybrid physical-chemical vapor deposition followed by low incident angle Ar ion milling. The ultrathin films as thin as 1.8 nm, or 6 unit cells, exhibit excellent superconducting properties such as high critical temperature (Tc and high critical current density (Jc. The results show the great potential of these ultrathin films for superconducting devices and present a possibility to explore superconductivity in MgB2 at the 2D limit.

  17. Influence of Process Control Agent on Characterization and Structure of Micron Chitosan Powders Prepared by Ball Milling Method

    Directory of Open Access Journals (Sweden)

    ZHANG Chuan-jie

    2016-12-01

    Full Text Available With ethyl alcohol or distilled water as process control agent (PCA, micron chitosan powder was prepared by ball milling method. The yield rate, particle size distribution, micro morphology, viscosity average molecular mass, chemical and crystal structures, and thermal properties of these different micron chitosan powders were measured. The results indicate that the yield rate of micron chitosan powders prepared with ethyl alcohol as PCA increases significantly, and improves to 94.7% from 25% while the amount of ethyl alcohol is 0.75mL/g. The particle size distribution of micron chitosan powder prepared with ethyl alcohol as PCA is concentrated, while the D50 and D90 in size are 824nm and 1629nm respectively. Chitosan do not react with ethyl alcohol used as PCA, but the viscosity average molecular mass of prepared micron chitosan powder decreases by 23%, the crystal structures are destroyed slightly, and its thermal stability is slightly weakened.

  18. In vitro metal ion release and biocompatibility of amorphous Mg{sub 67}Zn{sub 28}Ca{sub 5} alloy with/without gelatin coating

    Energy Technology Data Exchange (ETDEWEB)

    Chan, W.Y., E-mail: chan.wing.yue@sgh.com.sg [School of Mechanical and Aerospace Engineering, Nanyang Technological University (Singapore); Department of Plastic, Reconstructive and Aesthetic Surgery, Singapore General Hospital (Singapore); Chian, K.S.; Tan, M.J. [School of Mechanical and Aerospace Engineering, Nanyang Technological University (Singapore)

    2013-12-01

    Amorphous zinc-rich Mg–Zn–Ca alloys have exhibited good tissue compatibility and low hydrogen evolution in vivo. However, suboptimal cell–surface interaction on magnesium alloy surface observed in vitro could lead to reduced integration with host tissue for regenerative purpose. This study aims to improve cell–surface interaction of amorphous Mg{sub 67}Zn{sub 28}Ca{sub 5} alloy by coating a gelatin layer by electrospinning. Coated/uncoated alloys were immersed and extracted for 3 days under different CO{sub 2}. The immersion results showed that pH and metal ion release in the alloy extracts were affected by gelatin coating and CO{sub 2}, suggesting their roles in alloy biocorrosion and a mechanism has been proposed for the alloy–CO{sub 2} system with/without coating. Cytotoxicity results are evident that gelatin-coated alloy with 2-day crosslinking not only exhibited no indirect cytotoxicity, but also supported attachment of L929 and MG63 cell lines around/on the alloy with high viability. Therefore, amorphous Mg{sub 67}Zn{sub 28}Ca{sub 5} alloy coated with gelatin by electrospinning technique provides a useful method to improve alloy biocompatibility. - Highlights: • Electrospinning is a new method to coat amorphous Mg{sub 67}Zn{sub 28}Ca{sub 5} alloy with gelatin. • Gelatin-coated alloy has differential effect on pH and ion release at various CO{sub 2}. • L929 cell proliferation correlates with Mg{sup 2+} level in alloy extracts. • Biomimetic gelatin coating significantly improves cell–surface interaction.

  19. Crystal structure and stability of LiAlD4 with TiF3 additive

    International Nuclear Information System (INIS)

    Brinks, H.W.; Fossdal, A.; Fonnelop, J.E.; Hauback, B.C.

    2005-01-01

    LiAlD 4 samples with TiF 3 additives have been investigated by synchrotron X-ray diffraction, neutron diffraction and a Sieverts-type apparatus. Directly after ball milling there are no signs of any Ti-containing phases, and the unit-cell of LiAlD 4 and Al give no indication of any solid solutions. Hence it is concluded that the Ti is in an amorphous state directly after ball milling. Furthermore, no LiF was observed in the samples. Based on Sieverts-type measurements the plateau pressure at 80 deg C has been proved to be higher than 85 bar. Samples stored in a glove box are slowly desorbed, and after 6 months for a LiAlD 4 + TiF 3 sample, the reaction to LiD + Al is nearly finished

  20. Monitoring alloy formation during mechanical alloying process by x-ray diffraction techniques

    International Nuclear Information System (INIS)

    Abdul Kadir Masrom; Noraizam Md Diah; Mazli Mustapha

    2002-01-01

    Monitoring alloying (MA) is a novel processing technique that use high energy impact ball mill to produce alloys with enhanced properties and microscopically homogeneous materials starting from various powder mixtures. Mechanical alloying process was originally developed to produce oxide dispersion strengthened nickel superalloys. In principal, in high-energy ball milling process, alloy is formed by the result of repeated welding, fracturing and rewelding of powder particles in a high energy ball mill. In this process a powder mixture in a ball mill is subjected to high-energy collisions among balls. MA has been shown to be capable of synthesizing a variety of materials. It is known to be capable to prepare equilibrium and non-equilibrium phases starting from blended elemental or prealloyed powders. The process ability to produce highly metastable materials such as amorphous alloys and nanostructured materials has made this process attractive and it has been considered as a promising material processing technique that could be used to produce many advanced materials at low cost. The present study explores the conditions under which aluminum alloys formation occurs by ball milling of blended aluminum and its alloying elements powders. In this work, attempt was made in producing aluminum 2024 alloys by milling of blended elemental aluminum powder of 2024 composition in a stainless steel container under argon atmosphere for up to 210 minutes. X-ray diffraction together with thermal analysis techniques has been used to monitor phase changes in the milled powder. Results indicate that, using our predetermined milling parameters, alloys were formed after 120 minutes milling. The thermal analysis data was also presented in this report. (Author)

  1. A systematic study of ball passing frequencies based on dynamic modeling of rolling ball bearings with localized surface defects

    Science.gov (United States)

    Niu, Linkai; Cao, Hongrui; He, Zhengjia; Li, Yamin

    2015-11-01

    Ball passing frequencies (BPFs) are very important features for condition monitoring and fault diagnosis of rolling ball bearings. The ball passing frequency on outer raceway (BPFO) and the ball passing frequency on inner raceway (BPFI) are usually calculated by two well-known kinematics equations. In this paper, a systematic study of BPFs of rolling ball bearings is carried out. A novel method for accurately calculating BPFs based on a complete dynamic model of rolling ball bearings with localized surface defects is proposed. In the used dynamic model, three-dimensional motions, relative slippage, cage effects and localized surface defects are all considered. Moreover, localized surface defects are modeled accurately with consideration of the finite size of the ball, the additional clearance due to material absence, and changes of contact force directions. The reasonability of the proposed method for the prediction of dynamic behaviors of actual ball bearings with localized surface defects and for the calculation of BPFs is discussed by investigating the motion characteristics of a ball when it rolls through a defect. Parametric investigation shows that the shaft speed, external loads, the friction coefficient, raceway groove curvature factors, the initial contact angle, and defect sizes have great effects on BPFs. For a loaded ball bearing, the combination of rolling and sliding in contact region occurs, and the BPFs calculated by simple kinematical relationships are inaccurate, especially for high speed, low external load, and large initial contact angle conditions where severe skidding occurs. The hypothesis that the percentage variation of the spacing between impulses in a defective ball bearing was about 1-2% reported in previous investigations can be satisfied only for the conditions where the skidding effect in a bearing is slight. Finally, the proposed method is verified with two experiments.

  2. Mechanical properties and fracture mechanism of as-cast Mg{sub 77}TM{sub 12}Zn{sub 5}Y{sub 6} (TM = Cu, Ni) bulk amorphous matrix composites

    Energy Technology Data Exchange (ETDEWEB)

    Qiu, K.Q. [School of Materials Science and Engineering, Shenyang University of Technology, Shenyang 110178 (China)], E-mail: kqqiu@yahoo.com.cn; Hu, N.N.; Zhang, H.B. [School of Materials Science and Engineering, Shenyang University of Technology, Shenyang 110178 (China); Jiang, W.H. [Department of Materials Science and Engineering, The University of Tennessee, Knoxville, TN 37990 (United States); Ren, Y.L. [School of Materials Science and Engineering, Shenyang University of Technology, Shenyang 110178 (China); Liaw, P.K. [Department of Materials Science and Engineering, The University of Tennessee, Knoxville, TN 37990 (United States)

    2009-06-10

    Comparative investigations on the microstructures, thermal stability and mechanical properties of Mg{sub 77}Cu{sub 12}Zn{sub 5}Y{sub 6} and Mg{sub 77}Ni{sub 12}Zn{sub 5}Y{sub 6} bulk metallic glass matrix composites were carried out by using scanning electron microscopy (SEM), DSC and compressive tester. The results show that the microstructure of as-cast samples with 3 mm in diameter for Cu-containing alloy is consisted of Mg flakes and dotted Mg{sub 2}Cu phase in the amorphous matrix, while the as-cast Ni-containing alloy with the same diameter is mainly consisted of Mg flakes in the amorphous matrix. The glass transition temperature and supercooled liquid region are 413 K and 27 K for the Cu-containing, 443 K and 32 K for the Ni-containing amorphous matrix composites, respectively. The fracture strength, yield strength and plastic strain are 532 MPa, 390 MPa and 2.4% for the Cu-containing alloy, 667 MPa, 412 MPa and 7% for the Ni-containing alloy, respectively. Furthermore, the fracture mechanism for the amorphous matrix composites was discussed according to both the fracture surfaces and the stress-strain curves.

  3. Composites Strengthened with Graphene Platelets and Formed in Semisolid State Based on α and α/β MgLiAl Alloys

    Science.gov (United States)

    Dutkiewicz, Jan; Rogal, Łukasz; Fima, Przemyslaw; Ozga, Piotr

    2018-05-01

    MgLiAl base composites strengthened with graphene platelets were prepared by semisolid processing of ball-milled alloy chips with 2% of graphene platelets. Composites strengthened with graphene platelets show higher hardness and yield stress than the cast alloys, i.e., 160 MPa as compared to 90 MPa for as-cast alloy MgLi9Al1.5. Mechanical properties for MgLiAl-based composites were similar or higher than for composites based on conventional AZ91 or WE43 alloys. The strengthening however was not only due to the presence of graphene, but also phases resulting from the reaction between carbon and lithium, i.e., Li2C2 carbide. Graphene platelets were located at globules boundaries resulting from semisolid processing for all investigated composites. Graphene platelets were in agglomerates forming continuous layers at grain boundaries in the composite based on the alloy MgLi4.5Al1.5. The shape of agglomerates was more complex and wavy in the composite based on MgLi9Al1.5 alloy most probably due to lithium-graphene reaction. Electron diffraction from the two-phase region α + β in MgLi9Al1.5 indicated that [001]α and [110]β directions are rotated about 4° from the ideal relationship [001] hex || [110] bcc phases. It showed higher lattice rotation than in earlier studies what is most probably caused by lattice slip and rotation during semisolid pressing causing substantial deformation particularly within the β phase. Raman spectroscopy studies confirmed the presence of graphene platelets within agglomerates and in addition the presence mainly of Li2C2 carbides in composites based on MgLi4.5Al1.5 and Mg9Li1.5Al alloys. From the character of Raman spectra refinement of graphene platelets was found in comparison with their initial size. The graphene areas without carbides contain graphene nanoplatelets with lateral dimension close to initial graphene sample. Electron diffraction allowed to confirm the presence of Li2C2 carbide at the surface of agglomerates found from

  4. Effect of degassing temperature on the microstructure of a nanocrystalline Al-Mg alloy

    International Nuclear Information System (INIS)

    Ahn, Byungmin; Newbery, A. Piers; Lavernia, Enrique J.; Nutt, Steven R.

    2007-01-01

    The microstructural evolution of a nanocrystalline Al-Mg alloy was investigated to determine the effects of degassing temperature. Al 5083 powder was ball-milled in liquid nitrogen to obtain a nanocrystalline structure, then vacuum degassed to remove contaminants. The degassed powder was consolidated by cold isostatic pressing and then forged to produce bulk, low-porosity material. The material microstructure was analyzed at different stages using optical microscopy, transmission electron microscopy, and density measurements. The impurity concentration of the final product was also measured. The forged material exhibited a bimodal grain size distribution, consisting of both ultra fine and coarse grains. The bimodal distribution was attributed to the presence of residual coarse grains in the as-milled powder. Higher degassing temperatures resulted in higher density values and lower hydrogen content in the consolidated materials, although these materials also exhibited more extensive grain growth

  5. Hydrogen storage properties in the Mg_0_._7_5Ta_0_._2_5 system prepared by mechanical milling

    International Nuclear Information System (INIS)

    Ramirez G, J. A.

    2016-01-01

    Magnesium and most of its mixtures have slow sorption-desorption kinetics of hydrogen, which limits their technological application and their viability from the economic view point. Recently, has been observed that by the synthesis of advanced materials, using the mechanical milling technique, positive changes in the kinetics are introduced. In order to improve the sorption-desorption hydrogen properties, in the present work a mixture consisting of Mg_0_._7_5Ta_0_._2_5 was prepared using methanol as process control agent. To this end, the first methodological step was to carry out, by means of the mechanical milling technique, the synthesis of the mixture Mg_0_._7_5Ta_0_._2_5 in a Spex type vibratory mill at times of 6, 12, 18 and 24 h. Subsequently, the material was characterized by different analytical techniques such as scanning electron microscopy with elemental analysis, X-ray diffraction and N_2 physisorption analysis. Subsequently, hydrogen sorption experiments were carried out in a Parr reactor to evaluate the hydrogen storage capacity of the mixture, varying temperature parameters, pressure and time, in order to determine the optimal parameters of hydrogen sorption. The characterization of the hydrogen storage capacity was analyzed by the thermogravimetric analysis/differential scanning calorimetry technique coupled to a mass spectrometer. X ray diffraction analysis reveals that there is a mixture between the starting compounds, with an important refinement of the microstructure as a consequence of the mechanical milling process. The results of the hydrogen sorption tests at 1, 5 and 10 cycles showed that the storage of hydrogen in the Mg_0_._7_5Ta_0_._2_5 mixture can be carried out at a temperature of 25 degrees Celsius with a pressure of 2 atm and a contact time of 1 h. (Author)

  6. Preliminary Test of Upgraded Conventional Milling Machine into PC Based CNC Milling Machine

    International Nuclear Information System (INIS)

    Abdul Hafid

    2008-01-01

    CNC (Computerized Numerical Control) milling machine yields a challenge to make an innovation in the field of machining. With an action job is machining quality equivalent to CNC milling machine, the conventional milling machine ability was improved to be based on PC CNC milling machine. Mechanically and instrumentally change. As a control replacing was conducted by servo drive and proximity were used. Computer programme was constructed to give instruction into milling machine. The program structure of consists GUI model and ladder diagram. Program was put on programming systems called RTX software. The result of up-grade is computer programming and CNC instruction job. The result was beginning step and it will be continued in next time. With upgrading ability milling machine becomes user can be done safe and optimal from accident risk. By improving performance of milling machine, the user will be more working optimal and safely against accident risk. (author)

  7. MgF2 katkısının Vermikülit esaslı cam-seramiklerin işlenebilirlik özellikleri üzerine etkisi

    Directory of Open Access Journals (Sweden)

    Ediz Ercenk

    2017-04-01

    Full Text Available The study deals with production of the glass-ceramics from natural raw material vermiculite. The machinability properties of the glass-ceramic compositions were investigated depending on vermiculite and MgF2 contents. The compositions containing 80 %, 85 %, 90 % vermiculite, 5 % K2O and MgF2 as remainder were mixed by using a ball mill for 2 h and coded as VER80, VER85 and VER90. The mixed and milled powders were sieved and disc samples were prepared by pressing at 100 MPa. The shaped samples were sintered at 900-1100 ºC for 1 h. X-ray diffraction (XRD, scanning electron microscopy (SEM, and machinability test were conducted. The results have indicated that the samples have good sintering and machinability properties.

  8. Nd2Fe14C-based magnet with better permanent magnetic properties prepared by a simple mechanochemical method

    Science.gov (United States)

    Geng, Hongmin; Ji, Yuan; Zhang, Jingjing; Gao, Yuchao; Yan, Yu; Wang, Wenquan; Su, Feng; Du, Xiaobo

    2017-11-01

    Nd2Fe14C-based magnet is prepared by a mechanochemical method, namely high-energy ball-milling Nd2Fe11Bx (x = 0-0.15) alloy in heptane (C7H16), followed by annealing to 850 °C in vacuum. Under the action of high-energy ball-milling, Nd2Fe11Bx react with heptane to form NdH2+δ, Fe-(CB), C, etc. H2 is released and Nd2Fe17, Nd2Fe17Cx (x = 0-3), Nd2Fe14C, Nd carbides and α-Fe are formed in the subsequent annealing. C amount depends on ball-milling time t. Long time ball milling or high C content suppresses the formation of 2:17 phase and favors the formation of 2:14:1 phase in the final products. Excessive ball-milling results in the quick increase of α-Fe. The maximum of magnetically hard Nd2Fe14C is obtained at t = 4 h. For Nd2Fe11 samples, there exists considerable quantity of Nd carbides and α-Fe phase appears earlier and increases rapidly with extending the ball-milling time t. The addition of B element shortens the ball-milling time of the formation of maximum Nd2Fe14C and prominently suppresses the formation of Nd carbide and α-Fe. The optimum magnetic properties, coercivity iHc of 1193.7 kA/m, remanence Mr of 580.9 kA/m, maximum magnetic energy product (BH)max of 91.7 kJ/m3 is approaching to its theoretic value of 99.2 kJ/m3 for isotropic Nd2Fe14C magnet, are obtained in Nd2Fe11B0.06 alloy ball milled for 3.5 h.

  9. KSC ADVANCED GROUND BASED FIELD MILL V1

    Data.gov (United States)

    National Aeronautics and Space Administration — The Advanced Ground Based Field Mill (AGBFM) network consists of 34 (31 operational) field mills located at Kennedy Space Center (KSC), Florida. The field mills...

  10. Fabrication and characterization of Cu/YSZ cermet high-temperature electrolysis cathode material prepared by high-energy ball-milling method

    International Nuclear Information System (INIS)

    Lee, Sungkyu; Kang, Kyoung-Hoon; Kim, Jong-Min; Hong, Hyun Seon; Yun, Yongseung; Woo, Sang-Kook

    2008-01-01

    Cu/YSZ composites (40 and 60 vol.% Cu powder with balance YSZ) was successfully fabricated by high-energy ball-milling of Cu and YSZ powders at 400 rpm for 24 h, pressing into pellets (O 13 mm x 2 mm) and subsequent sintering process at 900 deg. C under flowing 5%-H 2 /Ar gas for use as cermet cathode material of high-temperature electrolysis (HTE) of water vapor in a more economical way compared with conventional Ni/YSZ cermet cathode material. The Cu/YSZ composite powders thus synthesized and sintered were characterized using various analytical tools such as XRD, SEM, and laser diffraction and scattering method. Electrical conductivity of sintered Cu/YSZ cermet pellets thus fabricated was measured using 4-probe technique and compared with that of Ni/YSZ cermets. The effect of composites composition on the electrical conductivity was investigated and marked increase in electrical conductivity for copper contents greater than 40 vol.% in the composite was explained by percolation threshold

  11. Pulsed current activated synthesis and rapid consolidation of a nanostructured Mg2Al4Si5O18 and its mechanical properties

    Science.gov (United States)

    Shon, In-Jin; Kang, Hyun-Su; Doh, Jung-Mann; Yoon, Jin-Kook

    2015-03-01

    Nanocrystalline materials have received much attention as advanced engineering materials, with improved mechanical properties. Attention has been directed to the application of nanomaterials, as they possess excellent mechanical properties (high strength, high hardness, excellent ductility and toughness). A singlestep synthesis and consolidation of nanostructured Mg2Al4Si5O18 was achieved by pulsed current heating, using the stoichiometric mixture of MgO, Al2O3 and SiO2 powders. Before sintering, the powder mixture was high-energy ball milled for 10 h. From the milled powder mixture, a highly dense nanostructured Mg2Al4Si5O18 compound could be obtained within one minute, under the simultaneous application of 80 MPa pressure, and a pulsed current. The advantage of this process is that it allows an instant densification to the near theoretical density, while sustaining the nanosized microstructure of raw powders. The sintering behavior, microstructure and mechanical properties of Mg2Al4Si5O18 were evaluated. The fracture toughness of a nanostructured Mg2Al4Si5O18 compound was higher than that of sub-micron Mg2Al4Si5O18 compound.

  12. Atomic pairwise distribution function analysis of the amorphous phase prepared by different manufacturing routes

    DEFF Research Database (Denmark)

    Boetker, Johan P.; Koradia, Vishal; Rades, Thomas

    2012-01-01

    was subjected to quench cooling thereby creating an amorphous form of the drug from both starting materials. The milled and quench cooled samples were, together with the crystalline starting materials, analyzed with X-ray powder diffraction (XRPD), Raman spectroscopy and atomic pair-wise distribution function...... (PDF) analysis of the XRPD pattern. When compared to XRPD and Raman spectroscopy, the PDF analysis was superior in displaying the difference between the amorphous samples prepared by milling and quench cooling approaches of the two starting materials....

  13. Structural and magnetic properties of Fe{sub 60}Al{sub 40} alloys prepared by means of a magnetic mill

    Energy Technology Data Exchange (ETDEWEB)

    Bernal-Correa, R. [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Manizales (Colombia); Rosales-Rivera, A., E-mail: arosalesr@unal.edu.c [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Manizales (Colombia); Pineda-Gomez, P. [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Manizales (Colombia); Universidad de Caldas, Manizales (Colombia); Salazar, N.A. [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Manizales (Colombia)

    2010-04-16

    A study on synthesis, structural and magnetic characterization of Fe{sub 60}Al{sub 40} (at.%) alloys prepared by means of mechanical alloying process is presented. The mechanical alloying was performed using a milling device with magnetically controlled ball movement (Uni-Ball-Mill 5 equipment) at several milling times. The characterization was carried out via X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The effects of milling time on the structural state, morphological evolution and magnetic behaviour of the Fe{sub 60}Al{sub 40} (at.%) alloys are discussed. Besides, in this current study we emphasize the result that indicating a ferro-para-ferromagnetic transition from a correlation between X-ray diffraction and magnetization data.

  14. Particle and powder characterisation of Bi-based superconductors

    International Nuclear Information System (INIS)

    Yavuz, M.; Guo, Y. C.; Liu, H. L.; Dou, S. X.; Vance, E. R.

    1996-01-01

    Full text: Superconductor precursor powder was ground in a planetary and an attrition mill using various combinations of grinding container, balls and carrier (dry and wet). Dry milling was found to be more effective than wet milling for reducing particle size irrespective of container and ball materials used in the planetary milling. On the other hand, wet milling was found more effective in the attrition milling. Serious Si contamination was observed in powders milled using agate grinding materials. Some C from polypropylene container was found after milling, but no Zr from YSZ balls. Effect of particle size on the property of Bi 2223/Ag tapes was investigated in terms of critical current density (J c ). Fine particle size was found to show high J c

  15. Processing of Syndiotactic Polystyrene to Microspheres for Part Manufacturing through Selective Laser Sintering

    Directory of Open Access Journals (Sweden)

    Nicolas Mys

    2016-10-01

    Full Text Available Syndiotactic polystyrene pellets were processed into powder form using mechanical (ball milling, rotor milling and physicochemical (spray drying techniques with the intention of using it as feed material for selective laser sintering. New materials are an important component in broadening the application window for selective laser sintering but must meet strict requirements to be used. Particles obtained were characterized in size and shape using SEM imaging, analyzed by software, and compared to the product obtained by conventional ball milling. Rotor milling and spray drying proved capable of making spherical powders, yet only rotor milling achieved particles with a mean diameter within the desired range of 45–97 µm. Subsequently, the obtained powders were examined for the effect each processing technique imparts on the intrinsic properties of the material. Differential scanning calorimetry analysis revealed amorphization for all methods and a reduction in crystallinity after processing, however, the reduction in crystallinity was acceptably low for the spray-dried and rotor-milled powders. Ball milling displayed an exceptional reduction in crystallinity, suggesting severe degradation. As a final test, the rotor-milled powder was subjected to single-layer test and displayed good coalescence and smooth morphology, albeit with a large amount of warpage.

  16. Crystal structure and stability of LiAlD{sub 4} with TiF{sub 3} additive

    Energy Technology Data Exchange (ETDEWEB)

    Brinks, H.W. [Department of Physics, Institute for Energy Technology, P.O. Box 40, Kjeller NO-2027 (Norway)]. E-mail: hwbrinks@ife.no; Fossdal, A. [Department of Physics, Institute for Energy Technology, P.O. Box 40, Kjeller NO-2027 (Norway); Fonnelop, J.E. [Department of Physics, Institute for Energy Technology, P.O. Box 40, Kjeller NO-2027 (Norway); Hauback, B.C. [Department of Physics, Institute for Energy Technology, P.O. Box 40, Kjeller NO-2027 (Norway)

    2005-07-19

    LiAlD{sub 4} samples with TiF{sub 3} additives have been investigated by synchrotron X-ray diffraction, neutron diffraction and a Sieverts-type apparatus. Directly after ball milling there are no signs of any Ti-containing phases, and the unit-cell of LiAlD{sub 4} and Al give no indication of any solid solutions. Hence it is concluded that the Ti is in an amorphous state directly after ball milling. Furthermore, no LiF was observed in the samples. Based on Sieverts-type measurements the plateau pressure at 80 deg C has been proved to be higher than 85 bar. Samples stored in a glove box are slowly desorbed, and after 6 months for a LiAlD{sub 4} + TiF{sub 3} sample, the reaction to LiD + Al is nearly finished.

  17. Reactive wetting of amorphous silica by molten Al–Mg alloys and their interfacial structures

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Laixin [Key Laboratory of Automobile Materials (Ministry of Education), Department of Materials Science and Engineering, Jilin University, No. 5988 Renmin Street, Changchun 130025 (China); School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083 (China); Shen, Ping, E-mail: shenping@jlu.edu.cn [Key Laboratory of Automobile Materials (Ministry of Education), Department of Materials Science and Engineering, Jilin University, No. 5988 Renmin Street, Changchun 130025 (China); Zhang, Dan [Editorial Office, Journal of Bionic Engineering, Jilin University, No. 5988 Renmin Street, Changchun 130025 (China); Jiang, Qichuan [Key Laboratory of Automobile Materials (Ministry of Education), Department of Materials Science and Engineering, Jilin University, No. 5988 Renmin Street, Changchun 130025 (China)

    2016-07-30

    Highlights: • The wettability improves with increasing Mg concentration and temperature. • Reaction product zone consists of layered structures relating with Mg concentration. • Formation of MgAl{sub 2}O{sub 4} and MgO at the interface does not promote the wettability. • Formation of Mg{sub 2}Si plays a dominant role in promoting the wettability. • Anomalous recession of the triple line was mainly due to diminishing Mg in the alloy. - Abstract: The reactive wetting of amorphous silica substrates by molten Al–Mg alloys over a wide composition range was studied using a dispensed sessile drop method in a flowing Ar atmosphere. The effects of the nominal Mg concentration and temperature on the wetting and interfacial microstructures were discussed. The initial contact angle for pure Al on the SiO{sub 2} surface was 115° while that for pure Mg was 35° at 1073 K. For the Al–Mg alloy drop, it decreased with increasing nominal Mg concentration. The reaction zone was characterized by layered structures, whose formation was primarily controlled by the variation in the alloy concentration due to the evaporation of Mg and the interfacial reaction from the viewpoint of thermodynamics as well as by the penetration or diffusion of Mg, Al and Si from the viewpoint of kinetics. In addition, the effects of the reaction and the evaporation of Mg on the movement of the triple line were examined. The spreading of the Al–Mg alloy on the SiO{sub 2} surface was mainly attributed to the formation of Mg{sub 2}Si at the interface and the recession of the triple line to the diminishing Mg concentration in the alloy.

  18. Fabrication of Al-20 wt%Si powder using scrap Si by ultra high-energy milling process

    Energy Technology Data Exchange (ETDEWEB)

    Kang, Won-Kyung [Division of Advanced Materials Engineering and Institute for Rare Metals, Kongju National University, 275, Budae-dong, Cheonan, Chungnam 330-717 (Korea, Republic of); Y Latin-Small-Letter-Dotless-I lmaz, Fikret [Department of Physics, Faculty of Art and Science, Gaziosmanpasa University, Tasliciftlik Campus, 60240 Tokat (Turkey); Kim, Hyo-Seob; Koo, Jar-Myung [Division of Advanced Materials Engineering and Institute for Rare Metals, Kongju National University, 275, Budae-dong, Cheonan, Chungnam 330-717 (Korea, Republic of); Hong, Soon-Jik, E-mail: hongsj@kongju.ac.kr [Division of Advanced Materials Engineering and Institute for Rare Metals, Kongju National University, 275, Budae-dong, Cheonan, Chungnam 330-717 (Korea, Republic of)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer High energy ball milling process has been successfully employed to produce Al-20Si alloy using scrap Si powders. Black-Right-Pointing-Pointer Fully finer and homogenous structure could be achieved after 60 min of milling time. Black-Right-Pointing-Pointer Si particles were not dissolved but uniformly dispersed in the Al matrix in a milled state. Black-Right-Pointing-Pointer The hardness of as-milled Al-20Si powder increased steadily with the increase of milling time. Black-Right-Pointing-Pointer Grain size and dispersion strengthening are two mechanisms being responsible for hardness increment. - Abstract: In this study, microstructural evolution and mechanical properties of Al-20 wt%Si and pure Al powders fabricated by ultra high-energy ball milling technique were investigated as a function of milling time. The microstructure and mechanical properties of the as-milled powders were examined by scanning electron microscope (SEM), energy dispersive spectrometry (EDS), X-ray diffractometer (XRD) and Vickers hardness tester. SEM observation showed that the particle size increased at an early stage of milling, and then decreased drastically with further milling. XRD and cross-sectional EDS-mapping analyses revealed that Si particles were not dissolved but uniformly dispersed in the Al matrix in a milled state. Vickers hardness of both pure Al and Al-Si powder increases with milling time, which attributes to the grain size strengthening and dispersion strengthening.

  19. Hybrid ABC Optimized MARS-Based Modeling of the Milling Tool Wear from Milling Run Experimental Data.

    Science.gov (United States)

    García Nieto, Paulino José; García-Gonzalo, Esperanza; Ordóñez Galán, Celestino; Bernardo Sánchez, Antonio

    2016-01-28

    Milling cutters are important cutting tools used in milling machines to perform milling operations, which are prone to wear and subsequent failure. In this paper, a practical new hybrid model to predict the milling tool wear in a regular cut, as well as entry cut and exit cut, of a milling tool is proposed. The model was based on the optimization tool termed artificial bee colony (ABC) in combination with multivariate adaptive regression splines (MARS) technique. This optimization mechanism involved the parameter setting in the MARS training procedure, which significantly influences the regression accuracy. Therefore, an ABC-MARS-based model was successfully used here to predict the milling tool flank wear (output variable) as a function of the following input variables: the time duration of experiment, depth of cut, feed, type of material, etc . Regression with optimal hyperparameters was performed and a determination coefficient of 0.94 was obtained. The ABC-MARS-based model's goodness of fit to experimental data confirmed the good performance of this model. This new model also allowed us to ascertain the most influential parameters on the milling tool flank wear with a view to proposing milling machine's improvements. Finally, conclusions of this study are exposed.

  20. Hybrid ABC Optimized MARS-Based Modeling of the Milling Tool Wear from Milling Run Experimental Data

    Directory of Open Access Journals (Sweden)

    Paulino José García Nieto

    2016-01-01

    Full Text Available Milling cutters are important cutting tools used in milling machines to perform milling operations, which are prone to wear and subsequent failure. In this paper, a practical new hybrid model to predict the milling tool wear in a regular cut, as well as entry cut and exit cut, of a milling tool is proposed. The model was based on the optimization tool termed artificial bee colony (ABC in combination with multivariate adaptive regression splines (MARS technique. This optimization mechanism involved the parameter setting in the MARS training procedure, which significantly influences the regression accuracy. Therefore, an ABC–MARS-based model was successfully used here to predict the milling tool flank wear (output variable as a function of the following input variables: the time duration of experiment, depth of cut, feed, type of material, etc. Regression with optimal hyperparameters was performed and a determination coefficient of 0.94 was obtained. The ABC–MARS-based model's goodness of fit to experimental data confirmed the good performance of this model. This new model also allowed us to ascertain the most influential parameters on the milling tool flank wear with a view to proposing milling machine's improvements. Finally, conclusions of this study are exposed.

  1. Hybrid ABC Optimized MARS-Based Modeling of the Milling Tool Wear from Milling Run Experimental Data

    Science.gov (United States)

    García Nieto, Paulino José; García-Gonzalo, Esperanza; Ordóñez Galán, Celestino; Bernardo Sánchez, Antonio

    2016-01-01

    Milling cutters are important cutting tools used in milling machines to perform milling operations, which are prone to wear and subsequent failure. In this paper, a practical new hybrid model to predict the milling tool wear in a regular cut, as well as entry cut and exit cut, of a milling tool is proposed. The model was based on the optimization tool termed artificial bee colony (ABC) in combination with multivariate adaptive regression splines (MARS) technique. This optimization mechanism involved the parameter setting in the MARS training procedure, which significantly influences the regression accuracy. Therefore, an ABC–MARS-based model was successfully used here to predict the milling tool flank wear (output variable) as a function of the following input variables: the time duration of experiment, depth of cut, feed, type of material, etc. Regression with optimal hyperparameters was performed and a determination coefficient of 0.94 was obtained. The ABC–MARS-based model's goodness of fit to experimental data confirmed the good performance of this model. This new model also allowed us to ascertain the most influential parameters on the milling tool flank wear with a view to proposing milling machine's improvements. Finally, conclusions of this study are exposed. PMID:28787882

  2. Fabrication of Metallic Glass Powder for Brazing Paste for High-Temperature Thermoelectric Modules

    Science.gov (United States)

    Seo, Seung-Ho; Kim, Suk Jun; Lee, Soonil; Seo, Won-Seon; Kim, Il-Ho; Choi, Soon-Mok

    2018-06-01

    Metallic glass (MG) offers the advantage of outstanding oxidation resistance, since it has disordered atomic-scale structure without grain boundaries. We fabricated Al-based MG ribbons (Al84.5Y10Ni5.5) by a melt spinning process. We evaluated the adhesion strength of interfaces between the Al-based MG and a Ni-coated Cu electrode formed under various conditions at high temperature. In addition, we attempted to optimize the process conditions for pulverizing MG ribbons to high-energy ball milling and planetary milling. We confirmed that the electrical resistivity of the Al-based MG ribbon was substantially reduced after annealing at high temperature (over 300°C) due to crystallization.

  3. Co-catalytic effect of Rh and Ru for the ethanol electro-oxidation in amorphous microparticulated alloys

    Energy Technology Data Exchange (ETDEWEB)

    Blanco, Tamara C.; Pierna, Angel R.; Barroso, Javier [Dpto. de Ingenieria Quimica y del Medio Ambiente, Universidad del Pais Vasco, San Sebastian (Spain)

    2011-11-15

    The ethanol electro-oxidation on platinum catalyst in acid media leads to the formation of acetaldehyde and acetic acid as main products. Another problem is the poisoning of the electro-catalyst surface with CO formed during the fuel oxidation reaction. To increase the performance of Direct Ethanol Fuel Cells (DEFCs) it is necessary to develop new electrode materials or modification of the existing Pt catalysts. This work presents the electrochemical response to ethanol and CO oxidation of different compositional amorphous alloys obtained by ball milling technique, used as electrodes. Alloys with Ni{sub 59}Nb{sub 40}Pt{sub 0.6}Rh{sub 0.4} and Ni{sub 59}Nb{sub 40}Pt{sub 0.6}Rh{sub 0.2}Ru{sub 0.2} composi-tions were studied. The current density towards ethanol oxidation decreases with the presence of ruthenium; however, this electrode shows the best tolerance to CO, with lower surface coverage (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  4. Co-catalytic effect of Rh and Ru for the ethanol electro-oxidation in amorphous microparticulated alloys

    International Nuclear Information System (INIS)

    Blanco, Tamara C.; Pierna, Angel R.; Barroso, Javier

    2011-01-01

    The ethanol electro-oxidation on platinum catalyst in acid media leads to the formation of acetaldehyde and acetic acid as main products. Another problem is the poisoning of the electro-catalyst surface with CO formed during the fuel oxidation reaction. To increase the performance of Direct Ethanol Fuel Cells (DEFCs) it is necessary to develop new electrode materials or modification of the existing Pt catalysts. This work presents the electrochemical response to ethanol and CO oxidation of different compositional amorphous alloys obtained by ball milling technique, used as electrodes. Alloys with Ni 59 Nb 40 Pt 0.6 Rh 0.4 and Ni 59 Nb 40 Pt 0.6 Rh 0.2 Ru 0.2 composi-tions were studied. The current density towards ethanol oxidation decreases with the presence of ruthenium; however, this electrode shows the best tolerance to CO, with lower surface coverage (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  5. Individual ball possession in soccer.

    Directory of Open Access Journals (Sweden)

    Daniel Link

    Full Text Available This paper describes models for detecting individual and team ball possession in soccer based on position data. The types of ball possession are classified as Individual Ball Possession (IBC, Individual Ball Action (IBA, Individual Ball Control (IBC, Team Ball Possession (TBP, Team Ball Control (TBC und Team Playmaking (TPM according to different starting points and endpoints and the type of ball control involved. The machine learning approach used is able to determine how long the ball spends in the sphere of influence of a player based on the distance between the players and the ball together with their direction of motion, speed and the acceleration of the ball. The degree of ball control exhibited during this phase is classified based on the spatio-temporal configuration of the player controlling the ball, the ball itself and opposing players using a Bayesian network. The evaluation and application of this approach uses data from 60 matches in the German Bundesliga season of 2013/14, including 69,667 IBA intervals. The identification rate was F = .88 for IBA and F = .83 for IBP, and the classification rate for IBC was κ = .67. Match analysis showed the following mean values per match: TBP 56:04 ± 5:12 min, TPM 50:01 ± 7:05 min and TBC 17:49 ± 8:13 min. There were 836 ± 424 IBC intervals per match and their number was significantly reduced by -5.1% from the 1st to 2nd half. The analysis of ball possession at the player level indicates shortest accumulated IBC times for the central forwards (0:49 ± 0:43 min and the longest for goalkeepers (1:38 ± 0:58 min, central defenders (1:38 ± 1:09 min and central midfielders (1:27 ± 1:08 min. The results could improve performance analysis in soccer, help to detect match events automatically, and allow discernment of higher value tactical structures, which is based on individual ball possession.

  6. Salt Fog Testing Iron-Based Amorphous Alloys

    International Nuclear Information System (INIS)

    Rebak, Raul B.; Aprigliano, Louis F.; Day, S. Daniel; Farmer, Joseph C.

    2007-01-01

    Iron-based amorphous alloys are hard and highly corrosion resistant, which make them desirable for salt water and other applications. These alloys can be produced as powder and can be deposited as coatings on any surface that needs to be protected from the environment. It was of interest to examine the behavior of these amorphous alloys in the standard salt-fog testing ASTM B 117. Three different amorphous coating compositions were deposited on 316L SS coupons and exposed for many cycles of the salt fog test. Other common engineering alloys such as 1018 carbon steel, 316L SS and Hastelloy C-22 were also tested together with the amorphous coatings. Results show that amorphous coatings are resistant to rusting in salt fog. Partial devitrification may be responsible for isolated rust spots in one of the coatings. (authors)

  7. Magnetic interactions in high-energy ball-milled NiZnFe2O4/SiO2 composites

    International Nuclear Information System (INIS)

    Pozo Lopez, G.; Silvetti, S.P.; Urreta, S.E.; Cabanillas, E.D.

    2007-01-01

    Composites Ni 0.5 Zn 0.5 Fe 2 O 4 /SiO 2 are obtained after high-energy ball milling precursor oxides, in stoichiometric proportions, for 200 h at room temperature and further isothermal annealing for 1 h at 1273 K, under air and argon atmosphere, respectively. After 200 h grinding, a complex microstructure develops with small hematite crystals mixed with SiO 2 and remanent NiO and ZnO particles, and very small NiZn ferrite clusters, reaching a mean size of ∼9 nm. The high temperature treatments remove the hematite grains from the powder and promote the growth of NiZn ferrite grains to reach mean sizes nearly ∼20 nm. For treatments in oxidizing atmospheres, the major phases are SiO 2 and NiZn ferrite, while for annealing in Ar a new phase appears, fayalite, which is paramagnetic at room temperature. The M-H loops are all well described by the sum of a ferromagnetic and a superparamagnetic-like contribution. The observed properties are interpreted considering the different magnetic phases obtained, their crystal sizes and their mutual interactions

  8. Low-temperature MIR to submillimeter mass absorption coefficient of interstellar dust analogues. II. Mg and Fe-rich amorphous silicates

    Science.gov (United States)

    Demyk, K.; Meny, C.; Leroux, H.; Depecker, C.; Brubach, J.-B.; Roy, P.; Nayral, C.; Ojo, W.-S.; Delpech, F.

    2017-10-01

    Context. To model the cold dust emission observed in the diffuse interstellar medium, in dense molecular clouds or in cold clumps that could eventually form new stars, it is mandatory to know the physical and spectroscopic properties of this dust and to understand its emission. Aims: This work is a continuation of previous studies aiming at providing astronomers with spectroscopic data of realistic cosmic dust analogues for the interpretation of observations. The aim of the present work is to extend the range of studied analogues to iron-rich silicate dust analogues. Methods: Ferromagnesium amorphous silicate dust analogues were produced by a sol-gel method with a mean composition close to Mg1-xFexSiO3 with x = 0.1, 0.2, 0.3, 0.4. Part of each sample was annealed at 500 °C for two hours in a reducing atmosphere to modify the oxidation state of iron. We have measured the mass absorption coefficient (MAC) of these eight ferromagnesium amorphous silicate dust analogues in the spectral domain 30-1000 μm for grain temperature in the range 10-300 K and at room temperature in the 5-40 μm range. Results: The MAC of ferromagnesium samples behaves in the same way as the MAC of pure Mg-rich amorphous silicate samples. In the 30-300 K range, the MAC increases with increasing grain temperature whereas in the range 10-30 K, we do not see any change of the MAC. The MAC cannot be described by a single power law in λ- β. The MAC of the samples does not show any clear trend with the iron content. However the annealing process has, on average, an effect on the MAC that we explain by the evolution of the structure of the samples induced by the processing. The MAC of all the samples is much higher than the MAC calculated by dust models. Conclusions: The complex behavior of the MAC of amorphous silicates with wavelength and temperature is observed whatever the exact silicate composition (Mg vs. Fe amount). It is a universal characteristic of amorphous materials, and therefore of

  9. MC3T3-E1 proliferation and differentiation on biphasic mixtures of Mg substituted β-tricalcium phosphate and amorphous calcium phosphate

    International Nuclear Information System (INIS)

    Singh, Satish S.; Roy, Abhijit; Lee, Boeun E.; Banerjee, Ipsita; Kumta, Prashant N.

    2014-01-01

    A low temperature aqueous approach was used to synthesize nanocrystalline, high surface area Mg 2+ substituted β-tricalcium phosphate (β-TCMP) to assess its potential use as a synthetic bone graft substitute. X-ray diffraction indicated that β-TCMP was the predominant crystalline phase formed. However, thermal analysis revealed the presence of a secondary amorphous phase which increased with increasing Mg 2+ concentration. Further analysis by Rietveld refinement indicated that the level of ionic substitution of Ca 2+ by Mg 2+ was significantly lower than the amount of Mg 2+ measured using elemental analysis, confirming the formation of a Mg 2+ rich secondary amorphous phase. MC3T3-E1 proliferation on substrates prepared using β-TCMP was assessed using the MTT assay. In comparison to commercially available β-TCP, increased proliferation was observed on samples prepared with 50% Mg, despite elevated Mg 2+ and PO 4 3− concentrations in culture media. Alkaline phosphatase (ALP) activity and qRT-PCR were used to study the effect of varying Mg 2+ substitution on osteogenic differentiation. Cells cultured on β-TCMP substrates prepared with increased Mg 2+ concentrations expressed significantly increased levels of ALP activity and osteogenic genes such as, osteocalcin, collagen-1, and Runx2, in comparison to those cultured on commercially available β-TCP

  10. C, N co-doped TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} composite coatings prepared from TiC{sub 0.7}N{sub 0.3} powder using ball milling followed by oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Hao, Liang, E-mail: haoliang@tust.edu.cn [Tianjin Key Lab of Integrated Design and On-line Monitoring for Light Industry & Food Machinery and Equipment, Tianjin (China); College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Wang, Zhenwei, E-mail: 1004329228@qq.com [School of Naval Architecture and Ocean Engineering, Harbin Institute of Technology, Weihai, No. 2, Wenhua West Road, Weihai 264209 (China); Zheng, Yaoqing, E-mail: 13612177268@163.com [College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Li, Qianqian, E-mail: 1482471595@qq.com [College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Guan, Sujun, E-mail: sujunguan1221@gmail.com [College of Mechanical Engineering & Graduate School, Chiba University, 1-33, Yayoi-cho, Inage-ku, Chiba 263-8522 (Japan); Zhao, Qian, E-mail: zhaoqian@tust.edu.cn [Tianjin Key Lab of Integrated Design and On-line Monitoring for Light Industry & Food Machinery and Equipment, Tianjin (China); College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Cheng, Lijun, E-mail: chenglijun@tust.edu.cn [Tianjin Key Lab of Integrated Design and On-line Monitoring for Light Industry & Food Machinery and Equipment, Tianjin (China); College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Lu, Yun, E-mail: luyun@faculty.chiba-u.jp [College of Mechanical Engineering & Graduate School, Chiba University, 1-33, Yayoi-cho, Inage-ku, Chiba 263-8522 (Japan); Liu, Jizi, E-mail: jzliu@njust.edu.cn [Herbert Gleiter Institute of Nanoscience, Nanjing University of Science and Technology, No. 200, Xiaolingwei Street, Nanjing 210094 (China)

    2017-01-01

    Highlights: • TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} coatings were prepared by ball milling followed by oxidation. • In situ co-doping of C and N with simultaneous TiO{sub 2} formation was observed. • Improved photocatalytic activity under UV/visible light was noticed. • Synergism in co-doping and heterojunction formation promoted carrier separation. - Abstract: Ball milling followed by heat oxidation was used to prepared C, N co-doped TiO{sub 2} coatings on the surfaces of Al{sub 2}O{sub 3} balls from TiC{sub 0.7}N{sub 0.3} powder. The as-prepared coatings were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and ultraviolet-visible spectrophotometer (UV–vis). The results show that continuous TiC{sub 0.7}N{sub 0.3} coatings were formed after ball milling. C, N co-doped TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} composite coatings were prepared after the direct oxidization of TiC{sub 0.7}N{sub 0.3} coatings in the atmosphere. However, TiO{sub 2} was hardly formed in the surface layer of TiC{sub 0.7}N{sub 0.3} coatings within a depth less than 10 nm during the heat oxidation of TiC{sub 0.7}N{sub 0.3} coatings in carbon powder. Meanwhile, the photocatalytic activity evaluation of these coatings was conducted under the irradiation of UV and visible light. All the coatings showed photocatalytic activity in the degradation of MB no matter under the irradiation of UV or visible light. The C, N co-doped TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} composite coatings showed the most excellent performance. The enhancement under visible light irradiation should attribute to the co-doping of carbon and nitrogen, which enhances the absorption of visible light. The improvement of photocatalytic activity under UV irradiation should attribute to the synergistic effect of C, N co-doping, the formation of rutile-anatase mixed phases and the TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} composite microstructure.

  11. Assessment of heavy metals introduced into food through milling process: health implications

    International Nuclear Information System (INIS)

    Adeti, P.J.

    2015-07-01

    The present study was conducted to characterised and assesss heavy metal contamination in food through milling process and their health implications. Grinding plate made from Ghana, India and Nigeria purchased from the Ghanaian open market were used for this work. Maize from the same farm was milled into flour using the three grinding plate inserted into three different corn milling machines operating on commercial bases. Th first grinding was done immediately after the insertion of the newly sharpened plates into the machines. The plates were left for continuous daily usage. Subsequent milling of the maize was done after intervals of one month. The grinding plates and maize flour was analysed using Atomic absorption spectrophometer (AAS). The resultes recorded indicated that the heavy metals content o the Ghanaian, Indian and Nigerian made plates had the e similar metal contents but varied in terms of the individual metal concentrations. Flour from the Ghanaian made plates had the highest level of contaminants with the least from that of the Indian made plates. Generally, the highest levels of contamination were observed in the fist milling for the three plates as compared to the three subsequent milling at monthly interval. The contamination levels showed a decreasing trend from the first month (first milling ) to the fourth month (fourth milling). Cu, Cr and Ni showed concentrations above the permissible limit set by FAO/WHO in milled maize using Ghanaian made plate. Copper (Cu) recorded a concentration value between 15.04 mg/kg to 10.21mg.kg, 11.25 mg/kg to 9.13mg/kg and 10.36mg/kg and 9.68mg/kg using the Ghanaian-, Indian and Nigerian made plate respectively. Chromium (Cr) recorded a concentration between 1.51 mg/kg to 0.96 mg/kg, 1.03mg/kg to 0.91 mg/kg and 0.98mg/kg to 0.80 mg/kg using Ghanaian-, Indian and Nigerian made plates respectively. Nickel (Ni) recorded a concentration value between 23.23 mg/kg to 10.43 mg/kg, 11.46mg/kg to 10.43 mg/kg and 12.55 mg

  12. The influence of milling on the dissolution performance of simvastatin

    DEFF Research Database (Denmark)

    Zimper, Ulrike; Aaltonen, Jaakko; Krauel-Goellner, Karen

    2012-01-01

    properties such as solubility and dissolution rate and, therefore, process induced solid state modifications need to be monitored. The aim of this study was two-fold: firstly, to investigate the dissolution rates of milled and unmilled simvastatin; and secondly, to screen for the main milling factors......, as well as factor interactions in a dry ball milling process using simvastatin as model drug, and to optimize the milling procedure with regard to the opposing responses particle size and process induced disorder by application of a central composite face centered design. Particle size was assessed...... by scanning electron microscopy (SEM) and image analysis. Process induced disorder was determined by partial least squares (PLS) regression modeling of respective X-ray powder diffractograms (XRPD) and Raman spectra. Valid and significant quadratic models were built. The investigated milling factors were...

  13. Crystallization degree change of expanded graphite by milling and annealing

    International Nuclear Information System (INIS)

    Tang Qunwei; Wu Jihuai; Sun Hui; Fang Shijun

    2009-01-01

    Expanded graphite was ball milled with a planetary mill in air atmosphere, and subsequently thermal annealed. The samples were characterized by using X-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM) and thermal gravimetric analysis (TGA). It was found that in the milling initial stage (less than 12 h), the crystallization degree of the expanded graphite declined gradually, but after milling more than 16 h, a recrystallization of the expanded graphite toke place, and ordered nanoscale expanded graphite was formed gradually. In the annealing initial stage, the non-crystallization of the graphite occurred, but, beyond an annealing time, recrystallizations of the graphite arise. Higher annealing temperature supported the recrystallization. The milled and annealed expanded graphite still preserved the crystalline structure as raw material and hold high thermal stability.

  14. Hybrid ABC Optimized MARS-Based Modeling of the Milling Tool Wear from Milling Run Experimental Data

    OpenAIRE

    Garc?a Nieto, Paulino Jos?; Garc?a-Gonzalo, Esperanza; Ord??ez Gal?n, Celestino; Bernardo S?nchez, Antonio

    2016-01-01

    Milling cutters are important cutting tools used in milling machines to perform milling operations, which are prone to wear and subsequent failure. In this paper, a practical new hybrid model to predict the milling tool wear in a regular cut, as well as entry cut and exit cut, of a milling tool is proposed. The model was based on the optimization tool termed artificial bee colony (ABC) in combination with multivariate adaptive regression splines (MARS) technique. This optimization mechanism i...

  15. Influence of milling time on microstructure and magnetic properties of Fe{sub 80}P{sub 11}C{sub 9} alloy produced by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Taghvaei, A.H. [Department of Materials Science and Engineering, Shiraz University of Technology, Shiraz (Iran, Islamic Republic of); Ghajari, F., E-mail: fati.ghajari@gmail.com [Department of Materials Science and Engineering, Shiraz University, Shiraz (Iran, Islamic Republic of); Markó, D. [IFW Dresden, Institute for Complex Materials, Helmholtzstr. 20, 01069 Dresden (Germany); Prashanth, K.G. [IFW Dresden, Institute for Complex Materials, Helmholtzstr. 20, 01069 Dresden (Germany); Additive manufacturing Center, Sandvik AB, 81181 Sandviken (Sweden)

    2015-12-01

    Fe{sub 80}P{sub 11}C{sub 9} alloy with amorphous/nanocrytalline microstructure has been synthesized by mechanical alloying of the elemental powders. The microstructure, thermal behavior and morphology of the produced powders have been studied by X-ray diffraction (XRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM), respectively. The crystallite size, lattice strain and fraction of the amorphous phase have been calculated by Rietveld refinement method. The results indicate that the powders microstructure consists of α-Fe(P,C) nanocrystals with an average diameter of 9 nm±1 nm dispersed in the amorphous matrix after 90 h of milling. Moreover, the fraction of amorphous phase initially increases up to 90 h of milling and then decreases after 120 h of milling, as a result of mechanical crystallization and formation of Fe{sub 2}P phase. The magnetic measurements show that while the saturation magnetization decreases continuously with the milling time, the coercivity exhibits a complicated trend. The correlation between microstructural changes and magnetic properties has been discussed in detail. - Highlights: • Glass formation was investigated in Fe{sub 80}P{sub 11}C{sub 9} by mechanical alloying. • Structural parameters were calculated by Rietveld refinement method. • Milling first increased and then decreased the fraction of amorphous phase. • Magnetic properties were significantly changed upon milling.

  16. Facile Fabrication of 100% Bio-based and Degradable Ternary Cellulose/PHBV/PLA Composites

    Directory of Open Access Journals (Sweden)

    Tao Qiang

    2018-02-01

    Full Text Available Modifying bio-based degradable polymers such as polylactide (PLA and poly(hydroxybutyrate-co-hydroxyvalerate (PHBV with non-degradable agents will compromise the 100% degradability of their resultant composites. This work developed a facile and solvent-free route in order to fabricate 100% bio-based and degradable ternary cellulose/PHBV/PLA composite materials. The effects of ball milling on the physicochemical properties of pulp cellulose fibers, and the ball-milled cellulose particles on the morphology and mechanical properties of PHBV/PLA blends, were investigated experimentally and statistically. The results showed that more ball-milling time resulted in a smaller particle size and lower crystallinity by way of mechanical disintegration. Filling PHBV/PLA blends with the ball-milled celluloses dramatically increased the stiffness at all of the levels of particle size and filling content, and improved their elongation at the break and fracture work at certain levels of particle size and filling content. It was also found that the high filling content of the ball-milled cellulose particles was detrimental to the mechanical properties for the resultant composite materials. The ternary cellulose/PHBV/PLA composite materials have some potential applications, such as in packaging materials and automobile inner decoration parts. Furthermore, filling content contributes more to the variations of their mechanical properties than particle size does. Statistical analysis combined with experimental tests provide a new pathway to quantitatively evaluate the effects of multiple variables on a specific property, and figure out the dominant one for the resultant composite materials.

  17. Characterization of Tool Wear in High-Speed Milling of Hardened Powder Metallurgical Steels

    Directory of Open Access Journals (Sweden)

    Fritz Klocke

    2011-01-01

    Full Text Available In this experimental study, the cutting performance of ball-end mills in high-speed dry-hard milling of powder metallurgical steels was investigated. The cutting performance of the milling tools was mainly evaluated in terms of cutting length, tool wear, and cutting forces. Two different types of hardened steels were machined, the cold working steel HS 4-2-4 PM (K490 Microclean/66 HRC and the high speed steel HS 6-5-3 PM (S790 Microclean/64 HRC. The milling tests were performed at effective cutting speeds of 225, 300, and 400 m/min with a four fluted solid carbide ball-end mill (0 = 6, TiAlN coating. It was observed that by means of analytically optimised chipping parameters and increased cutting speed, the tool life can be drastically enhanced. Further, in machining the harder material HS 4-2-4 PM, the tool life is up to three times in regard to the less harder material HS 6-5-3 PM. Thus, it can be assumed that not only the hardness of the material to be machined plays a vital role for the high-speed dry-hard cutting performance, but also the microstructure and thermal characteristics of the investigated powder metallurgical steels in their hardened state.

  18. Chemical synthesis and characterization of magnesium substituted amorphous calcium phosphate (MG-ACP)

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Donghyun [Department of Biomedical Engineering, Chung-Ang University, 221 Heukseok-Dong, Dongjak-Gu, Seoul 156-756 (Korea, Republic of); Kumta, Prashant N., E-mail: pkumta@pitt.edu [Department of Bioengineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Mechanical Engineering and Materials Sceince, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Chemical and Petroleum Engineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States)

    2010-10-12

    Amorphous calcium phosphate (ACP) was synthesized by a simple aqueous precipitation using CaCl{sub 2} and Na{sub 3}PO{sub 4} in the presence of MgCl{sub 2} to ensure the formation of the ACP phase at room temperature. Magnesium substituted ACP phases corresponding to two different compositions representing the two most prominent calcium phosphate phases (hydroxyapatite: Ca + Mg/P = 1.67 and tricalcium phosphate: Ca + Mg/P = 1.5) were synthesized by this simple approach. Both compositions of ACP phases resulted in their transformation into {beta}-tricalcium phosphate upon heat treatment in air at 600 deg. C. X-ray diffraction (XRD), heat treatment, scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) and Brunauer-Emmett-Teller (BET) analyses were used to characterize the phase, thermal stability, surface area, and morphology of the synthesized ACP powders corresponding to the two different nominal Ca/P compositions. Although it is known that {alpha}-TCP is the phase that appears upon heat treatment at 600 deg. C unsubstituted ACP, substitution of magnesium ion in ACP (both TCP and HA composition) stabilized the structure of {beta}-TCMP phase at 600 deg. C. Moreover, FT-IR analysis revealed that the ACP phase regardless of the composition, exhibited characteristic bands corresponding to that of HA, with the exception of the ACP corresponding to HA composition which exhibited a prominent OH vibrational mode.

  19. Bending strength of glass-ceramics based on 3CaO.P2O5-SiO2-MgO glass system

    International Nuclear Information System (INIS)

    Daguano, J.K.M.F.; Suzuki, P.A.; Santos, C.; Fernandes, M.H.V.; Elias, C.N.

    2009-01-01

    In this work, the Modulus of Rupture of bioactive glass-ceramic based on 3CaO.P 2 O 5 -SiO 2 -MgO system was investigated, aiming its use in bone-restorations. The mechanical property was correlated with microstructural and crystallographic features of this material. High-purity starting-powders, CaCO 3 , SiO 2 , MgO, Ca (H 2 PO 4 ).H 2 O, were used in this study. The powders were mixed in a stoichiometric ratio, using planetary ball-mill. The suspensions were dried, sieved and melted at 1600 deg C, for 4h. The casting ones were cooled quickly until annealing temperature 700 deg C, in which remained for 2h, with controlled cooling-rate until ambient temperature. Bulks of glass were heat-treated with temperatures varying between 700 deg C and 1100 deg C, for 4h, being after that, cooled at 3 deg C/min. Bioactive glass and glass-ceramic were characterized by HRXRD (high resolution X-ray diffraction), where whitlockite was main phase. The microstructure was analyzed by scanning electronic microscopy. Modulus of Rupture was determined by four-point bending testing using specimens of 1.5 x 2 x 25 mm and glasses presented strength near to 70MPa, while glass ceramics treated at 975 deg C-4h, presented bending strength of 120MPa. (author)

  20. Preparation and characterisation of Co–Fe–Ni–M-Si–B (M = Zr, Ti) amorphous powders by wet mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Neamţu, B.V., E-mail: Bogdan.Neamtu@stm.utcluj.ro [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 103-105, Muncii Avenue, 400641, Cluj-Napoca (Romania); Chicinaş, H.F.; Marinca, T.F. [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 103-105, Muncii Avenue, 400641, Cluj-Napoca (Romania); Isnard, O. [Université Grenoble Alpes, Institut NEEL, F-38042, Grenoble (France); CNRS, Institut NEEL, 25 rue des martyrs, BP166, F-38042, Grenoble (France); Chicinaş, I. [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 103-105, Muncii Avenue, 400641, Cluj-Napoca (Romania)

    2016-07-15

    Co-based amorphous alloys were prepared via wet mechanical alloying process starting from elemental powders. The reference alloy Co{sub 70}Fe{sub 4}Ni{sub 2}Si{sub 15}B{sub 9} (at. %) as well as the alloys derived from this composition by the substitution of 5 at.% of Zr or Ti for Si or B (Co{sub 70}Fe{sub 4}Ni{sub 2}Si{sub 15}B{sub 4}Zr{sub 5}, Co{sub 70}Fe{sub 4}Ni{sub 2}Si{sub 15}B{sub 4}Ti{sub 5}, Co{sub 70}Fe{sub 4}Ni{sub 2}Si{sub 10}B{sub 9}Zr{sub 5} and Co{sub 70}Fe{sub 4}Ni{sub 2}Si{sub 10}B{sub 9}Ti{sub 5}) are obtained in amorphous state, according to X-ray diffraction (XRD) investigation, after 40 h of milling. The calculated amount of amorphous fraction reaches 99% after 40 h of milling. The largest increase of the crystallisation temperature was induced by the substitution of Zr or Ti for Si while, regardless of the type of substitution, an important increase of the Curie temperature of the alloy was obtained. A Co-based solid solution, with Co{sub 2}Si and Co{sub 2}B phases, result after crystallisation of the amorphous alloys as proved by XRD investigations. Saturation magnetisation of the alloys decreases upon increasing milling time, however it remains larger than the saturation magnetisation of the reference alloy. This was discussed in correlation with the specificity of the wet mechanical alloying process and the influence of the chemical bonding between Co and metalloids atoms over the magnetic moment of Co. - Highlights: • Co–Fe–Ni–M-Si–B (M = Zr, Ti) amorphous powders were prepared by wet MA. • Amorphisation of the alloy is reached after 40 h of wet MA for any composition. • Magnetisation decrease upon increasing milling time. • Substituting 5% Zr/Ti for Si increases significantly the alloy's thermal stability. • Substitution of 5 at. % Zr/Ti for Si increases the saturation magnetisation by 20%.