Sample records for vhts powder xrd

  1. Powder XRD investigations on dotriacontane in mixtures: Phase ...

    Indian Academy of Sciences (India)

    Abstract. Powder XRD investigations on dotriacontane-decane and dotriacontane-decanol mixtures are made. Phase strength, phase separation and formation of superlattices are discussed. The role of tunnel-like defects is considered.

  2. High pressure single crystal and powder XRD study for neighborite (United States)

    Liu, H.


    After Murakami et al. (2004) identified the post-perovskite (ppv) phase transition in MgSiO3 perovskite (pv) at pressures and temperatures consistent with the onset of Earth's D" layer, lots of post-perovskite type phase transitions were founded in other similar systems. These discoveries provided a better understanding of heterogeneous structures and seismic anisotropy observed in the controversial region of the lower mantle. With previous experimental evidence showing the analogue system of neighborite NaMgF3 will transform from pv to ppv at 30 GPa, we performed high quality single crystal XRD experiment, which led to a more precise structure determination. Using helium as pressure medium, one metastable low symmetric phase before the pv-ppv structure transition was discovered, whose total energy was calculated as well. The comparison between single crystal and powder XRD data will be presented, and potential application will be discussed.

  3. Determination of Size Distributions in Nanocrystalline Powders by TEM, XRD and SAXS

    DEFF Research Database (Denmark)

    Jensen, Henrik; Pedersen, Jørgen Houe; Jørgensen, Jens Erik


    Crystallite size distributions and particle size distributions were determined by TEM, XRD, and SAXS for three commercially available TiO2 samples and one homemade. The theoretical Guinier Model was fitted to the experimental data and compared to analytical expressions. Modeling of the XRD spectra...... the size distribution obtained from the XRD experiments; however, a good agreement was obtained between the two techniques. Electron microscopy, SEM and TEM, confirmed the primary particle sizes, the size distributions, and the shapes obtained by XRD and SAXS. The SSEC78 powder and the commercially...... available powders showed different morphologies. The SSEC78 powder showed the narrowest sizes distribution while UV100 and TiO2_5nm consisted of the smallest primary particles. SSEC78, UV100, and TiO2_5nm consisted of both primary particles as well as a secondary structure comprised of nanosized primary...

  4. XRD analysis and microstructure of milled and sintered V, W, C, and Co powders

    CSIR Research Space (South Africa)

    Bolokang, AS


    Full Text Available ; ? Sintering ...-1 International Journal of Refractory Metals and Hard Materials Volume 29, Issue 1, January 2011, Pages 108?111 XRD analysis and microstructure of milled and sintered V, W, C, and Co powders ? A.S. Bolokang ? M.J. Phasha ? C. Oliphant ? D. Motaung ? a...

  5. Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument (United States)

    Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.


    A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

  6. X-ray powder diffraction at the XRD1 beamline at LNLS. (United States)

    Carvalho, A M G; Araújo, D H C; Canova, H F; Rodella, C B; Barrett, D H; Cuffini, S L; Costa, R N; Nunes, R S


    Various upgrades have been completed at the XRD1 beamline at the Brazilian synchrotron light source (LNLS). The upgrades are comprehensive, with changes to both hardware and software, now allowing users of the beamline to conduct X-ray powder diffraction experiments with faster data acquisition times and improved quality. The main beamline parameters and the results obtained for different standards are presented, showing the beamline ability of performing high-quality experiments in transmission geometry. XRD1 operates in the 5.5-14 keV range and has a photon flux of 7.8 × 109 photons s-1 (with 100 mA) at 12 keV, which is one of the typical working energies. At 8 keV (the other typical working energy) the photon flux at the sample position is 3.4 × 1010 photons s-1 and the energy resolution ΔE/E = 3 × 10-4.

  7. Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD. (United States)

    Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo


    Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

  8. A Possible Path from BCS through HTS to VHTS (United States)

    Chu, C. W.


    Three years after celebrating the 50th anniversary of the BCS theory and the 20th anniversary of the discovery of high temperature superconductivity (HTS), it appears to be most fitting for us to contemplate the possibility of very high temperature superconductivity (VHTS). VHTS, preferably at room temperature, if achieved, could change the world both scientifically and technologically. Unfortunately, it has long been considered by some to belong to the domain of science fiction and to occur only ``at an astronomical distance and under an astronomical pressure.'' With the advent of liquid nitrogen superconductivity in 1987, the outlook has become much brighter. Currently, there appears to be no reason, either theoretical or experimental, why VHTS would be impossible, in spite of the 2006 prediction of the death of HTS by 2010-2015 through the so-called scientometric analysis of the publication record of the previous 20 years. The recent discovery of the new class of Fe-pnictide HTSs fuels more cautious optimism. Since its inception, BCS theory has provided the basic framework for the occurrence and understanding of superconductivity, but it has failed to show where and how to find superconductivity at a higher temperature. This may be attributed to the small energy scale of superconductivity in comparison with those of other excitations in the solids. After examining existing data, we believe that a holistic multidisciplinary enlightened empirical approach appears to be the most effective way to discover novel superconductors with higher transition temperatures. In this talk, I shall present several possible approaches toward VHTS that we are currently pursuing, after briefly summarizing what has happened in the long search for HTS and VHTS.

  9. Surface characterization of corn stalk superfine powder studied by FTIR and XRD. (United States)

    Zhao, Xiaoyan; Chen, Jun; Chen, Fengliang; Wang, Xianchang; Zhu, Qingjun; Ao, Qiang


    Corn stalk superfine powder was ground by a special designed machine. The physical-chemical properties of corn stalk powders with particle sizes of >300, 300-150, 150-74, 74-37 and particle size distributions of the powders were: d(90)=362, 147, 74, 40 and 12 μm. The size of corn stalk powders was smaller, the surface area (from 1.188 to 2.432 m(2)/g) and bulk density (from 0.103 to 0.1145 g/ml) were greater. Light microscopy (LM) and scanning electron microscopy (SEM) observations revealed the shape and surface morphology of five types of corn stalk powders. FTIR analysis showed that some position of absorbing peaks was shifted as the powder particle size decreased. X-ray diffraction analyses for corn stalk coarse and superfine powders revealed no evident changes in X-ray pattern. However, the crystallinity, intensity of crystal peaks and crystal size of corn stalk powders with particle sizes from >300 to 300-150 μm dropped, then, as the size of the powders decreased, the crystallinity, intensity of crystal peaks and crystal size increased in some degree. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Phase quantification of mullite-zirconia and zircon commercial powders using PAC and XRD techniques

    Energy Technology Data Exchange (ETDEWEB)

    Rendtorff, Nicolas M.; Conconi, Maria S.; Aglietti, Esteban F. [Centro de Tecnologia de Recursos Minerales y Ceramica (CETMIC: CONICET-CIC) (Argentina); Chain, Cecilia Y.; Pasquevich, Alberto F. [Universidad Nacional de La Plata, Departamento de Fisica, IFLP, Facultad de Ciencias Exactas (Argentina); Rivas, Patricia C. [CONICET (Argentina); Martinez, Jorge A., E-mail:; Caracoche, Maria C. [Universidad Nacional de La Plata, Departamento de Fisica, IFLP, Facultad de Ciencias Exactas (Argentina)


    The short range technique of the Perturbed Angular Correlation (PAC) and x-ray diffraction (Rietveld) methods have been employed to determine the phase content in commercial mullite-zirconia and zircon raw materials that are ordinarily used to produce ceramic materials. The PAC technique, which probes zirconium-containing compounds at nanoscopic level, showed that zircon contains crystalline ZrSiO{sub 4} and an important amount of a structurally distorted zircon, which is also observed accompanying monoclinic zirconia in mullite-zirconia. This particular zircon phase was not detected by the long range x-ray diffraction-Rietveld technique. After an annealing treatment, important changes in crystalline contents of the powders allow confirming, by the x-ray diffraction-Rietveld method, the preexistence of this particular zircon phase. This fact must be taken into account when preparing multicomposites based on the present raw materials.

  11. Use of an Ultrasonic/Sonic Driller/Corer to Obtain Sample Powder for CHEMIN, a Combined XRD/XRF Instrument (United States)

    Chipera, S. J.; Bish, D. L.; Vaniman, D. T.; Sherrit, S.; Bar-Cohen, Y.; Sarrazin, P.; Blake, D. F.


    A miniature CHEMIN XRD/XRF (X-Ray Diffraction/X-Ray Fluourescence) instrument is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed in order to enable XRD analysis on an extraterrestrial body is how best to obtain a representative sample powder for analysis. For XRD powder diffraction analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a 2-dimensional detector as used in the CHEMIN instrument will produce good results with poorly prepared powders, the quality of the data will improve if the sample is fine-grained and randomly oriented. An Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL is an effective mechanism of sampling rock to produce cores and powdered cuttings. It requires low axial load (XRF spectrometer such as CHEMIN, powders obtained from the JPL ultrasonic drill were analyzed and the results were compared to carefully prepared powders obtained using a laboratory bench scale Retsch mill.

  12. Powder XRD studies on n-C28H58: n-CxH2x (x= 10, 12, 14, 16, 18 ...

    Indian Academy of Sciences (India)

    Powder XRD investigations were made on mixtures of title compounds and strength of monoclinic, orthorhombic and super-lattice phases were evaluated. Interpretations were made in terms of the influence of tunnel-like defects (TLIDs) and a linear relationship was noticed between the strength of orthorhombic phase and ...

  13. Temperature-Induced Desorption of Methyl tert-Butyl Ether Confined on ZSM-5: An In Situ Synchrotron XRD Powder Diffraction Study

    Directory of Open Access Journals (Sweden)

    Elisa Rodeghero


    Full Text Available The temperature-induced desorption of methyl tert-butyl ether (MTBE from aqueous solutions onto hydrophobic ZSM-5 was studied by in situ synchrotron powder diffraction and chromatographic techniques. This kind of information is crucial for designing and optimizing the regeneration treatment of such zeolite. The evolution of the structural features monitored by full profile Rietveld refinements revealed that a monoclinic (P21/n to orthorhombic (Pnma phase transition occurred at about 100 °C. The MTBE desorption process caused a remarkable change in the unit-cell parameters. Complete MTBE desorption was achieved upon heating at about 250 °C. Rietveld analysis demonstrated that the desorption process occurred without any significant zeolite crystallinity loss, but with slight deformations in the channel apertures.

  14. Solid-state one-way photoisomerisation of Z,E,Z-1,6-(4,4'-diphenyl)hexa-1,3,5-triene dicarboxylate examined using higher-order derivative spectra and powder XRD patterns. (United States)

    Sonoda, Yoriko; Goto, Midori; Ichimura, Kunihiro


    Higher order derivative spectra were applied at first to one-way ZEZ-to-EEE photoisomerisation of dimethyl ester (ZEZ-DPH1) of the titled compound in a methylcyclohexane solution. Many common crossing points emerged in UV-induced derivative-spectral changes to reveal the direct ZEZ-to-EEE photoisomerisation without the transient formation of an intermediate to suggest the bicycle-pedal mechanism. The solid-state photoisomerisation was subsequently monitored by tracing changes in the fourth-order derivatives of absorption spectra of a thin crystalline layer of ZEZ-DPH1 prepared by the drop-casting method, because the distortion of absorption spectra due to light scattering is cancelled. It was suggested that the solid-state photochemical event consists of three steps: fast ZEZ-to-EEE photoisomerisation, a subsequent slow ZEZ-to-EEE photoisomerisation and very slow disappearance of the EEE-isomer. Studies on powder XRD were also carried out for a drop-cast solid layer of ZEZ-DPH1 to disclose the coexistence of a crystal form other than the original one, and the former exhibited faster ZEZ-to-EEE photoisomerisation when compared with the original crystal form. The results revealed by XRD analysis are in line with those obtained by higher-order derivative spectra, confirming the solid-state one-way photoisomerisation to take place through the bicycle-pedal process.

  15. (YSZ) powders

    Indian Academy of Sciences (India)


    XRD pattern for YSZ gel calcined at 900°C. Figure 3. Particle size distribution of the dry and wet ground slurries (20 vol.% solid content at a pH of 3). A. powder dry ground for 1 h; B, C, D, E. wet ground for 1, 2, 4, 10 h, res- pectively. Figure 4. Zeta-potential variation with pH for aqueous sus- pensions of 900°C calcined YSZ ...

  16. Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation (United States)

    Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.


    Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

  17. Green synthesis of silver nanoparticles and their characterization by XRD (United States)

    Mehta, B. K.; Chhajlani, Meenal; Shrivastava, B. D.


    A cost effective and environment friendly technique for green synthesis of silver nanoparticles has been reported. Silver nanoparticles have been synthesized using ethanol extract of fruits of Santalum album (Family Santalaceae), commonly known as East Indian sandalwood. Fruits of S.album were collected and crushed. Ethanol was added to the crushed fruits and mixture was exposed to microwave for few minutes. Extract was concentrated by Buchi rotavaporator. To this extract, 1mM aqueous solution of silver nitrate (AgNO3) was added. After about 24 hr incubation Ag+ ions in AgNO3 solution were reduced to Ag atoms by the extract. Silver nanoparticles were obtained in powder form. X-ray diffraction (XRD) pattern of the prepared sample of silver nanoparticles was recorded The diffractogram has been compared with the standard powder diffraction card of JCPDS silver file. Four peaks have been identified corresponding to (hkl) values of silver. The XRD study confirms that the resultant particles are silver nanoparticles having FCC structure. The average crystalline size D, the value of the interplanar spacing between the atoms, d, lattice constant and cell volume have been estimated. Thus, silver nanoparticles with well-defined dimensions could be synthesized by reduction of metal ions due to fruit extract of S.album.

  18. The effect of size-selective samplers (cyclones) on XRD response

    CSIR Research Space (South Africa)

    Pretorius, CJ


    Full Text Available The study evaluated five size-selective samplers used in the South African mining industry to determine how their performance affects the X-ray powder diffraction (XRD) response when respirable dust samples are analysed for quartz using direct...

  19. In situ high temperature XRD studies of ZnO nanopowder prepared ...

    Indian Academy of Sciences (India)

    This is a promising method for large area deposition at low temperature inspite of being simple, inexpensive and safe. The particle size, lattice parameters and crystal structure of ZnO nanopowder are characterized by in situ high temperature X-ray diffraction (XRD). Surface morphology of powder was studied using ...

  20. [Infrared spectroscopy and XRD studies of coral fossils]. (United States)

    Chen, Quan-li; Zhou, Guan-min; Yin, Zuo-wei


    Coral fossil is an old remain of multicellular animal on the earth, and formed by various geological processes. The structural characteristics and compositions of the coral fossils with different color and radial texture on the surface were studied by infrared absorption spectroscopy and X-ray powder diffraction analyses. The results show that the studied coral fossils mainly are composed of SiO2, and the radial microstructure characterized by the calcareous coral cross-section is preserved. It is formed by metasomatism by SiO2. The infrared absorption spectra of the coral fossil with different color and texture are essentially the same, showing typical infrared absorption spectra of the quartz jade. XRD analysis shows that the main components of the coral fossils with different color and texture are consistent and mainly composed of SiO2 with a trace amount of other minerals and without CaCO3.

  1. Síntese de ferrita NiFe2O4 e sua incorporação em compósitos de poliamida 6: Parte 1: caracterização estrutural por drx e mev dos pós e dos compósitos Synthesis of NiFe2O4 ferrite and its incorporation in nylon 6: Part 1: structural characterization by xrd and sem of ferrite powders and its composites

    Directory of Open Access Journals (Sweden)

    Daniella C. Bezerra


    Full Text Available As ferritas geralmente são absorvedoras de radiação eletromagnética e apresentam a versatilidade de poderem ser manufaturadas com geometrias diferentes, e usadas na forma de ferritas policristalinas (corpo sinterizado ou de compósitos de ferrita (adição de pó em matriz apropriada. A poliamida 6, por sua vez, pertence a uma classe de polímeros atraentes para aplicações em engenharia devido à combinação de propriedades como: estabilidade dimensional, boa resistência ao impacto sem entalhe e excelente resistência química. O objetivo deste trabalho foi sintetizar pós de ferrita NiFe2O4, e avaliar a adição destes em concentrações de 10, 30, 50 e 60% em massa a uma matriz polimérica de poliamida 6 usando um misturador da Haake Blücher, para obter compósitos de poliamida 6/NiFe2O4. Os pós e os compósitos foram caracterizados por difração de raios X (DRX e microscopia eletrônica de varredura (MEV. Os difratogramas de raios X mostraram picos característicos da poliamida 6 e da ferrita. Por MEV foi observada a formação de aglomerados grandes para a concentração de 60% e, uma grande quantidade de poros. Para a concentração de 10%, as partículas ficaram mais dispersas, com menos aglomerados e menos poros no compósito.Ferrites normally absorb electromagnetic radiation, being versatile in that they can be manufactured in different geometries and used as polycrystalline ferrites (sintered body or composites of ferrite (with addition of the powder to an appropriate matrix. On the other hand, nylon 6 is an attractive polymer for engineering applications due to the combination of properties such as dimensional stability, good impact strength without notch indentation and excellent chemical resistance. The aim of this paper was to synthesize ferrite (NiFe2O4 powders and to evaluate their addition in concentrations of 10, 30, 50 and 60 wt% into a nylon 6 polymer matrix using a Haake Blücher mixer. The powders and the

  2. Sample Handling System for in-situ Powder X-ray Diffraction Instruments. Project (United States)

    National Aeronautics and Space Administration — The proposed innovation is a Powder Handling System (PHS) that will deliver powdered samples to in situ planetary XRD instruments and provide unique means of...

  3. Composition and microstructure of MTA and Aureoseal Plus: XRF, EDS, XRD and FESEM evaluation. (United States)

    Cianconi, L; Palopoli, P; Campanella, V; Mancini, M


    The aim of this study was to determine the chemical composition and the phases' microstructure of Aureoseal Plus (OGNA, Italy) and ProRoot MTA (Dentsply Tulsa Dental, USA) and to compare their characteristics. Study Design: Comparing Aureoseal Plus and ProRoot MTA microstructure by means of several analyses type. The chemical analysis of the two cements was assessed following the UNI EN ISO 196-2 norm. X-Ray fluorescence (XRF) was used to determine the element composition. The crystalline structure was analysed quantitatively using x-ray diffraction (XRD). Powders morphology was evaluated using a scanning electron microscope (SEM) with backscattering detectors, and a field emission scanning electron microscope (FESEM). Elemental analysis was performed by energy dispersive x-ray analysis (EDS). The semi-quantitative XRF analysis showed the presence of heavy metal oxides in both cements. The XRD spectra of the two cements reported the presence of dicalcium silicate, tricalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, bismuth oxide and gypsum. SEM analysis showed that ProRoot MTA powder is less coarse and more homogeneous than Aureoseal. Both powders are formed by particles of different shapes: round, prismatic and oblong. The EDS analysis showed that some ProRoot MTA particles, differently from Aureoseal, contain Ca, Si, Al and Fe. Oblong particles in ProRoot and Aureoseal are rich of bismuth. The strong interest in developing new Portland cement-based endodontic sealers will create materials with increased handling characteristics and physicochemical properties. A thorough investigation on two cement powders was carried out by using XRF, XRD, SEM and EDS analysis. To date there was a lack of studies on Aureoseal Plus. This cement is similar in composition to ProRoot MTA. Despite that it has distinctive elements that could improve its characteristics, resulting in a good alternative to MTA.

  4. Hybrid Powder - Single Crystal X-Ray Diffraction Instrument for Planetary Mineralogical Analysis of Unprepared Samples Project (United States)

    National Aeronautics and Space Administration — We propose to develop a planetary exploration XRD/XRF instrument based on a hybrid diffraction approach that complements powder XRD analysis, similar to that of the...

  5. Application of quantitative XRD on the precipitation of struvite from Brine Water (United States)

    Heraldy, E.; Rahmawati, F.; Heryanto; Putra, D. P.


    The present studies have been conducted to quantify the varied phases in struvite formation from brine water as the magnesium source. The quantitative X-ray Diffraction (QXRD) method was performed to quantitatively determine the crystal phases and amorphous content of struvite samples. Substantial phase samples were employed quantitative analysis to calibrate against known phase composition information by Rietveld refinement on powder XRD data. The results showed that brine water could be considered as magnesium source the formation of struvite products. The study demonstrated that in general, the high N:P molar ratio (both pH 9 and 10) might lead to the significant formation of struvite.

  6. XRD total scattering of the CZTS nanoparticle absorber layer for the thin film solar cells

    DEFF Research Database (Denmark)

    Symonowicz, Joanna; Jensen, Kirsten M. Ø.; Engberg, Sara Lena Josefin

    -ray Diffraction data with X-ray total scattering with Pair Distribution Function analysis. Powder neutron diffraction will furthermore allow characterization of the cation disorder on the metal sites in the kesterite structure. The nanoparticle ink is also characterized by XRD, EDS, and Raman spectroscopy...... to revolutionize the solar energy market. However, to commercialize CZTS nanoparticle thin films, the efficiency issues must yet be resolved. In order to do so, it is vital to understand in detail their nanoscale atomic structure. CZTS crystallize in the kesterite structure, where Cu and Zn is distributed between...... the cation sites in the structure. The cation distribution affects the properties of the CZTS nanoparticles. Here, we use the hot-injection synthesis method to prepare CZTS nanoparticles of different compositions. Information on the atomic structure is obtained by combining Rietveld refinement of Powder X...

  7. Characterization of combustion synthesized zirconia powder by UV ...

    Indian Academy of Sciences (India)

    Fine powders of zirconia were prepared by employing combustion method with varying fuel to precursor molar ratios. The zirconia powders contained more amount of monoclinic phase as the fuel content was increased. This aspect was studied using XRD, IR and UV-vis diffuse reflectance techniques. The surface acidbase ...

  8. Instrumental characterization of clay by XRF, XRD and FTIR

    Indian Academy of Sciences (India)

    Instrumental characterizations of the clay were performed by different techniques such as XRF, XRD and FTIR. XRF shows the chemical compositions of the clay where Al-oxide and silica oxide are present in major quantity whereas XRD confirms the presence of these minerals in clay. FTIR studies show the presence of ...

  9. Powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Hart, M.


    the importance of x-ray powder diffraction as an analytical tool for phase identification of materials was first pointed out by Debye and Scherrer in Germany and, quite independently, by Hull in the US. Three distinct periods of evolution lead to ubiquitous application in many fields of science and technology. In the first period, until the mid-1940`s, applications were and developed covering broad categories of materials including inorganic materials, minerals, ceramics, metals, alloys, organic materials and polymers. During this formative period, the concept of quantitative phase analysis was demonstrated. In the second period there followed the blossoming of technology and commercial instruments became widely used. The history is well summarized by Parrish and by Langford and Loueer. By 1980 there were probably 10,000 powder diffractometers in routine use, making it the most widely used of all x-ray crystallographic instruments. In the third, present, period data bases became firmly established and sophisticated pattern fitting and recognition software made many aspects of powder diffraction analysis routine. High resolution, tunable powder diffractometers were developed at sources of synchrotron radiation. The tunability of the spectrum made it possible to exploit all the subtleties of x-ray spectroscopy in diffraction experiments.

  10. A coprecipitation technique to prepare ZnNb 2 O 6 powders

    Indian Academy of Sciences (India)

    ... on heating at 750°, produced ZN powders. For comparison, ZN powders were also prepared by the traditional solid state method. The phase contents and lattice parameters were studied by the powder X-ray diffraction (XRD). Particle size and morphology were studied by transmission electron spectroscopy (TEM).

  11. The Crystal Structure of Micro- and Nanopowders of ZnS Studied by EPR of Mn^sup 2+^ and XRD

    National Research Council Canada - National Science Library

    Valentyna Nosenko; Igor Vorona; Valentyn Grachev; Stanislav Ishchenko; Nikolai Baran; Yurii Becherikov; Anton Zhuk; Yuliya Polishchuk; Vasyl Kladko; Alexander Selishchev


      The crystal structure of micro- and nanopowders of ZnS doped with different impurities was analyzed by the electron paramagnetic resonance (EPR) of Mn2+ and XRD methods. The powders of ZnS:Cu, ZnS:Mn, ZnS:Co...

  12. Laboratory Detection and Analysis of Organic Compounds in Rocks Using HPLC and XRD Methods (United States)

    Dragoi, D.; Kanik, I.; Bar-Cohen, Y.; Sherrit, S.; Tsapin, A.; Kulleck, J.


    In this work we describe an analytical method for determining the presence of organic compounds in rocks, limestone, and other composite materials. Our preliminary laboratory experiments on different rocks/limestone show that the organic component in mineralogical matrices is a minor phase on order of hundreds of ppm and can be better detected using high precision liquid chromatography (HPLC). The matrix, which is the major phase, plays an important role in embedding and protecting the organic molecules from the harsh Martian environment. Some rocks bear significant amounts of amino acids therefore, it is possible to identify these phases using powder x-ray diffraction (XRD) by crystallizing the organic. The method of detection/analysis of organics, in particular amino acids, that have been associated with life will be shown in the next section.

  13. Synthesis, XRD and spectroscopic characterization of pharmacologically active Cu(II) and Zn(II) complexes (United States)

    Gull, Parveez; Hashmi, Athar Adil


    The present contribution accounts for the synthesis and structural elucidation of a newly synthesised copper and zinc containing schiff base compounds obtained by the condensation of 1, 2-diphenylethane-1, 2-dione and dinitrophenyl hydrazine as main ligand and benzene-1,2-diamine as co-ligand respectively. The synthesised compounds were characterized by several techniques, including elemental analysis, molar conductance and electronic, FT-IR, XRD, mass and 1H NMR spectral studies. The analytical and molar conductance values indicated that the complexes have square planar and tetrahedral geometry respectively. X-ray powder diffraction illustrates that they are crystalline in nature. The copper and zinc complexes were screened for their antimicrobial potential against some bacterial and fungi strains and the assay indicate that these complexes are good antimicrobial agents against these tested pathogens.

  14. Infrared spectra, Raman laser, XRD, DSC/TGA and SEM ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 34; Issue 4. Infrared spectra, Raman laser, XRD, DSC/TGA and SEM investigations on the preparations of selenium metal, (Sb2O3, Ga2O3, SnO and HgO) oxides and lead carbonate with pure grade using acetamide precursors. Moamen S Refat Khaled M Elsabawy.

  15. Conodont bioapatite resembles vertebrate enamel by XRD properties

    Directory of Open Access Journals (Sweden)

    Jüri Nemliher


    Full Text Available XRD properties of Phanerozoic conodont apatite material were studied. It was found out that in terms of crystallinity the apatite resembles the enamel tissue of modern vertebrates. In terms of crystal lattice, apatite of conodonts is independent of taxa on the one hand and of chemistry of the surrounding rock type on the other hand.

  16. XRD and FTIR structural investigation of gadolinium-zinc-borate glass ceramics (United States)

    Borodi, G.; Pascuta, P.; Stefan, R.; Dan, V.; Pop, V.; Radulescu, D.


    X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy measurements have been employed to investigate the (Gd2O3)xṡ(B2O3)(60-x)ṡ(ZnO)40 glass ceramics system, with 0 ≤ x ≤ 15 mol%. After heat treatment applied at 860 °C for 2 h, some structural changes were observed and new crystalline phases appeared in the structure of the samples. In these glass ceramics four crystalline phases were identified using powder diffraction files (PDF 2), namely ZnB4O7, Zn4O(B6O12), Zn3(BO3)2 and GdBO3. From the XRD data, the average unit-cell parameter and the quantitative ratio of the crystallographic phases in the studied samples were evaluated. FTIR data revealed that the BO3, BO4 and ZnO4 are the main structural units of these glass ceramics network. The compositional dependence of the different structural units which appear in the studied samples was followed.

  17. Talcum powder poisoning (United States)

    ... better the chance for recovery. Breathing in talcum powder can lead to very serious lung problems, even death. Use caution when using talcum powder on babies. Talc-free baby powder products are ...

  18. Synthesis of Cu-coated Graphite Powders Using a Chemical Reaction Process

    Energy Technology Data Exchange (ETDEWEB)

    Jang, Jun-Ho; Park, Hyun-Kuk; Oh, Ik-Hyun [Korea Institute of Industrial Technology (KITECH), Gwangju (Korea, Republic of); Lim, Jae-Won [Chonbuk National University, Jeonju (Korea, Republic of)


    In this paper, Cu-coated graphite powders for a low thermal expansion coefficient and a high thermal conductivity are fabricated using a chemical reaction process. The Cu particles adhere to the irregular graphite powders and they homogeneously disperse in the graphite matrix. Cu-coated graphite powders are coarser at approximately 3-4 μm than the initial graphite powders; furthermore, their XRD patterns exhibit a low intensity in the oxide peak with low Zn powder content. For the passivation powders, the transposition solvent content has low values, and the XRD pattern of the oxide peaks is almost non-existent, but the high transposition solvent content does not exhibit a difference to the non-passivation treated powders.

  19. Resin-Powder Dispenser (United States)

    Standfield, Clarence E.


    Resin-powder dispenser used at NASA's Langley Research Center for processing of composite-material prepregs. Dispenser evenly distributes powder (resin polymer and other matrix materials in powder form) onto wet uncured prepregs. Provides versatility in distribution of solid resin in prepreg operation. Used wherever there is requirement for even, continuous distribution of small amount of powder.

  20. Comparison of the mechanically alloyed (V,W)C and (V,W)C-co powders

    CSIR Research Space (South Africa)

    Bolokang, AS


    Full Text Available in XRD patterns because they were of extremely fine grain size.As a result of the loss ofVandWthrough oxidation, free carbonwas also found in the final powder. The lattice parameter of the (V,W)C powder increased with milling time up to a maximum...

  1. Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: Spectral, thermal, XRD and antimicrobial studies (United States)

    Sundararajan, M. L.; Jeyakumar, T.; Anandakumaran, J.; Karpanai Selvan, B.


    Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, 1H NMR, 13C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, 1H NMR, 13C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base.

  2. Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: spectral, thermal, XRD and antimicrobial studies. (United States)

    Sundararajan, M L; Jeyakumar, T; Anandakumaran, J; Karpanai Selvan, B


    Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, (1)H NMR, (13)C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, (1)H NMR, (13)C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. A Combined XRD/XRF Instrument for Lunar Resource Assessment (United States)

    Vaniman, D. T.; Bish, D. L.; Chipera, S. J.; Blacic, J. D.


    Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of

  4. Production of Dense Compact Billet From Ti-Alloy Powder Using Equal Channel Angular Extrusion (United States)


    b) Fig. 5 Images of as-received Ti6Al4V powder (a) Scanning Electron...XRD analysis of Ti6Al4V powder showing peaks of α and ß-Ti. Fig. 7 TEM micrographs of as-received Ti...of as-received Ti6Al4V powder. 10 4.2 Experimental Techniques ECAE with back pressure was performed using a specially designed unit

  5. Recovery Of Electrodic Powder From Spent Lithium Ion Batteries (LIBs

    Directory of Open Access Journals (Sweden)

    Shin S.M.


    Full Text Available This study was focused on recycling process newly proposed to recover electrodic powder enriched in cobalt (Co and lithium (Li from spent lithium ion battery. In addition, this new process was designed to prevent explosion of batteries during thermal treatment under inert atmosphere. Spent lithium ion batteries (LIBs were heated over the range of 300°C to 600°C for 2 hours and each component was completely separated inside reactor after experiment. Electrodic powder was successfully recovered from bulk components containing several pieces of metals through sieving operation. The electrodic powder obtained was examined by X-ray diffraction (XRD, energy dispersive X-ray spectroscopy (EDS, and atomic absorption spectroscopy (AA and furthermore image of the powder was taken by scanning electron microscopy (SEM. It was finally found that cobalt and lithium were mainly recovered to about 49 wt.% and 4 wt.% in electrodic powder, respectively.



  7. The effect of concentration of glycerol and electric current on the morphology and particle size of electrodeposited cadmium powder

    Directory of Open Access Journals (Sweden)

    S. G. Viswanath


    Full Text Available Cadmium powder was obtained by electrodeposition of cadmium from glycerol and sulphuric acid. The morphology and particle size of these powders were studied. Broken dendrites, intermingled with spongy and irregular particles were observed in the powder. Around 60% of particles were below 100 µm. XRD studies showed that particles with sizes between 212.2 and 303.2 nm were present in the powder. The apparent density of cadmium powder decreased with increase in concentration of glycerol. The stability of the powder and current efficiency were also studied

  8. Aluminum powder metallurgy processing

    Energy Technology Data Exchange (ETDEWEB)

    Flumerfelt, J.F.


    The objective of this dissertation is to explore the hypothesis that there is a strong linkage between gas atomization processing conditions, as-atomized aluminum powder characteristics, and the consolidation methodology required to make components from aluminum powder. The hypothesis was tested with pure aluminum powders produced by commercial air atomization, commercial inert gas atomization, and gas atomization reaction synthesis (GARS). A comparison of the GARS aluminum powders with the commercial aluminum powders showed the former to exhibit superior powder characteristics. The powders were compared in terms of size and shape, bulk chemistry, surface oxide chemistry and structure, and oxide film thickness. Minimum explosive concentration measurements assessed the dependence of explosibility hazard on surface area, oxide film thickness, and gas atomization processing conditions. The GARS aluminum powders were exposed to different relative humidity levels, demonstrating the effect of atmospheric conditions on post-atomization processing conditions. The GARS aluminum powders were exposed to different relative humidity levels, demonstrating the effect of atmospheric conditions on post-atomization oxidation of aluminum powder. An Al-Ti-Y GARS alloy exposed in ambient air at different temperatures revealed the effect of reactive alloy elements on post-atomization powder oxidation. The pure aluminum powders were consolidated by two different routes, a conventional consolidation process for fabricating aerospace components with aluminum powder and a proposed alternative. The consolidation procedures were compared by evaluating the consolidated microstructures and the corresponding mechanical properties. A low temperature solid state sintering experiment demonstrated that tap densified GARS aluminum powders can form sintering necks between contacting powder particles, unlike the total resistance to sintering of commercial air atomization aluminum powder.

  9. Chemical characterization of selected high copper dental amalgams using XPS and XRD techniques

    Energy Technology Data Exchange (ETDEWEB)

    Talik, E. [A. Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland)]. E-mail:; Babiarz-Zdyb, R. [A. Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Dziedzic, A. [Medical University of Silesia, Department of Conservative Dentistry and Periodontology, Akademicki 17 Sqr., 41-209 Bytom (Poland)


    The study was carried out to analyze some dependencies between the composition of seven high copper dental amalgams and mercury release behavior, as well as oxygen reactivity of metallic elements. Chemical comparative analysis of selected dental amalgams was carried out using X-ray photoelectron spectroscopy (XPS) technique and X-ray diffraction (XRD) method. The X-ray powder diffraction measurements revealed two main phases for measured amalgams: {gamma}{sub 1}-(Ag{sub 2}Hg{sub 3}) and {eta}'-(Cu{sub 6}Sn{sub 5}). The amount of mercury obtained by the XPS method was lower than the value quoted in the manufacturer's literature, which suggested evaporation of mercury under the UHV conditions. A linear decrease of oxygen and carbon contamination with the growing amount of Cu and Ag was observed. The XPS analysis showed that a high Sn concentration caused less resistance to oxidation. Some of the amalgams contained some extra elements, such as Bi, In, and Zn. All samples contained lead in metallic state and oxides. The amount of Ag, Cu, Sn ingredients determines the main properties of high copper amalgams and plays an important role in mercury evaporation. High tin concentration combined with the presence of smaller amounts of silver and copper (high Sn/Ag ratio) may influence the increase of mercury vaporization.

  10. Mirrored low-energy channel for the MiniXRD

    Energy Technology Data Exchange (ETDEWEB)

    Dutra, Eric [National Security Technologies, LLC. (NSTec), Mercury, NV (United States); MacNeil, Lawrence [National Security Technologies, LLC. (NSTec), Mercury, NV (United States); Raphaelian, Mark [National Security Technologies, LLC. (NSTec), Mercury, NV (United States); Compton, Steve; Jacoby, Barry


    X-ray Diodes (XRDs) are currently used for spectroscopic measurements, measuring X-ray flux, and estimating spectral shape of the VUV to soft X-ray spectrum. A niche exists for an inexpensive, robust X-ray diode that can be used for experiments in hostile environments on multiple platforms, including explosively driven experiments that have the potential for destroying the diode during the experiment. A multiple channel stacked filtered array was developed with a small field of view where a wider parallel array could not be used, but filtered channels for energies lower than 1000 eV were too fragile to deploy under normal conditions. To achieve both the robustness and the required low-energy detection ability, the researchers designed a small low-energy mirrored channel with a spectral sensitivity from 30 to 1000 eV. The stacked MiniXRD X-ray diode system design incorporates the mirrored low-energy channel on the front of the stacked filtered channels to allow the system to work within a small field of view. We will present results that demonstrate this is a promising solution for low-energy spectrum measurements.

  11. Borax as a lubricant in powder metallurgy

    Directory of Open Access Journals (Sweden)

    Héctor Geovanny Ariza-Suarez


    were compacted at 700 MPa in a uniaxial press of 15 tons. DSC-TGA analysis of the mixture with borax was realized. The specimens were sintered in a plasma reactor at 1000 for 30 minutes, with a combined atmosphere of hydrogen and argon. Microhardness and density of the sintered samples was haracterized. XRD analysis was realized to detect possible compounds formation by interaction of borax. This paper shows that borax can be used as a lubricant in powder metallurgy.

  12. The effect of precursor powder size on the microstructure and integranular properties of Bi2223 superconductors

    Directory of Open Access Journals (Sweden)

    I. Abdolhosseini


    Full Text Available  We have studied the effect of precursor powder size on the microstructure and intergranular behavior of polycrystalline Bi2223 superconductors using the XRD, SEM, electrical resistivity and AC susceptibility techniques. Polycrystalline Bi2223 superconductors were prepared from the powders with different milling times. The XRD results show that by decreasing the precursor powder size the Bi2223 phase fraction increases. It was found that the grain size and grain connectivity improved by decreasing the precursor powder size. Analysis of the temperature dependence of the AC susceptibility near the transition temperature (Tc has been done employing Beans critical state model. The observed variation of intergranular critical current densities (Jc with temperature indicates that the decreasing of precursor powder size in the Bi2223 system cases an increase in the intergranular critical current density.

  13. XRD and XPS characterisation of transition metal silicide thin films (United States)

    Tam, P. L.; Cao, Y.; Nyborg, L.


    Binary transition metal silicides based on the systems Ti-Si, Fe-Si, Ni-Si and Cr-Si were fabricated on Si wafers by means of ion-beam co-sputter deposition and subsequent annealing. The crystalline structures of the phases formed were identified from the characteristic patterns acquired by means of X-ray diffraction (XRD) measurements. The phase formation sequences were described by means of the Pretorius' effective heat of formation (EHF) model. For the Ti-Si, Fe-Si and Ni-Si systems, single phase thin films of TiSi2, β-FeSi2 and NiSi2 were generated as the model predicts, while a mixture of CrSi + CrSi2 phases was obtained for the Cr-Si system. The surface chemical condition of individual specimens was analysed by using X-ray photoelectron spectroscopy (XPS). The chemical shifts of transition metal 2p3/2 peaks from their metallic to silicide states were depicted by means of the Auger parameters and the Wagner plots. The positive chemical shift of 2.0 eV for Ni 2p3/2 peak of NiSi2 is mainly governed by the initial-state effects. For the other silicide specimens, the initial-state and final-state effects may oppose one another with similar impact. Consequently, smaller binding energy shifts of both negative and positive character are noted; a positive binding energy shift of 0.3 eV for the Fe 2p3/2 level was shown for β-FeSi2 and negative binding energy shifts of 0.1 and 0.3 eV were determined for CrSi + CrSi2 and TiSi2, respectively.

  14. Titanium Powder Metallurgy Forgings. (United States)


  15. XRD and FTIR study of the effect of ultra high molecular weight polyethylene (UHMWPE) as binder on kaolin geopolymer ceramics (United States)

    Ahmad, R.; Abdullah, Mohd Mustafa Al Bakri; Hussin, K.; Sandu, A. V.


    The effect of addition of Ultra High Molecular Weight Polyethylene (UHMWPE) as binder on Kaolin Geopolymer Ceramics was study using infrared spectroscopy (FTIR) and X-ray diffraction (XRD) method. UHMWPE is added to the optimum kaolin geopolymer ceramics that obtained by mechanical performance, phase and microstructure analysis with the concentration of NaOH, solid/liquid and Na2SiO3/NaOH ratio of 12 M, 1.0 and 0.24 respectively. Kaolin geopolymer powders with addition of Ultra High Molecular Weight Polyethylene content of 2, 4, 6 and 8 (wt. %) were pressed into pellets followed by sintering at 1200 °C. At this temperature, the amorphous phase of geopolymer were fully crystallized. The results obtained by the XRD testing confirm that amorphous geopolymer transform to crystalline nepheline ceramics upon heating. The phase analysis for Kaolin geopolymer ceramics with addition of UHMWPE are similar to the kaolin geopolymer ceramics without UHMWPE indicates that the incorporation of a little amount of UHMWPE does not affect the structure feature of geopolymer. The increasing in intensity of nepheline peak contribute to high strength. The FTIR spectra showed the disappearance of water band after sinter at high temperature.

  16. Sinterability and microstructure evolution during sintering of ferrous powder mixtures

    Directory of Open Access Journals (Sweden)

    Kétner Bendo Demétrio


    Full Text Available The present work is focused on ferrous powder metallurgy and presents some results of a development of a suitable masteralloy for use as an additive to iron powder for the production of sintered steels. The masteralloy was produced by melting a powder mixture containing approximately Fe + 20% Ni + 20% Mn + 20% Si + 1% C (wt%, in order to obtain a cast billet that was converted into fine powder by crushing and milling. It was observed presence of SiC in the masteralloy after melting that is undesirable in the alloy. Si element should be introduced by using ferrosilicon. Sintered alloys with distinct contents of alloying elements were prepared by mixing the masteralloy powder to plain iron powder. Samples were produced by die compaction of the powder mixtures and sintering at 1200 °C in a differential dilatometer in order to record their linear dimensional behaviour during heating up and isothermal sintering, aiming at studying the sinterability of the compacts. Microstructure development during sintering was studied by SEM, XRD and microprobe analyses.

  17. Structural studies of carbon nanotubes by powder x-ray diffraction at SPring-8 and KEK PF

    CERN Document Server

    Maniwa, Y; Fujiwara, A


    Powder X-ray diffraction (XRD) studies on carbon nanotubes (CNTs) using synchrotron radiation are reported. In spite of the observed broad XRD peak profiles of two-dimensional triangular (hexagonal) lattice of single-wall carbon nanotubes (SWNTs), it was shown that useful structural information, such as the tube diameter and its distribution, can be deduced from detailed analysis of the characteristic XRD patterns. In particular, powder-XRD measurements were performed to study the phase transition of encapsulated materials inside SWNTs. In the C sub 7 sub 0 -one dimensional (1D) crystals formed inside SWNTs, importance of one-dimensionality in the C sub 7 sub 0 -molecular dynamics was suggested. It was also shown that water inside SWNTs undergoes a phase transition from liquid to an ice-nanotube structure below -38degC. Conversion process from SWNT to double-wall carbon nanotube (DWNT) was also studied by XRD.

  18. Compaction of Titanium Powders

    Energy Technology Data Exchange (ETDEWEB)

    Stephen J. Gerdemann; Paul D. Jablonski


    Accurate modeling of powder densification has been an area of active research for more than 60 years. The earliest efforts were focused on linearization of the data because computers were not readily available to assist with curve-fitting methods. In this work, eight different titanium powders (three different sizes of sponge fines <150 μm, <75 μm, and < 45 μm; two different sizes of a hydride-dehydride [HDH] <75 μm and < 45 μm; an atomized powder; a commercially pure [CP] Ti powder from International Titanium Powder [ITP]; and a Ti 6 4 alloy powder) were cold pressed in a single-acting die instrumented to collect stress and deformation data during compaction. From these data, the density of each compact was calculated and then plotted as a function of pressure. The results show that densification of all the powders, regardless of particle size, shape, or chemistry, can be modeled accurately as the sum of an initial density plus the sum of a rearrangement term and a work-hardening term. These last two terms are found to be a function of applied pressure and take the form of an exponential rise.

  19. Compaction of Titanium Powders

    Energy Technology Data Exchange (ETDEWEB)

    Gerdemann, Stephen,J; Jablonski, Paul, J


    Accurate modeling of powder densification has been an area of active research for more than 60 years. The earliest efforts were focused on linearization of the data because computers were not readily available to assist with curve-fitting methods. In this work, eight different titanium powders (three different sizes of sponge fines<150 {micro}m,<75 {micro}m, and<45 {micro}m; two different sizes of a hydride-dehydride [HDH]<75 {micro}m and<45 {micro}m; an atomized powder; a commercially pure [CP] Ti powder from International Titanium Powder [ITP]; and a Ti 6 4 alloy powder) were cold pressed in a single-acting die instrumented to collect stress and deformation data during compaction. From these data, the density of each compact was calculated and then plotted as a function of pressure. The results show that densification of all the powders, regardless of particle size, shape, or chemistry, can be modeled accurately as the sum of an initial density plus the sum of a rearrangement term and a work-hardening term. These last two terms are found to be a function of applied pressure and take the form of an exponential rise.

  20. Low temperature synthesis of magnesium oxide and spinel powders by a sol-gel process

    Directory of Open Access Journals (Sweden)

    Li-Zhai Pei


    Full Text Available Magnesium oxide and magnesium aluminate (MgAl2O4 spinel (MAS powders have been synthesized by a simple aqueous sol-gel process using citrate polymeric precursors derived from magnesium chloride, aluminium nitrate and citrate. The thermal decomposition of the precursors and subsequent formation of cubic MgO and MAS were investigated by X-ray diffraction (XRD, scanning electron microscopy (SEM, thermogravimetry-differential scanning calorimetry (TG-DSC and Fourier transform infrared spectra (FTIR. The single phase cubic MgO powder and MAS powder form after heat treatment at 800 and 1200 °C, respectively. The particle size of the MgO and MAS powders is about 100 nm and several micrometers, respectively. Ball milling eliminates the size of MgO and MgAl2O4 spinel powders by decreasing the conglomeration of the powders.

  1. Waste Fiber Powder Functionalized with Silver Nanoprism for Enhanced Raman Scattering Analysis


    Tang, Bin; Zeng, Tian; Liu, Jun; Zhou, Ji; Ye, Yong; Wang, Xungai


    Biomass disks based on fine powder produced from disposed wool fibers were prepared for surface-enhanced Raman scattering (SERS). The wool powders (WPs) were modified by silver nanoprisms via an assembly method and then pressed into disks using a hydraulic laboratory pellet press. Scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were used to characterize the WPs and disks before and after treatment with silver nanoparticles (AgNPs). The W...

  2. Powder Diffraction: By Decades (United States)

    David, William I. F.

    This introductory chapter reviews the first 100 years of powder diffraction, decade by decade, from the earliest X-ray powder diffraction measurements of the crystal structure of graphite through to the diversity and complexity of twenty-first century powder diffraction. Carbon features as an illustrative example throughout the discussion of these ten decades from graphite and the disorder of carbon black through to lonsdaleite, the elusive hexagonal polymorph of diamond, and C60, the most symmetrical of molecules. Electronics and computing have played a leading role in the development of powder diffraction, particularly over the past 60 years, and the Moore's Law decade-by-decade rise in computing power is clear in the increasing complexity of powder diffraction experiments and material systems that can be studied. The chapter concludes with a final discussion of decades - the four decades of length-scale from the ångstrom to the micron that not only represent the domain of powder diffraction but are also the distances that will dominate twenty-first century science and technology.

  3. Biaxially textured articles formed by powder metallurgy (United States)

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.


    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100} orientation texture; and further having a Curie temperature less than that of pure Ni.

  4. Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF (United States)

    Blake, D. F.; Bish, D.; Vaniman, D.; Chipera, S.; Sarrazin, P.; Collins, S. A.; Elliott, S. T.


    X-Ray Diffraction (XRD) is the most direct and accurate method for determining mineralogy. The CHEMIN XRD/XRF instrument has shown promising results on a variety of mineral and rock samples. Additional information is contained in the original extended abstract.

  5. On iron contamination in mechanically alloyed Cr-Si powders

    Energy Technology Data Exchange (ETDEWEB)

    Fernandes, Bruno B. [Universidade do Vale do Paraiba, Instituto de Pesquisa e Desenvolvimento, Sao Jose dos, Campos-SP, CEP 12244-000 (Brazil); Rodrigues, Geovani [Faculdade de Engenharia Quimica de Lorena, Departamento de Engenharia de Materiais, Caixa Postal 116, Lorena-SP, CEP 12600-970 (Brazil); Coelho, Gilberto C. [Faculdade de Engenharia Quimica de Lorena, Departamento de Engenharia de Materiais, Caixa Postal 116, Lorena-SP, CEP 12600-970 (Brazil); Ramos, Alfeu S. [Universidade do Vale do Paraiba, Instituto de Pesquisa e Desenvolvimento, Sao Jose dos, Campos-SP, CEP 12244-000 (Brazil)]. E-mail:


    The present work reports on iron contamination and phase transformation during high-energy ball milling from high-purity elemental powder Cr-25Si, Cr-37.5Si, Cr-50Si, and Cr-66Si mixtures (at%) and their subsequent heat treatment. Samples were characterized in the as-milled state as well as after heat treatment by X-ray diffraction (XRD), scanning electron microscopy (SEM), and microanalysis via energy dispersive spectrometry (EDS). Only Cr peaks were observed in Cr-25Si and Cr-37.5Si powders after milling for 200 h, suggesting that amorphous phases can be formed. In Cr-50Si and Cr-66Si powders, the CrSi and CrSi{sub 2} phases were formed during ball milling, respectively. In Cr-25Si and Cr-50Si milled powders, heat-treated at 1200 deg. C for 4 h, the formation of the Cr{sub 3}Si and CrSi phases dissolving up to 15 and 16.9 at%Fe, respectively, was noted. In addition, the ternary Cr{sub 9}Fe{sub 9}Si{sub 2} phase was also formed in heat-treated Cr-25Si powders. A small amount of Cr{sub 5}Si{sub 3} and CrSi{sub 2} was formed in heat-treated Cr-37.5Si and Cr-66Si powders, respectively.

  6. The structural properties of barium cobalt hexaferrite powder prepared by a simple heat treatment method

    Energy Technology Data Exchange (ETDEWEB)

    Chauhan, Chetna, E-mail: [Electrical Engineering Department, Institute of Technology, Nirma University, Ahmedabad-382 481. Gujarat. India (India); Jotania, Rajshree, E-mail: [Department of Physics, University School of Sciences, Gujarat University, Ahmeabad – 380009. Gujarat. India (India)


    The W-type barium hexaferrite was prepared using a simple heat treatment method. The precursor was calcinated at 650°C for 3 hours and then slowly cooled to room temperature in order to obtain barium cobalt hexaferrite powder. The prepared powder was characterised by different experimental techniques like XRD, FTIR and SEM. The X-ray diffractogram of the sample shows W-and M phases. The particle size calculated by Debye Scherrer formula. The FTIR spectra of the sample was taken at room temperature by using KBr pallet method which confirms the formation of hexaferrite phase. The morphological study on the hexaferrite powder was carried out by SEM analysis.

  7. The structural properties of barium cobalt hexaferrite powder prepared by a simple heat treatment method (United States)

    Chauhan, Chetna; Jotania, Rajshree


    The W-type barium hexaferrite was prepared using a simple heat treatment method. The precursor was calcinated at 650°C for 3 hours and then slowly cooled to room temperature in order to obtain barium cobalt hexaferrite powder. The prepared powder was characterised by different experimental techniques like XRD, FTIR and SEM. The X-ray diffractogram of the sample shows W-and M phases. The particle size calculated by Debye Scherrer formula. The FTIR spectra of the sample was taken at room temperature by using KBr pallet method which confirms the formation of hexaferrite phase. The morphological study on the hexaferrite powder was carried out by SEM analysis.

  8. Chemical synthesis of hollow sea urchin like nanostructured polypyrrole particles through a core-shell redox mechanism using a MnO2 powder as oxidizing agent and sacrificial nanostructured template


    Benhaddad, Lynda; Bernard, Marie-Claude; Deslouis, Claude; Makhloufi, Laid; Messaoudi, Bouzid; Pailleret, Alain; Takenouti, Hisasi


    International audience; Hollow sea urchin shaped nanostructured polypyrrole powder was successfully synthesized chemically in an acidic medium through a core-shell redox mechanism by using a nanostructured MnO2 powder as oxidizing agent and sacrificial template simultaneously. The morphology and the structure of MnO2 powder based reactant and produced polypyrrole powder were characterized respectively by using FEG-SEM, TEM, EDX and XRD techniques, which led us to demonstrate clearly the forma...

  9. A coprecipitation technique to prepare ZnNb2O6 powders

    Indian Academy of Sciences (India)


    were also prepared by the traditional solid state method. The phase contents and lattice parameters were studied by the powder X-ray diffraction (XRD). Particle size and morphology were studied by transmission electron spectroscopy (TEM). Keywords. Ceramics; electronic materials; electron microscopy; X-ray diffraction.

  10. Preparation of ultrafine LiTaO 3 powders by citrate gel method

    Indian Academy of Sciences (India)

    ... stoichiometric ratio was heated in a water bath. This gel on decomposition at 700°C produced fine crystallites of ternary oxide, LiTaO3 (LT). The phase contents and lattice parameters were studied by powder X-ray diffraction (XRD). Particle size and morphology were studied by transmission electron spectroscopy (TEM).

  11. Mineralogical Composition of the Mexican Ordinary Chondrite Type Meteorite: A Raman, Infrared and XRD Study (United States)

    Ostrooumov, M.


    The Raman microprobe (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of seven mexican meteorites: Aldama, Cosina, El Pozo, Escalon, Nuevo Mercurio,Pacula, Zapotitlan Salinas.

  12. Karakteristik Beberapa Jenis Antibiotik Berdasarkan Pola Difraksi Sinar-X (XRD Dan Spektrum FTIR

    Directory of Open Access Journals (Sweden)

    Mirzan T Razzak


    Full Text Available Telah dilakukan pengukuran karakteristik difraksi sinar-x (XRD terhadap beberapa jenisantibiotik. Penelitian ini bertujuan untuk memahami karakteristik difraksi sinar-x suatuantibiotik sebagai upaya untuk identifikasi antibiotik secara cepat. Dalam penelitian ini diamatikarakteristik difraksi sinar-x dari 15 (lima belas antibiotik yang tersedia di pasaran. SpektrumXRD diukur pada sudut 2 antara 5 – 75 untuk dibandingkan dan dievaluasi mengenai bentukkristalnya. Selanjutnya diukur pula spektrum XRD dari pencampuran antibiotik dengan tepungtapioka. Pengukuran spektrum infrared dengan FTIR juga dilakukan untuk menguji konsistensihasil evaluasi spektrum XRD. Hasil penelitian menunjukkan bahwa amoxicillin dan ampicillinmempunyai struktur kristal yang sama, yaitu orthorombic primitif. Sayangnya baik XRDmaupun FTIR, tidak memberikan nilai kuantitatif pada antibiotik. Oleh sebab itu, perbedaankonsentrasi dengan pencampuran tepung tapioka tidak dapat dideteksi. Walaupun demikian,metode ini terbukti dapat digunakan untuk membedakan komposisi zat penyusun antibiotiksecara cepat dan akurat.

  13. Demystifying Mystery Powders. (United States)

    Kotar, Michael


    Describes science activities which use simple chemical tests to distinguish between materials and to determine some of their properties. Explains the water, iodine, heat, acid, baking soda, acid/base indicator, glucose, and sugar tests. Includes activities to enhance chemical testing and a list of suggested powders for use. (RT)

  14. Photocatalytic and antibacterial activity of ZnO powders prepared via sol-gel method

    Directory of Open Access Journals (Sweden)

    Weerachai Sangchay


    Full Text Available We report on synthesis of ZnO powders via sol-gel method. The prepared powders were calcined at the temperature of 300, 500 and 700°C for 1 h with the heating rate of 10°C/min. The microstructures of the fabricated powders were characterized by SEM and XRD techniques, and the results show that all samples were the agglomeration and spherical shape and reveal only the wurtzite phase. The photocatalytic activities of the powders were also tested via the degradation of methylene blue (MB solution under UV irradiation. Finally, antibacterial activity efficiency was evaluated by the inactivation of E. coli. It was observed that higher calcined at the temperature gives better photocatalytic and antibacterial activity. With the highest calcined at the temperature investigated in this experiment (T700 condition the powders show photocatalytic and antibacterial activities of 80.06 and 99.00%, respectively.

  15. Recovery Of Electrodic Powder From Spent Nickel-Metal Hydride Batteries (NiMH

    Directory of Open Access Journals (Sweden)

    Shin S.M.


    Full Text Available This study was focused on recycling process newly proposed to recover electrodic powder enriched in nickel (Ni and rare earth elements (La and Ce from spent nickel-metal hydride batteries (NiMH. In addition, this new process was designed to prevent explosion of batteries during thermal treatment under inert atmosphere. Spent nickel metal hydride batteries were heated over range of 300°C to 600°C for 2 hours and each component was completely separated inside reactor after experiment. Electrodic powder was successfully recovered from bulk components containing several pieces of metals through sieving operation. The electrodic powder obtained was examined by X-ray diffraction (XRD and energy dispersive X-ray spectroscopy (EDX and image of the powder was taken by scanning electron microscopy (SEM. It was finally found that nickel and rare earth elements were mainly recovered to about 45 wt.% and 12 wt.% in electrodic powder, respectively.

  16. Rietveld refinement on XRD and TEM study of nanocrystalline PbZr0:5Ti0:5O3 ceramics prepared with a soft chemistry route

    Directory of Open Access Journals (Sweden)

    Mandal T.K.


    Full Text Available PbZr0:5Ti0:5O3 nanopowders (~27 nm have been prepared by a controlled reconstructive thermal decomposition and crystallization from an amorphous polymeric precursor with polyvinyl alcohol (PVA and sucrose at 400 to 700 °C in air. The Rietveld refinement of the XRD profiles which were recorded at room temperature for the PbZr0:5Ti0:5O3 powder prepared by a thermal treatment at 700 °C for 2 h, confirmed the P4mm tetragonal crystal structure of the as prepared PbZr0:5Ti0:5O3 nanopowders, with a = 0.4036 nm and c = 0.4147 nm. A hexagonal symmetry (R3c, with a = 0.5774 nm and c = 1.4212 nm, was also detected from Rietveld refinement analysis. Thus, tetragonal and hexagonal phases were found to coexist with the as prepared PbZr0:5Ti0:5O3 nanopowders. The average particle size (D of the PbZr0:5Ti0:5O3 powders, estimated with the help of the specific surface area, measured by BET method, was 26.1 nm. Average D value, calculated by D2θ1/2 in the XRD peaks with the Debye-Scherrer relation was ~24 nm. TEM study made it possible to measure the particle size of PbZr0:5Ti0:5O3 powders with an average diameter of 27 nm.

  17. Powder injection molding of Stellite 6 powder: Sintering, microstructural and mechanical properties

    Energy Technology Data Exchange (ETDEWEB)

    Gülsoy, H. Özkan [Marmara University, Technology Faculty, Metall. and Mater. Eng., 34722 Istanbul (Turkey); Özgün, Özgür, E-mail: [Bingol University, Faculty of Engineering and Architecture, Mechanical Eng. Dep., 12000 Bingol (Turkey); Bilketay, Sezer [Marmara University, Technology Faculty, Metall. and Mater. Eng., 34722 Istanbul (Turkey)


    The purpose of this study was to produce Co-based Stellite 6 superalloy components by using the method of Powder Injection Molding (PIM) and to characterize the microstructural and mechanical properties of the produced components. The experimental studies were started through the formation of feedstock by mixing Stellite 6 powder with a multicomponent binder system. Prepared feedstock was formed by utilizing powder injection molding technique. Then the molded samples were subjected to the solvent and thermal debinding processes. Different sintering cycles were applied to the raw components for the purpose of determining the optimum sintering conditions. The densities of the sintered components were determined in accordance with the Archimedes' principle. The microstructural characterization was performed through scanning electron microscope (SEM) analysis, energy dispersive spectrometry (EDS) analyses, and X-ray diffraction (XRD) analysis. Hardness measurement and tensile test were conducted in order to determine the mechanical properties. The results illustrated that the injection molded Stellite 6 components were composed of fine and equiaxed grains, plenty of carbide precipitates exhibiting homogenous distribution throughout the microstructure formed at the grain boundaries and thus the mechanical properties were considerably high.

  18. The Improvement Effect of Dispersant in Fluorite Flotation: Determination by the Analysis of XRD and FESEM-EDX

    Directory of Open Access Journals (Sweden)

    Y. J. Li


    Full Text Available Different dispersants were added in the dispersion process to improve the efficiency of fluorite flotation. The types and dosage of dispersant on the improvement of fluorite flotation were investigated; when the sodium polyacrylate (SPA was used as the dispersant and its addition is 0.5%, the concentrate grade of CaF2 increased from 90% to 98% and the fluorite recovery increased from 81% to 85%. Methods of X-ray powder diffraction (XRD, field emission scanning electron microscopy (FESEM, and Energy dispersive X-ray spectrometer (EDX were used to characterize the sample. According to the analysis of results, the optimal sample consisted of CaF2 and very little CaCO3 in the size range of 0–5 μm. It could be concluded that the mechanism of improvement for the concentrate grade and recovery of CaF2 was attributed to the change of potential energy barrier which caused the separation of particles with different charge. All results indicate that SPA has a great potential to be an efficient and cost-effective dispersant for the improvement of fluorite flotation.

  19. Functionalized hyperbranched polyethylene powder supports. (United States)

    Bergbreiter, D E; Tao, G; Kippenberger, A M


    [reaction: see text] Polyethylene powders with useful loadings of functional groups are accessible by hyperbranched grafting chemistry. Using a 200 microm diameter high-density powder, loadings of up to 0.4 mmol/g of CO(2)H groups are attained. The carboxylic acid groups in the resulting powders can be further functionalized covalently or ionically and resulting powders have the physical durability and solvent resistance associated with polyethylene itself.

  20. Powder diffraction at ALBA synchrotron


    Aranda, Miguel A. G.


    This talk is devoted to explain the uses of powder diffraction at MSPD (material science and powder diffraction) of ALBA synchrotron light source. General characteristics of the beamline are: Station 1 - High Pressure Diffraction on powders with diamond anvil cell (DAC) and CCD detector. Microdiffraction; and Station 2 - High Resolution Powder Diffraction with Multicrystal- and Silicon-Strip detector. Energy Range: 8-50keV; Typical beam size: 4x1mm; all typical sample geometries possible: cap...

  1. Comparison between powder and slices diffraction methods in teeth samples

    Energy Technology Data Exchange (ETDEWEB)

    Colaco, Marcos V.; Barroso, Regina C. [Universidade do Estado do Rio de Janeiro (IF/UERJ), RJ (Brazil). Inst. de Fisica. Dept. de Fisica Aplicada; Porto, Isabel M. [Universidade Estadual de Campinas (FOP/UNICAMP), Piracicaba, SP (Brazil). Fac. de Odontologia. Dept. de Morfologia; Gerlach, Raquel F. [Universidade de Sao Paulo (FORP/USP), Rieirao Preto, SP (Brazil). Fac. de Odontologia. Dept. de Morfologia, Estomatologia e Fisiologia; Costa, Fanny N. [Coordenacao dos Programas de Pos-Graduacao de Engenharia (LIN/COPPE/UFRJ), RJ (Brazil). Lab. de Instrumentacao Nuclear


    Propose different methods to obtain crystallographic information about biological materials are important since powder method is a nondestructive method. Slices are an approximation of what would be an in vivo analysis. Effects of samples preparation cause differences in scattering profiles compared with powder method. The main inorganic component of bones and teeth is a calcium phosphate mineral whose structure closely resembles hydroxyapatite (HAp). The hexagonal symmetry, however, seems to work well with the powder diffraction data, and the crystal structure of HAp is usually described in space group P63/m. Were analyzed ten third molar teeth. Five teeth were separated in enamel, detin and circumpulpal detin powder and five in slices. All the scattering profile measurements were carried out at the X-ray diffraction beamline (XRD1) at the National Synchrotron Light Laboratory - LNLS, Campinas, Brazil. The LNLS synchrotron light source is composed of a 1.37 GeV electron storage ring, delivering approximately 4x10{sup -1}0 photons/s at 8 keV. A double-crystal Si(111) pre-monochromator, upstream of the beamline, was used to select a small energy bandwidth at 11 keV . Scattering signatures were obtained at intervals of 0.04 deg for angles from 24 deg to 52 deg. The human enamel experimental crystallite size obtained in this work were 30(3)nm (112 reflection) and 30(3)nm (300 reflection). These values were obtained from measurements of powdered enamel. When comparing the slice obtained 58(8)nm (112 reflection) and 37(7)nm (300 reflection) enamel diffraction patterns with those generated by the powder specimens, a few differences emerge. This work shows differences between powder and slices methods, separating characteristics of sample of the method's influence. (author)

  2. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite

    Energy Technology Data Exchange (ETDEWEB)

    Reyes-Gasga, José, E-mail: [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Martínez-Piñeiro, Esmeralda L., E-mail: [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Rodríguez-Álvarez, Galois, E-mail: [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Tiznado-Orozco, Gaby E., E-mail: [Unidad Académica de Odontología, Universidad Autónoma de Nayarit, Edificio E7, Ciudad de la Cultura “Amado Nervo”, C.P. 63190 Tepic, Nayarit (Mexico); García-García, Ramiro, E-mail: [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); and others


    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI){sub XRD} index is related to the crystal structure of the samples and the (CI){sub FTIR} index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI){sub XRD} value indicated that enamel is more crystalline than synthetic HAP, while (CI){sub FTIR} indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. - Highlights: • XRD and FTIR crystallinity indices for tooth enamel and synthetic HAP were obtained. • SEM and TEM images were more correlated with (CI){sub XRD} than with (CI){sub FTIR}. • Regardless of the temperature, (CI){sub XRD} and (CI){sub FTIR} showed similar behavior. • XRD and FTIR crystallinity indices resulted in a fast and qualitative measurement.

  3. Advanced powder processing

    Energy Technology Data Exchange (ETDEWEB)

    Janney, M.A. [Oak Ridge National Lab., TN (United States)


    Gelcasting is an advanced powder forming process. It is most commonly used to form ceramic or metal powders into complex, near-net shapes. Turbine rotors, gears, nozzles, and crucibles have been successfully gelcast in silicon nitride, alumina, nickel-based superalloy, and several steels. Gelcasting can also be used to make blanks that can be green machined to near-net shape and then high fired. Green machining has been successfully applied to both ceramic and metal gelcast blanks. Recently, the authors have used gelcasting to make tooling for metal casting applications. Most of the work has centered on H13 tool steel. They have demonstrated an ability to gelcast and sinter H13 to near net shape for metal casting tooling. Also, blanks of H13 have been cast, green machined into complex shape, and fired. Issues associated with forming, binder burnout, and sintering are addressed.

  4. Dispersing powders in liquids

    CERN Document Server

    Nelson, RD


    This book provides powder technologists with laboratory procedures for selecting dispersing agents and preparing stable dispersions that can then be used in particle size characterization instruments. Its broader goal is to introduce industrial chemists and engineers to the phenomena, terminology, physical principles, and chemical considerations involved in preparing and handling dispersions on a commercial scale. The book introduces novices to: - industrial problems due to improper degree of dispersion; - the nomenclature used in describing particles; - the basic physica

  5. Sintering of HDH Ti Powder

    Directory of Open Access Journals (Sweden)

    Kováčik Jaroslav


    Full Text Available Titanium powders prepared by hydro-dehydration process (HDH powder were pressure less sintered in vacuum oven at different temperatures, time and green density. The sintering properties of powders of two particle sizes - 30 and 150 microns were investigated. The usual powder metallurgical (PM results were observed, i.e., decreasing final porosity with increasing sintering temperature and time at constant heating rate. Higher green density leading to higher final density for both powder sizes was also observed. The obtained results will be used as comparative material for future sintering experiments of Ti based composites.

  6. Definitive Mineralogical Analysis of Mars Analog Rocks Using the CheMin XRD/XRF Instrument (United States)

    Blake, D. F.; Sarrazin, P.; Bish, D. L.; Feldman, S.; Chipera, S. J.; Vaniman, D. T.; Collins, S.


    Mineral identification is a critical component of Mars Astrobiological missions. Chemical or elemental data alone are not definitive because a single elemental or chemical composition or even a single bonding type can represent a range of substances or mineral assemblages. Minerals are defined as unique structural and compositional phases that occur naturally. There are about 15,000 minerals that have been described on Earth, all uniquely identifiable via diffraction methods. There are likely many minerals yet undiscovered on Earth, and likewise on Mars. If an unknown phase is identified on Mars, it can be fully characterized by structural (X-ray Diffraction, XRD) and elemental analysis (X-ray Fluorescence, XRF) without recourse to other data because XRD relies on the principles of atomic arrangement for its determinations. XRD is the principal means of identification and characterization of minerals on Earth.

  7. Synthesis of α-Fe2O3 Superfine Powders with Steel Pickling Waste Water and Dust Water in the Production of Bleaching Powder

    Directory of Open Access Journals (Sweden)

    Chen Li


    Full Text Available A simple method of resource processing was developed by applying the material preparation technology to hazardous waste utilization. The iron oxide was synthesized by this method with steel pickling waste water and dust water in the production of bleaching powder. The effect of temperature on the synthesis was studied. X-Ray diffraction (XRD, transmission electron microscope (TEM showed that the iron oxide samples are bright red and spherical α-Fe2O3 powders, and the particle size analysis exhibited that the size of samples prepared at 70 °C and 80 °C were between 250-300nm.

  8. Page 1 994 M Jayachandran et al Table 1. A correlation of the XRD ...

    Indian Academy of Sciences (India)

    Table 1. A correlation of the XRD studies and the possible chemical reactions in the sol-gel synthesis of cadmium tin oxide (5 g batches). Calcination Phases temperature observed in. (°C) Chemical reaction XRD pattern. 700 Cd(OH)2 — CdC + H2O Cd'O. SnO2 . xH2O — SnO2 + xH2O SnO2. 800 CdC + SnO2 - Có2SnO4+ ...

  9. Thermal decomposition of dolomite under CO2: insights from TGA and in situ XRD analysis


    Valverde, J.M.; Perejón, Antonio; Medina, Santiago; Pérez-Maqueda, Luis A.


    Thermal decomposition of dolomite in the presence of CO2 in a calcination environment is investigated by means of in situ X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The in situ XRD results suggest that dolomite decomposes directly at a temperature around 700 °C into MgO and CaO. Immediate carbonation of nascent CaO crystals leads to the formation of calcite as an intermediate product of decomposition. Subsequently, decarbonation of this poorly crystalline calcite occurs whe...

  10. Powder Production and Particle Engineering for Dry Powder Inhaler Formulations. (United States)

    Lin, Yu-Wei; Wong, Jennifer; Qu, Li; Chan, Hak-Kim; Zhou, Qi Tony


    Dry powder inhalers have become increasingly attractive for pulmonary delivery of locally and systemically effective medications. In comparison to the liquid counterparts, such as nebulisation and pressurised metered dose inhalers, the powder form generally offers better chemical stability, improved portability and potentially superior patient adherence. Currently, the aerosol performance between dry powder inhalers varies to a large extent due to differences in the design of inhaler device and formulation. The particulate properties have a significant influence on the inter-particle interactions, which impacts on the aerosolisation of the inhaled powder. In this review, critical particulate properties that affect aerosol performance are discussed. Recent advances in powder production and particle engineering techniques are also assessed, aiming to develop new inhaled powder formulations or improve the aerosolisation efficiency of existing products.


    Directory of Open Access Journals (Sweden)

    Marija Korać


    Full Text Available This paper is a contribution to characterization of Cu-Al2O3 powders with nanostructure designed for the production of dispersion strengthened contact materials. New materials with predetermined properties can be successfully synthesized by utilizing the principles of hydrometallurgy and powder metallurgy. The results show a development of a new procedure for the synthesis. The applied characterization methods were differential thermal and thermogravimetric analysis (DTA-TGA, X-ray diffraction (XRD, scanning electron microscopy (SEM, Transmission Electron Microscopy (TEM: Focused Ion Beam (FIB and Analytical Electron Microscopy (AEM. Nanostructure characteristics, particle size in range 20-50 nm, and uniform distribution of dispersoide in copper matrix were validated.

  12. Synthesis and characterization of nanocrystalline Al 2024-B4C composite powders by mechanical alloying (United States)

    Varol, T.; Canakci, A.


    In the present work, the effect of milling parameters on the morphology and microstructure of nanostructure Al2024-B4C composite powders obtained by mechanical alloying (MA) was studied. The effects of milling time and B4C content on the morphology, microstructure and particle size of nanostructure Al2024-B4C composite powders have been investigated. Different amounts of B4C particles (0, 5, 10 and 20 wt.%) were mixed with Al2024 powders and milled in a planetary ball mill for 30, 60, 120, 300, 420 and 600 min. Al 2024-B4C composite powders were characterized using a scanning electron microscope (SEM), laser particle-size analyzer, X-ray diffraction analysis (XRD) and the Vickers microhardness test. The results showed that the nanostructure Al2024-B4C composite powders were produced when they were milled for 600 min. The size of composite powder in the milled powder mixture was affected by the milling time and content of B4C particles. Moreover, it was observed that when MA reached a steady state, the properties of composite powders were stabilized.

  13. Understanding the Crystallinity Indices Behavior of Burned Bones and Teeth by ATR-IR and XRD in the Presence of Bioapatite Mixed with Other Phosphate and Carbonate Phases

    Directory of Open Access Journals (Sweden)

    Giampaolo Piga


    Full Text Available We have critically investigated the ATR-IR spectroscopy data behavior of burned human teeth as opposed to the generally observed behavior in human bones that were subjected to heat treatment, whether deliberate or accidental. It is shown that the deterioration of the crystallinity index (CI behavior sometimes observed in bones subjected to high temperature appears to be of higher frequency in the case of bioapatite from teeth. This occurs because the formation of the β-tricalcium phosphate (β-TCP phase, otherwise known as whitlockite, clearly ascertained by the X-ray diffraction (XRD patterns collected on the same powdered specimens investigated by ATR-IR. These results point to the need of combining more than one physicochemical technique even if apparently well suitable, in order to verify whether the assumed conditions assessed by spectroscopy are fully maintained in the specimens after temperature and/or mechanical processing.

  14. The precursors effects on biomimetic hydroxyapatite ceramic powders. (United States)

    Yoruç, Afife Binnaz Hazar; Aydınoğlu, Aysu


    In this study, effects of the starting material on chemical, physical, and biological properties of biomimetic hydroxyapatite ceramic powders (BHA) were investigated. Characterization and chemical analysis of BHA powders were performed by using XRD, FT-IR, and ICP-AES. Microstructural features such as size and morphology of the resulting BHA powders were characterized by using BET, nano particle sizer, pycnometer, and SEM. Additionally, biological properties of the BHA ceramic powders were also investigated by using water-soluble tetrazolium salts test (WST-1). According to the chemical analysis of BHA ceramic powders, chemical structures of ceramics which are prepared under different conditions and by using different starting materials show differences. Ceramic powders which are produced at 80°C are mainly composed of hydroxyapatite, dental hydroxyapatite (contain Na and Mg elements in addition to Ca), and calcium phosphate sulfide. However, these structures are altered at high temperatures such as 900°C depending on the features of starting materials and form various calcium phosphate ceramics and/or their mixtures such as Na-Mg-hydroxyapatite, hydroxyapatite, Mg-Whitlockit, and chloroapatite. In vitro cytotoxicity studies showed that amorphous ceramics produced at 80°C and ceramics containing chloroapatite structure as main or secondary phases were found to be extremely cytotoxic. Furthermore, cell culture studies showed that highly crystalline pure hydroxyapatite structures were extremely cytotoxic due to their high crystallinity values. Consequently, the current study indicates that the selection of starting materials which can be used in the production of calcium phosphate ceramics is very important. It is possible to produce calcium phosphate ceramics which have sufficient biocompatibility at physiological pH values and by using appropriate starting materials. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. XRD and TEM analysis of microstructure in the welding zone of 9Cr ...

    Indian Academy of Sciences (India)


    Abstract. Under the condition of tungsten inert gas shielded welding (TIG) + shielded metal arc welding. (SMAW) technology, the microstructure in the welding zone of 9Cr–1Mo–V–Nb (P91) heat-resisting steel is studied by means of X-ray diffractometry (XRD) and transmission electron microscopy (TEM). The test.

  16. Dynamic XRD, Shock and Static Compression of CaF2 (United States)

    Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew; Smith, Jesse; Sinogeikin, Stanislav


    The high-pressure behavior of CaF2 is probed with x-ray diffraction (XRD) combined with both dynamic compression, using a two-stage light gas gun, and static compression, using diamond anvil cells. We use XRD to follow the unfolding of a shock-driven, fluorite to cotunnite phase transition, on the timescale of nanoseconds. The dynamic behavior of CaF2 under shock loading is contrasted with that under static compression. This work leverages experimental capabilities at the Advanced Photon Source: dynamic XRD and shock experiments at the Dynamic Compression Sector, as well as XRD and static compression in diamond anvil cell at the High-Pressure Collaborative Access Team. These experiments and cross-platform comparisons, open the door to an unprecedented understanding of equations of state and phase transitions at the microstructural level and at different time scales and will ultimately improve our capability to simulate the behavior of materials at extreme conditions. Sandia National Laboratories is a multi-mission laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

  17. XRD and optical microscopic studies of Co(III) complexes containing ...

    Indian Academy of Sciences (India)


    XRD and optical microscopic studies of Co(III) complexes. 343. Figure 1. Optical micrograph of the complexes: (a) [MLCl]2+, (b) [ML2]3+, (c) [ML2]3+, (d) [ML2]3+, containing acetone,. (e) [ML2T2]3+, (f) [MLTCl]2+ and (g) [MLA3]3+, M = Co(en)2.

  18. Effect of sample moisture content on XRD-estimated cellulose crystallinity index and crystallite size (United States)

    Umesh P. Agarwal; Sally A. Ralph; Carlos Baez; Richard S. Reiner; Steve P. Verrill


    Although X-ray diffraction (XRD) has been the most widely used technique to investigate crystallinity index (CrI) and crystallite size (L200) of cellulose materials, there are not many studies that have taken into account the role of sample moisture on these measurements. The present investigation focuses on a variety of celluloses and cellulose...

  19. Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, David K [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Lee, Christopher [Pennsylvania State University; Dazen, Kevin [Pennsylvania State University; Kafle, Kabindra [Pennsylvania State University; Moore, Andrew [North Carolina State University; Park, Sunkyu [North Carolina State University; Kim, Seong H. [Pennsylvania State University


    Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It is demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.

  20. Microstructure and properties of gravity sintered 316l stainless steel powder with nickel boride addition

    Directory of Open Access Journals (Sweden)

    Božić Dušan


    Full Text Available The present work demonstrates a procedure for synthesis of stainless steel powder by gravity sintering method. As an additive to the basic powder, NiB powder was added in the amount of 0.2 - 1.0 wt.%. Gravity sintering was done in vacuum, at the temperatures of 1100°C-1250°C, in the course of 3 - 60 min, using ceramic mould. Structural characterization was conducted by XRD, and microstructural analysis by optical and scanning electron microscope (SEM. Mechanical properties were investigated by tensile tests with steel rings. Density and permeability were determined by standard techniques for porous samples. Gravity sintered stainless steel with NiB addition had more superior mechanical and physico-chemical properties compared to stainless steel obtained by standard powder metallurgy procedures - pressing and sintering. [Projekat Ministarstva nauke Republike Srbije, br. 172005

  1. Effect of the powder particle size on the wear behavior of boronized AISI 304 stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Guenen, Ali [Mustafa Kemal Univ., Hatay (Turkey). Dept. of Metallurgy and Material Engineering; Kuecuek, Yilmaz; Oege, Mecit; Goek, M. Sabri [Bartin Univ. (Turkey). Dept. of Mechanical Engineering; Er, Yusuf [Firat Univ., Elazig (Turkey); Cay, V. Veli [Dicle Univ., Diyarbakir (Turkey). Civil Aviation Higher School


    In this study, the AISI 304 steel specimens were boronized with nanoboron of the size of 10 50 nm and commercial Ekabor 3 powders (<1400 μm) at 950 C to 1000 C for 2 h and 4 h. Boronized steel specimens were characterized via SEM, microhardness and XRD analyses. Abrasive wear behavior of the specimens, boronized at different temperatures and treatment durations, were examined. The fixed ball micro-abrasion tests were carried out using the abrasive slurry, prepared with different SiC powder particle sizes on the boronized specimens at different rotational speeds. The specimens boronized with nanoboron powders exhibited a higher hardness and abrasive wear resistance than the samples boronized with the Ekabor 3 powders.

  2. Synthesis and Characterization of Nanocrystalline Al-20 at. % Cu Powders Produced by Mechanical Alloying

    Directory of Open Access Journals (Sweden)

    Molka Ben Makhlouf


    Full Text Available Mechanical alloying is a powder processing technique used to process materials farther from equilibrium state. This technique is mainly used to process difficult-to-alloy materials in which the solid solubility is limited and to process materials where nonequilibrium phases cannot be produced at room temperature through conventional processing techniques. This work deals with the microstructural properties of the Al-20 at. % Cu alloy prepared by high-energy ball milling of elemental aluminum and copper powders. The ball milling of powders was carried out in a planetary mill in order to obtain a nanostructured Al-20 at. % Cu alloy. The obtained powders were characterized using scanning electron microscopy (SEM, differential scanning calorimetry (DSC and X-ray diffraction (XRD. The structural modifications at different stages of the ball milling are investigated with X-ray diffraction. Several microstructure parameters such as the crystallite sizes, microstrains and lattice parameters are determined.

  3. 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: [Instituto de Investigaciones Metalurgicas, UMSNH, Edificio U, Ciudad Universitaria, Morelia, Michoacan 58000 (Mexico)


    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.

  4. Conformation and location of amorphous and semi-crystalline regions in C-type starch granules revealed by SEM, NMR and XRD. (United States)

    Wang, Shujun; Yu, Jinglin; Yu, Jiugao


    The conformations and locations of amorphous and semi-crystalline regions in C-type starch granules from Chinese yam were evaluated by a combination of morphology and spectroscopy studies during acid hydrolysis. Scanning electron micrographs showed that amorphous or less crystalline areas were essentially located in the centre part of C-type starch granules, whereas the semi-crystalline and amorphous growth rings were found mainly in the outer part of the granules. (13)C cross-polarization magic angle spinning NMR ((13)C CP/MAS NMR) showed that amorphous regions were hydrolyzed faster than the crystalline ones. In addition, B-type polymorphs were shown to be hydrolyzed more rapidly than A-types. Powder X-ray diffraction (XRD) also revealed that the B-polymorph was hydrolyzed more rapidly than the A-type. XRD showed that the amorphous or less crystalline areas were mainly located in the core of starch granules, while the amorphous growth rings are distributed toward the outside of the granules and alternatively arranged with semi-crystalline growth rings. The amorphous or less crystalline areas predominantly consisted of the B-polymorph whereas the outer semi-crystalline and amorphous growth rings were mostly composed of the A-polymorph. Copyright © 2008 Elsevier Ltd. All rights reserved.

  5. Using Variable Temperature Powder X-Ray Diffraction to Determine the Thermal Expansion Coefficient of Solid MgO (United States)

    Corsepius, Nicholas C.; DeVore, Thomas C.; Reisner, Barbara A.; Warnaar, Deborah L.


    A laboratory exercise was developed by using variable temperature powder X-ray diffraction (XRD) to determine [alpha] for MgO (periclase)and was tested in the Applied Physical Chemistry and Materials Characterization Laboratories at James Madison University. The experiment which was originally designed to provide undergraduate students with a…

  6. Ti-Mg alloy powder synthesis via mechanochemical reduction of TiO2 by elemental magnesium

    CSIR Research Space (South Africa)

    Mushove, T


    Full Text Available with 15% excess Mg. The powder mixture was mechanically milled in a Simoloyer high energy ball mill for 5 different durations. Contamination was minimised by processing under a high purity argon atmosphere. Changes in phase composition were studied by XRD...

  7. Indigenous tooth powders = Covert lead poisoning?

    National Research Council Canada - National Science Library

    Hegde, Sapna; Shubha, A; Rao, B


    .../almond shell, coconut shell and its sheath, wood, coal and other powders (sand, common salt-powder and crystalline, brick and tile powder, tobacco, areca nut). [4] In addition, a variety of indigenous tooth powders are marketed which are very popular with the local people. Many of these age-old formulations of tooth powders may contain ha...

  8. Synthesis and characterization of bismuth alkaline titanate powders

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Huerta, A.M., E-mail: [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Dominguez-Crespo, M.A. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Hernandez-Perez, M.A. [ESIQIE, Metalurgia, Instituto Politecnico Nacional, Mexico, D. F (Mexico); Garcia-Zaleta, D.S. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Brachetti-Sibaja, S.B. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Instituto Tecnologico de Ciudad Madero, Av. 1o. de Mayo esq. Sor Juana Ines de la Cruz s/n Col. Los Mangos C.P.89440 Cd. Madero Tamaulipas (Mexico)


    In this work, samples of bismuth alkaline titanate, (K{sub 0.5}Na{sub 0.5}){sub (2-x/2)}Bi{sub (x/6)}TiO{sub 3}, (x = 0.05-0.75) have been prepared by conventional ceramic technique and molten salts. Metal oxides or carbonates powders were used as starting raw materials. The crystalline phase of the synthesized powders was identified by the X-ray diffraction (XRD) and particle morphology was characterized by scanning electron microscopy (SEM). Solid state reaction method was unsuccessful to obtain pellets. From XRD results, a rhombohedral structure was detected and the parameter lattice were estimated to be a = 5.5478 A and {alpha} = 59.48{sup o}. These parameters were used to refine the structure by Rietveld analysis. SEM results showed several morphologies. Apparently, bismuth is promoting the grain growth whose sizes vary from 30 nm to 180 nm It is expected that these materials can be utilized in practical applications as substitutes for lead zirconatetitanate (PZT)-based ceramics.

  9. Effect of zircon on sintering, composition and microstructure of magnesia powders

    Directory of Open Access Journals (Sweden)

    Peng C.


    Full Text Available The effects of zircon on sintering, composition and microstructure of fused magnesia powders were studied by XRD, SEM and EDAX. With the increase of zircon content up to 6 wt%, the strength of sintered samples increased but the apparent porosity decreased. 6 wt% is an appropriate content of zircon to possess better properties of samples, and in this case the samples have a dense microstructure and lower content of glass phase. The presence of a liquid phase resulting from zircon addition is the main reason to improve sintering of magnesia powders.

  10. Method of manufacturing powder particles

    NARCIS (Netherlands)

    Borra, J.P.D.


    The invention relates to a method of manufacturing a dry powder particle, preferably using electro-hydrodynamic spraying, wherein two oppositely charged aerosol streams are contacted. The invention allows for the manufacture of powders having various, controllable compositions and shapes. In

  11. Synthesis, characterization and electrochemical performance of core/shell structured carbon coated silicon powders for lithium ion battery negative electrodes

    Directory of Open Access Journals (Sweden)

    Tuğrul Çetinkaya


    Full Text Available Surface of nano silicon powders were coated with amorphous carbon by pyrolysis of polyacronitrile (PAN polymer. Microstructural characterization of amorphous carbon coated silicon powders (Si-C were carried out using scanning electron microscopy (SEM and thickness of carbon coating is defined by transmission electron microscopy (TEM. Elemental analyses of Si-C powders were performed using energy dispersive X-ray spectroscopy (EDS. Structural and phase characterization of Si-C composite powders were investigated using X-ray diffractometer (XRD and Raman spectroscopy. Produced Si-C powders were prepared as an electrode on the copper current collector and electrochemical tests were carried out using CR2016 button cells at 200 mA/g constant current density. According to electrochemical test results, carbon coating process enhanced the electrochemical performance by reducing the problems stem from volume change and showed 770 mAh/g discharge capacity after 30 cycles.

  12. Microanalysis of clay-based pigments in paintings by XRD techniques

    Czech Academy of Sciences Publication Activity Database

    Hradil, David; Bezdička, Petr; Hradilová, J.; Vašutová, V.


    Roč. 125, MAR (2016), s. 10-20 ISSN 0026-265X R&D Projects: GA ČR(CZ) GA14-22984S Institutional support: RVO:61388980 Keywords : Clay minerals * Earth pigments * Clay -binder interaction * Powder X-ray micro-diffraction * Quantitative phase microanalysis Subject RIV: DB - Geology ; Mineralogy Impact factor: 3.034, year: 2016

  13. Powder-Bed Stabilization for Powder-Based Additive Manufacturing

    Directory of Open Access Journals (Sweden)

    Andrea Zocca


    Full Text Available The most successful additive manufacturing (AM technologies are based on thelayer-by-layer depositionof a flowable powder. Although considered as the third industrial revolution, one factor still limiting these processes to become completely autonomous is the often necessary build-up of support structures. Besides the prevention of lateral shifts of the part during the deposition of layers, the support assures quality and stability to the built process. The loose powder itself surrounding the built object, or so-called powder-bed, does not provide this sustenance in most existent technology available. Here we present a simple but effective and economical method for stabilizing the powder-bed, preventing distortions in the geometry with no need for support structures. This effect, achieved by applying an air flow through the powder-bed, is enabling an entirely autonomous generation of parts and is a major contribution to all powder-based additive manufacturing technologies. Moreover, it makes powder-based AM independent of gravitational forces, which will facilitate crafting items in space from a variety of powdery materials.

  14. Shot peening induced phase transformations and residual stresses measurements on austempered cast irons by XRD

    Energy Technology Data Exchange (ETDEWEB)

    Zambon, A. (DIMEG, Univ. di Padova (Italy)); Tiziani, A. (DIMEG, Univ. di Padova (Italy)); Giordano, L. (DIMEG, Univ. di Padova (Italy)); Bonollo, F. (DIMEG, Univ. di Padova (Italy)); Molinari, A. (Dip. Ing. Mater., Univ. di Trento (Italy))


    The present work is aimed at evaluating the effect on the residual stress pattern of two concurrent phenomena induced on austempered cast irons by Shot Peening: stresses due to the deformation and stresses produced by the transformation of the mechanically unstable retained austenite. According to XRD determinations of the amounts of the retained austenite variations and of the corresponding stress values, the leading phenomenon in the residual stresses settlment seems to be deformation related. (orig.)

  15. Characterisation of spray dried soy sauce powders made by adding crystalline carbohydrates to drying carrier. (United States)

    Wang, Wei; Zhou, Weibiao


    This study aimed to reduce stickiness and caking of spray dried soy sauce powders by introducing a new crystalline structure into powder particles. To perform this task, soy sauce powders were formulated by using mixtures of cellulose and maltodextrin or mixtures of waxy starch and maltodextrin as drying carriers, with a fixed carrier addition rate of 30% (w/v) in the feed solution. The microstructure, crystallinity, solubility as well as stickiness and caking strength of all the different powders were analysed and compared. Incorporating crystalline carbohydrates in the drying carrier could significantly reduce the stickiness and caking strength of the powders when the ratio of crystalline carbohydrates to maltodextrin was above 1:5 and 1:2, respectively. X-ray Diffraction (XRD) results showed that adding cellulose or waxy starch could induce the crystallinity of powders. Differential Scanning Calorimetry (DSC) results demonstrated that the native starch added to the soy sauce powders did not fully gelatinize during spray drying. Copyright © 2014 Elsevier Ltd. All rights reserved.

  16. Effect of ball to powder weight ratio on the mechanochemical synthesis of MoSi2-TiC nanocomposite powder

    Directory of Open Access Journals (Sweden)

    Mohamad Zakeri


    Full Text Available MoSi2-TiC nanocomposite powders were successfully synthesized with different ball to powder weight ratios (BPR by ball milling of Mo, Si, Ti and graphite elemental powders. Formation of this composite was studied by X-ray diffraction (XRD. Morphology and microstructure of the milled powders were monitored by scanning and transmission electron microscopy (SEM and TEM, respectively. There was incomplete formation in BPR 5:1 after 30 hours of milling, however, the formation of this composite was completed after 10 hours in BPRs 15:1 and 20:1. Higher BPRs with longer milling time led to partially transformation of β to α MoSi2. Based on Rietveld refinement analysis, and subsequent verification by TEM image, nanostructure powders with the mean grain size less than 25 nm were obtained in all BPRs. Very fine submicron powders in agglomerated ones for BPRs 10:1 and 15:1were obtained at the end of milling.

  17. Thermal and structural study of guava (Psidium guajava L powders obtained by two dehydration methods

    Directory of Open Access Journals (Sweden)

    Coralia Osorio


    Full Text Available Two food products (powders were obtained by hot-air drying or lyophilisation methods on the whole guava fruits. The powders were characterised by sensory and thermal analyses (TGA-DSC, infrared spectroscopy (IR, X-ray diffraction (XRD and scanning electron microscopy (SEM. Thermal, morphological and structural characterisations showed a similar behaviour for the two solids. TGA-DSC and IR showed the presence of pectin as the main constituent of solids. A semi-crystalline profile was evidenced by XRD, and lamellar/spherical morphologies were observed by SEM. Sensory analyses revealed an aroma highly related to guava. These value-added food products are an alternative to process guava and avoid loss during postharvest handling.

  18. [Study on the vibrational spectra and XRD characters of Huanglong jade from Longling County, Yunnan Province]. (United States)

    Pei, Jing-cheng; Fan, Lu-wei; Xie, Hao


    Based on the conventional test methods, the infrared absorption spectrum, Raman spectrum and X-ray diffraction (XRD) were employed to study the characters of the vibration spectrum and mineral composition of Huanglong jade. The testing results show that Huanglong jade shows typical vibrational spectrum characteristics of quartziferous jade. The main infrared absorption bands at 1162, 1076, 800, 779, 691, 530 and 466 cm(-1) were induced by the asymmetric stretching vibration, symmetrical stretching vibration and bending vibration of Si-O-Si separately. Especially the absorption band near 800 cm(-1) is split, which indicates that Huanglong jade has good crystallinity. In Raman spectrum, the main strong vibration bands at 463 and 355 cm(-1) were attributed to bending vibration of Si-O-Si. XRD test confirmed that Quartz is main mineral composition of Huanglong jade and there is a small amount of hematite in red color samples which induced the red color of Huanglong jade. This is the first report on the infrared, Raman and XRD spectra feature of Huanglong jade. It will provide a scientific basis for the identification, naming and other research for huanglong jade.

  19. Effect of γ-irradiation on clays and organoclays: a Mössbauer and XRD study (United States)

    Gournis, D.; Mantaka-Marketou, A. E.; Karakassides, M. A.; Petridis, D.

    The interaction of γ-rays with smectite clays induces noticeable changes in the structure and physicochemical properties of the minerals. For sodium-montmorillonite, Mössbauer spectra show that γ-irradiation causes a partial reduction of trivalent iron to the divalent state due to hydrogen radicals production from the radiolysis of interlayer water. The XRD results show no change in the interlayer space upon irradiation and therefore the radiolysis of interlayer water causes no measurable changes in the architectural organization of the interlayer environment. Intercalation of simple organic molecules (ethylene glycol, tert-butanol and tetraalkylammonium salts) causes partial oxidation of structural divalent iron and affects the Mössbauer parameters of the M1 and M2 ferric components. Irradiation of ethylene glycol- or tert-butanol-clay composites indicates reduction of trivalent iron to the divalent state. XRD data show that the irradiation of clay-ethylene glycol complex causes collapse of the initial double layer of glycol molecules to a single layer complex. Finally, XRD results show that the effects of γ-irradiation on clay-tetraalkylammonium complexes depend upon the chain length of the organic cations.

  20. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite. (United States)

    Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E; García-García, Ramiro; Brès, Etienne F


    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI)XRD index is related to the crystal structure of the samples and the (CI)FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI)XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI)FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. © 2013.

  1. Mineralogical composition of the meteorite El Pozo (Mexico): a Raman, infrared and XRD study. (United States)

    Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol


    The Raman (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of El Pozo meteorite (an ordinary chondrite L5 type; village Valle of Allende, founded in State of Chihuahua, Mexico: 26°56'N and 105°24'W, 1998). RMP measurements in the range of 100-3500 cm(-1) revealed principal characteristic bands of the major minerals: olivine, two polymorph modifications of pyroxene (OPx and CPx) and plagioclase. Some bands of the minor minerals (hematite and goethite) were also identified. All these minerals were clearly distinguished using IR and XRD techniques. XRD technique has shown the presence of some metallic phases such as kamacite and taenite as well as troilite and chromite. These minerals do not have characteristic Raman spectra because Fe-Ni metals have no active modes for Raman spectroscopy and troilite is a weak Raman scatterer. Raman mapping microspectroscopy was a key part in the investigation of El Pozo meteorite's spatial distribution of the main minerals because these samples are structurally and chemically complex and heterogeneous. The mineral mapping by Raman spectroscopy has provided information for a certain spatial region on which a spatial distribution coexists of the three typical mineral assemblages: olivine; olivine+orthopyroxene; and orthopyroxene. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Preparation of superconductor precursor powders (United States)

    Bhattacharya, Raghunath; Blaugher, Richard D.


    A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals, such as nitrate salts of thallium, barium, calcium, and copper, which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of thallium in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.


    Directory of Open Access Journals (Sweden)

    Yash Mishra


    Full Text Available In this study, the adsorption potential of Teak (Tectona grandis leaf powder (TLP toremove Methylene blue (MB and Malachite Green (MG dye molecules from aqueoussolution was investigated. Batch experiments were conducted to evaluate the influenceof operational parameters such as, pH (2−9, adsorbent dosage (1−7 g/L, contact time(15−150 minutes and initial dye concentration (20−120 mg/L at stirring speed of 150rpm for the adsorption of MB and MG on TLP. Maximum removal efficiency of 98.4%and 95.1% was achieved for MB and MG dye, respectively. The experimentalequilibrium data were analysed using Langmuir, Freundlich and Temkin isothermmodels and it was found that, it fitted well to the Freundlich isotherm model. Thesurface structure and morphology of the adsorbent was characterized using scanningelectron microscopy (SEM and the presence of functional groups and its interactionwith the dye molecules were analysed using Fourier transform infrared spectroscopy(FTIR. Based on the investigation, it has been demonstrated that the teak leaf powderhas good potential for effective adsorption of methylene blue and malachite green dye.

  4. Micro-XRD and temperature-modulated DSC investigation of nickel-titanium rotary endodontic instruments. (United States)

    Alapati, Satish B; Brantley, William A; Iijima, Masahiro; Schricker, Scott R; Nusstein, John M; Li, Uei-Ming; Svec, Timothy A


    Employ Micro-X-ray diffraction and temperature-modulated differential scanning calorimetry to investigate microstructural phases, phase transformations, and effects of heat treatment for rotary nickel-titanium instruments. Representative as-received and clinically used ProFile GT and ProTaper instruments were principally studied. Micro-XRD analyses (Cu Kalpha X-rays) were performed at 25 degrees C on areas of approximately 50 microm diameter near the tip and up to 9 mm from the tip. TMDSC analyses were performed from -80 to 100 degrees C and back to -80 degrees C on segments cut from instruments, using a linear heating and cooling rate of 2 degrees C/min, sinusoidal oscillation of 0.318 degrees C, and period of 60s. Instruments were also heat treated 15 min in a nitrogen atmosphere at 400, 500, 600 and 850 degrees C, and analyzed. At all Micro-XRD analysis regions the strongest peak occurred near 42 degrees , indicating that instruments were mostly austenite, with perhaps some R-phase and martensite. Tip and adjacent regions had smallest peak intensities, indicative of greater work hardening, and the intensity at other sites depended on the instrument. TMDSC heating and cooling curves had single peaks for transformations between martensite and austenite. Austenite-finish (A(f)) temperatures and enthalpy changes were similar for as-received and used instruments. Heat treatments at 400, 500 and 600 degrees C raised the A(f) temperature to 45-50 degrees C, and heat treatment at 850 degrees C caused drastic changes in transformation behavior. Micro-XRD provides novel information about NiTi phases at different positions on instruments. TMDSC indicates that heat treatment might yield instruments with substantial martensite and improved clinical performance.


    Directory of Open Access Journals (Sweden)

    Menik Sri Wahyuni, Erna Hastuti


    Full Text Available Cangkang kerang jenis Anadara Granosa merupakan bahan keramik yang  termasuk ke dalam jenis zat padat kristal. Sebagai langkah awal dilakukan penelitian dengan sampel cangkang kerang (CaCO3  yaitu melakukan karakterisasi menggunakan dua  alat yang berbeda yaitu X Ray Diffraction (XRD dan X Ray Physics Basic Unit, ini dilakukan untuk mengetahui perbedaan antara kedua alat tersebut. Dalam karakterisasi cangkang kerang (CaCO3 menggunakan X–Ray Diffraction dan X – Ray Physics Basic  Unit  tahapan – tahapannya antara lain: (1 cangkang kerang dicuci dengan alkohol  dan  gelombang ultrasonik, (2  penghalusan secara  manual  dan  ball  milling,  (3 Karakterisasi menggunakan XRD dan X-Ray Physics Basic Unit, (4 Pengamatan serbuk cangkang kerang  menggunakan Transmission Electron Microscopy (TEM dan mikroskop inverted, (5 analisa.Dari hasil karakterisasi menggunakan XRD diketahui strukturnya adalah ortorombik, dengan nilai parameter kisi a 4.96630,  b 7.95950, c 5.75030, sedangkan untuk nilai Rp, Rwp, Rexp, RB   dan GOF masih  belum  didapatkan  hasil  yang  baik,  hal  ini disebabkan  cangkang kerang  merupakan bahan alam yangbersifat heterogen. ini dapat dilihat dari hasil foto TEM yang masih kurang jelas. Sedangkan hasil difraksi sinar x menggunakan X-Ray Physics Basic Unit tidak didapatkan puncak yang jelas, namun dapat dihitung energi tertinggi pada sudut 18o    yaitu 2,006.10-6    d -1  dan  energi terendah pada sudut 58o   sebesar 1,171.10-6   d -1. Dan dari pengamatan dengan mikroskop inverted didapatkan ukuran butir sampel antara 1.28 sampai 0.85  µF .

  6. Niobium and chromium rich coatings tailored by laser alloying: XRD analysis at high temperatures

    Directory of Open Access Journals (Sweden)

    Adilson Rodrigues da Costa


    Full Text Available Laser treatment technologies have been widely used to modify superficial layers of different materials. In this work we prepare Nb and Cr rich coatings according to laser alloying technique using cast iron as substrate material. Nb and Cr are intensive used in order to overcome challenges like good chemical and mechanical performance at high temperatures. Following laser alloying the surface-modified samples were submitted to an "in situ" XRD analysis under controlled high temperature and atmosphere. The phase transitions registered point to transformations that do not implies formation of fragile phases or cracks induced by high volumes modifications.

  7. The XRD Amorphous Component in John Klein Drill Fines at Yellowknife Bay, Gale Crater, Mars (United States)

    Morris, Richard V.; Ming,, Douglas W.; Blake, David; Vaniman, David; Bish, David L; Chipera, Steve; Downs, Robert; Morrison, Shaunna; Gellert, Ralf; Campbell, Iain; hide


    Drill fines of mudstone (targets John Klein and Cumberland) from the Sheepbed unit at Yel-lowknife Bay were analyzed by MSL payload elements including the Chemistry and Mineralogy (CheMin), APXS (Alpha Particle X-Ray Spectrometer), and Sample Analysis at Mars (SAM) instruments. CheMin XRD results show a variety of crystalline phases including feldspar, pyroxene, olivine, oxides, oxyhydroxides, sulfates, sulfides, a tri-octahedral smectite, and XRD amorphous material. The drill fines are distinctly different from corresponding analyses of the global soil (target Rocknest) in that the mudstone samples contained detectable phyllosilicate. Here we focus on John Klein and combine CheMin and APXS data to calculate the chemical composition and concentration of the amorphous component. The chemical composition of the amorphous plus smectite component for John Klein was calculated by subtracting the abundance-weighted chemical composition of the individual XRD crystalline components from the bulk composition of John Kline as measured by APXS. The chemical composition of individual crystalline components was determined either by stoichiometry (e.g., hematite and magnetite) or from their unit cell parameters (e.g., feldspar, olivine, and pyroxene). The chemical composition of the amorphous + smectite component (approx 71 wt.% of bulk sample) and bulk chemical composition are similar. In order to calculate the chemical composition of the amorphous component, a chemical composition for the tri-octahedral smectite must be assumed. We selected two tri-octahedral smectites with very different MgO/(FeO + Fe2O3) ratios (34 and 1.3 for SapCa1 and Griffithite, respectively). Relative to bulk sample, the concentration of amorphous and smectite components are 40 and 29 wt.% for SapCa1 and 33 and 36 wt.% for Griffithite. The amount of smectite was calculated by requiring the MgO concentration to be approx 0 wt.% in the amorphous component. Griffithite is the preferred smectite because

  8. Study of the suitability of a commercial hydroxyapatite powder to obtain sintered compacts for medical applications (United States)

    Palacio, C.; Jaramillo, D.; Correa, S.; Arroyave, M.


    Hydroxyapatite (HA) is a material widely used by the medical community due to its Ca/P ratio is comparable to the Ca/P ratio of bones and teeth, which promotes osteoinduction and osteoconduction processes when in contact with bone tissue, either as volume piece or coating. This work focuses on studying the quality of the commercial HA powder MKnano-#MKN-HXAP-S12 µm, after processing, to obtain sintered compact discs with suitable physical and chemical characteristics for implants applications. The HA powder was processed through calcination, grinding, pressing and sintering to evaluate the effect of such as procedures in the compacts dics quality. The raw powder was characterized by laser diffraction, SEM, XRF, XRD, TGA and DSC while the characteristics of the obtained compact discs were determined by dilatometry and XRD to identify the sintering temperature range, constituent phases, the amorphous content and the crystallinity degree, parameters that allow determining their suitability for implants applications. Although, it was not possible to obtain sintered compacts with the suitable chemical composition and without fractures, this work allowed to identify the parameters that determine the suitability of a HA powder to obtain sintered compacts for medical applications, as well as the characterization protocol that allows the evaluation of such parameters.

  9. Structure and shear in a cohesive powder

    NARCIS (Netherlands)

    Janssen, R.J.M.


    Handling of powders and granular materials is of great importance to industry. However, the knowledge of many powder related processes in industry is poor. In this work, the flow behaviour of powder has been investigated with an advanced tester: the Flexible Wall Biaxial Tester. Flow of powder

  10. XRD, TEM, and thermal analysis of Arizona Ca-montmorillonites modified with didodecyldimethylammonium bromide. (United States)

    Sun, Zhiming; Park, Yuri; Zheng, Shuilin; Ayoko, Godwin A; Frost, Ray L


    An Arizona SAz-2 calcium montmorillonite was modified by a typical dialkyl cationic surfactant (didodecyldimethylammonium bromide, abbreviated to DDDMA) through direct ion exchange. The obtained organoclays were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), high-resolution thermogravimetric analysis (HR-TG), and infrared emission spectroscopy (IES). The intercalation of surfactants greatly increased the basal spacing of the interlayers and the conformation arrangement of the loaded surfactant were assessed based on the XRD and TEM measurements. This work shows that the dialkyl surfactant can be directly intercalated into the montmorillonite without first undergoing Na(+) exchange. Moreover, the thermal stability of organoclays and the different arrangements of the surfactant molecules intercalated in the SAz-2 Ca-montmorillonite were determined by a combination of TG and IES techniques. The detailed conformational ordering of different intercalated surfactants under different conditions was also studied. The surfactant molecule DDDMA has proved to be thermally stable even at 400°C which indicates that the prepared organoclay is stable to significantly high temperatures. This study offers new insights into the structure and thermal stabilities of SAz-2 Ca-montmorillonite modified with DDDMA. The experimental results also confirm the potential applications of organic SAz-2 Ca-montmorillonites as adsorbents and polymer-clay nanocomposites. Copyright © 2013 Elsevier Inc. All rights reserved.

  11. An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments (United States)

    Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.


    By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

  12. Study of polymer film formation and their characterization using NMR, XRD and DSC

    Energy Technology Data Exchange (ETDEWEB)

    Ghoshal, Sushanta


    Film formation and their characterization of three eco-friendly polymers, namely gelatin, starch and poly(vinyl alcohol) (PVOH) were studied using nuclear magnetic resonance (NMR), wide-angle X-ray diffractometry (XRD) and differential scanning calorimetry (DSC) techniques. Polymer solutions were prepared using water as a solvent followed by casting. The drying process of the cast sample was monitored at room temperature with a single-sided NMR scanner until complete solidification occurred. Depth-dependent NMR profiles with microscopic resolution were acquired at different stages of sample drying. Each profile point was accumulated from the echo decay. Spin-spin relaxation times (T{sub 2}) were measured from the echo decays at different layers and were correlated with the drying process during film formation. Additionally, spin-lattice relaxation times (T{sub 1}) were determined. Depending on the polymer studied and the initial concentration of each polymer, different types of molecular dynamics were observed at different heights during evaporation of the solvent. The study indicates that each polymer shows a spatial heterogeneity in the molecular dynamics during drying. In the advanced stage of drying process, the microscopic arrangement of the polymer chains during their solidification is influenced by this dynamic heterogeneity and determines the final structure of the film. XRD of the film in its final state confirmed the structural heterogeneity identified by the NMR.

  13. Mechanical properties of single nanostructures investigated by in-situ AFM and micro-XRD

    Energy Technology Data Exchange (ETDEWEB)

    Cornelius, Thomas; Scheler, Thomas; Magalhaes-Paniago, Rogerio; Metzger, Till Hartmut [ESRF, Grenoble (France)


    In recent years, nanostructures attracted enormous attention due to size-effects influencing the structural, optical, electrical, and mechanical properties of materials with low dimensions. Concerning the mechanical properties mainly the plastic regime was explored showing a trend that ''smaller is stronger''. In contrast, studies of the elastic behaviour of nanowires revealed contradictory results concerning the influence of size-effects on the elasticity. To investigate single nanoobjects in the elastic regime, we combined an in-situ AFM with XRD in a microfocused beam. The AFM is used to image the sample surface, to select an individual nanostructure, and to apply pressure on a chosen object. Due to the interaction between the AFM-tip and the compressed object the resonance frequency of the AFM force sensor shifts to larger values enabling us to derive the stiffness of the contact area. Simultaneous to the pressure application, XRD images around a pre-defined Bragg peak are recorded. These images allow for the determination of the elastic lattice parameter change in-situ. From the contact stiffness and the lattice parameter change, the Young modulus of an individual nanoobject is derived. Here, we present results both for SiGe islands grown by liquid-phase epitaxy on Si wafers and GaAs nanorods created by selective-area metalorganic vapor phase epitaxy on GaAs substrates.

  14. Effects of acid treatment on the clay palygorskite: XRD, surface area, morphological and chemical composition

    Energy Technology Data Exchange (ETDEWEB)

    Xavier, Katiane Cruz Magalhaes; Santos, Maria do Socorro Ferreira dos; Santos, Maria Rita Morais Chaves; Oliveira, Marilia Evelyn Rodrigues; Osajima, Josy Antevelli; Silva Filho, Edson Cavalcanti da [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil); Carvalho, Maria Wilma Nunes Cordeiro, E-mail: [Universidade Federal de Campina Grande (UFCG), PB (Brazil)


    The palygorskite is an aluminum-magnesium silicate that has a fibrous morphology. Their physicochemical characteristics are the result of high surface area, porosity and thermal resistance which make it an attractive adsorbent. Its adsorption capacity can be increased through chemical reactions and/or heat treatments. The objective of this work is to verify the effects of acid activation on the palygorskite, treated with HCl at 90 °C at concentrations of 2, 4 and 6 mol L{sup -1} in 2 and 4 hours, with clay/acid solution ratio 1 g 10 mL{sup -1} and characterized by techniques: XRF, XRD and surface area. A significant increase in specific surface area was observed in the sample treated with HCl at the concentration 6 mol L{sup -1}. The changes were more pronounced at stricter concentrations of acidity, with decreasing intensity of reflection of the clay indicated in the XRD. These changes were confirmed in the XRF with the leaching of some oxides and with increasing concentration of SiO{sub 2}. (author)

  15. Upgrades to the XRD1 beamline optics and endstation at the LNLS (United States)

    Canova, H.; Fontoura, A.; Neuenschwander, R. T.; Diaz, B.; Rodella, C. B.


    XRD1 was the first X-ray diffraction beamline to be built at the LNLS and after approximately 12 years of operation it was substantially updated to improve beam stability, increase the reliability of the monochromator movement as well as provide an experimental hutch that would meet the demands of users. The improvements included the construction of an independent concrete slab below the mirror and monochromator to minimize the vibrations originating from the floor. In addition, the installation of new monochromator mechanisms as well as the replacement of the two Si(111) crystals were performed in order to attain higher precision, stability and reproducibility during operation. Moreover, the diffractometer was replaced by a 3-circle heavy duty diffractometer from Newport to collect XRD patterns primarily in capillary geometry. A robotic arm was installed for fast and automated replacement of samples as well as to secure a cryojet or a hot air blower in front of the sample during measurements. In addition, a housing equipped with 24 Mythen detectors was installed at the beamline allowing for extremely fast data acquisition. Another upgrade was the integration of motors and control systems from PXI National Instruments and Galil controllers with Phytron. These systems are crucial for the next upgrade that is underway at the beamline: enabling remote access for users to collect their measurements without the need to travel to the LNLS.

  16. Exploration of geo-mineral compounds in granite mining soils using XRD pattern data analysis (United States)

    Koteswara Reddy, G.; Yarakkula, Kiran


    The purpose of the study was to investigate the major minerals present in granite mining waste and agricultural soils near and away from mining areas. The mineral exploration of representative sub-soil samples are identified by X-Ray Diffractometer (XRD) pattern data analysis. The morphological features and quantitative elementary analysis was performed by Scanning Electron Microscopy-Energy Dispersed Spectroscopy (SEM-EDS).The XRD pattern data revealed that the major minerals are identified as Quartz, Albite, Anorthite, K-Feldspars, Muscovite, Annite, Lepidolite, Illite, Enstatite and Ferrosilite in granite waste. However, in case of agricultural farm soils the major minerals are identified as Gypsum, Calcite, Magnetite, Hematite, Muscovite, K-Feldspars and Quartz. Moreover, the agricultural soils neighbouring mining areas, the minerals are found that, the enriched Mica group minerals (Lepidolite and Illite) the enriched Orthopyroxene group minerals (Ferrosilite and Enstatite). It is observed that the Mica and Orthopyroxene group minerals are present in agricultural farm soils neighbouring mining areas and absent in agricultural farm soils away from mining areas. The study demonstrated that the chemical migration takes place at agricultural farm lands in the vicinity of the granite mining areas.

  17. The use of micro-XRD for the study of glaze color decorations

    Energy Technology Data Exchange (ETDEWEB)

    Pradell, T.; Molina, G. [Universitat Politecnica de Catalunya, Dpt. Fisica i Enginyeria Nuclear, Castelldefels (Spain); Molera, J.; Pla, J. [Universitat de Vic, GRTD, Escola Politecnica Superior, Vic (Spain); Labrador, A. [BM16-ESRF, LLS, BP 220, Grenoble Cedex (France); Lund University, MAX IV Laboratory, Lund (Sweden)


    The compounds responsible for the colors and decorations in glass and glazed ceramics include: coloring agents (transition-metal ions), pigments (micro- and nanoprecipitates of compounds that either do not dissolve or recrystallize in the glassy matrix) and opacifiers (microcrystalline compounds with high light scattering capability). Their composition, structure and range of stability are highly dependent not only on the composition but also on the procedures followed to obtain them. Chemical composition of the colorants and crystallites may be obtained by means of SEM-EDX and WDX. Synchrotron radiation micro-X-ray diffraction (SR-micro-XRD) has a small beam size adequate (10 to 50 microns footprint size) to obtain the structural information of crystalline compounds and high brilliance, optimal for determining the crystallites even when present in low amounts. In addition, in glass decorations the crystallites often appear forming thin layers (from 10 to 100 micrometers thick) and they show a depth-dependent composition and crystal structure. Their nature and distribution across the glass/glaze decorations gives direct information on the technology of production and stability and may be related to the color and appearance. A selection of glass and glaze coloring agents and decorations are studied by means of SR-micro-XRD and SEM-EDX including: manganese brown, antimony yellow, red copper lusters and cobalt blue. The selection includes Medieval (Islamic, and Hispano Moresque) and Renaissance tin-glazed ceramics from the 10th to the 17th century AD. (orig.)

  18. Addressing difficulties in using XRD intensity for structural study of thin films

    Energy Technology Data Exchange (ETDEWEB)

    Ramadan, A.A.; El-Shabiny, A.M. [XRD Department, National Research Center, Dokky, Giza (Egypt); Abd El-Mongy, A.A.; Mater, A.T.; Mostafa, S.H.; El-Sheheedy, E.A.; Hashem, H.M. [Physics Department, Faculty of Science, Helwan University, Helwan (Egypt)


    The problem of structure investigation of thin films using laboratory XRD diffraction intensities was discussed as a matter of debate. Is the variation in relative intensities of the diffraction patterns due to crystallographic preferred orientation, lattice defects or both? The answer to this question shows a discrepancy in the literatures. The present work is an attempt to propose a possible approach to judge the most probable answer. Thin films of SnO{sub 2} were prepared by spray pyrolysis technique using solution of different SnCl{sub 2} concentrations (molarity); at fixed substrate temperature and deposition time. The theoretically calculated integrated intensities together with the experimentally obtained and calculated XRD data (relative intensities, texture coefficients and profile analysis) were considered together in order to get the proper picture of the structure characteristics of the prepared films. The complete picture can be assembled by integration and correlation of all the crystallographic information that are extracted from the diffraction pattern including not only the observed intensities but also the size/strain analysis and lattice parameters. (copyright 2009 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  19. XRD- and infrared-probed anisotropic thermal expansion properties of an organic semiconducting single crystal. (United States)

    Mohanraj, J; Capria, E; Benevoli, L; Perucchi, A; Demitri, N; Fraleoni-Morgera, A


    The anisotropic thermal expansion properties of an organic semiconducting single crystal constituted by 4-hydroxycyanobenzene (4HCB) have been probed by XRD in the range 120-300 K. The anisotropic thermal expansion coefficients for the three crystallographic axes and for the crystal volume have been determined. A careful analysis of the crystal structure revealed that the two different H-bonds stemming from the two independent, differently oriented 4HCB molecules composing the unit cell have different rearrangement patterns upon temperature variations, in terms of both bond length and bond angle. Linearly Polarized Mid InfraRed (LP-MIR) measurements carried out in the same temperature range, focused on the O-H bond spectral region, confirm this finding. The same LP-MIR measurements, on the basis of a semi-empirical relation and of geometrical considerations and assumptions, allowed calculation of the -CNH-O- hydrogen bond length along the a and b axes of the crystal. In turn, the so-calculated -CNH-O- bond lengths were used to derive the thermal expansion coefficients along the corresponding crystal axes, as well as the volumetric one, using just the LP-MIR data. Reasonable to good agreement with the same values obtained from XRD measurements was obtained. This proof-of-principle opens interesting perspectives about the possible development of a rapid, low cost and industry-friendly assessment of the thermal expansion properties of organic semiconducting single crystals (OSSCs) involving hydrogen bonds.

  20. Preparation and Characterization of Ag-Doped BaTiO3 Conductive Powders

    Directory of Open Access Journals (Sweden)

    Sue Hao


    Full Text Available BaTiO3 powders doped with Ag at different Ag/Ba molar ratios were prepared by sol-gel method. The resistivity reached the lowest point of 5.644 Ω·m when Ag concentration was 0.10 at% and the powders were calcined for two times at 800°C and 500°C. XRD and FTIR investigations showed that no new substance was formed after the doping and calcining process, but the particle size and the strength of Ti-O bond in modified BaTiO3 crystal cell all changed. The conductivity of Ag-doped BaTiO3 powders with different Ag concentrations and through different preparing methods was discussed by using defect theory.

  1. Synthesis of NiWO4 powder crystals of polyhedron for photocatalytic degradation of Rhodamine (United States)

    Hao, Meifeng; Meng, Xiangrui; Miao, Yuqing


    The NiWO4 powder crystals were synthesized by a simple hydrothermal method. It is found that the morphologies of most of NiWO4 particles are the polyhedron including cube, decahedron and dodecahedron et al. The typical cubic structures show the side length around 3 μm. SEM, TEM, XRD, FTIR and UV-vis were employed to characterize the NiWO4 powder crystals. The band gap value of 1.48 eV was calculated according to UV-vis. The NiWO4 powder crystals exhibit high photocatalytic activity toward the degradation of Rh B under both UV and visible irradiations. Especially, under UV, only 17% Rh B remains after 40 min UV photodegradation and only 80 min is needed for the complete degradation.

  2. Microstructure Evolution of Ni-Based ODS Superalloy Powders During Horizontal Rotary Ball Milling

    Directory of Open Access Journals (Sweden)

    Lee H.-E.


    Full Text Available Microstructure evolution of Ni-based oxide dispersion-strengthened alloy powders with milling time is investigated. The elemental powders having a nominal composition of Ni-15Cr-4.5Al-4W-2.5Ti-2Mo-2Ta-0.15Zr-1.1Y2O3 in wt % were ball-milled by using horizontal rotary ball milling with the change of milling velocity. Microstructure observation revealed that large aggregates were formed in the early stages of ball milling, and further milling to 5 h decreased particle size. The average crystalline size, estimated by the peak broadening of XRD, decreased from 28 nm to 15 nm with increasing milling time from 1 h to 5 h. SEM and EPMA analysis showed that the main elements of Ni and Cr were homogeneously distributed inside the powders after ball milling of 5 h.

  3. Fabrication of Single-Phase NiTi by Combustion Synthesis of Mechanically Activated Powders

    Directory of Open Access Journals (Sweden)

    S. Mousavi Nasab


    Full Text Available Single-phase NiTi was fabricated through the thermal explosion mode of combustion synthesis of mechanically activated powders. Combustion and ignition temperatures of combustion synthesis were investigated in different milling times. In this process, equiatomic powder mixtures of nickel and titanium were activated by planetary ball mill and pressed into disk-shaped pellets then heated in a tube furnace, while temperature-time profile was recorded. X-ray diffraction analysis (XRD was performed on milled powders as well as synthesized samples. Scanning electron microscopy (SEM was also used to study the microstructural evolution during milling. The results showed that there was a threshold milling time to obtain single-phase NiTi. It was also seen that the ignition temperature and combustion temperature were reduced significantly by increasing milling time.

  4. Fabrication of joint Bi-2223/Ag superconducting tapes with BSCCO superconducting powders by diffusion bonding

    Energy Technology Data Exchange (ETDEWEB)

    Guo Wei, E-mail: [School of Mechanical Engineering and Automation, Beihang University, Beijing 100191 (China); Department of Mechanical Engineering, Tsinghua University and Key Laboratory for Advanced Manufacturing by Materials Processing Technology, Ministry of Education of PR China, Beijing 100084 (China); Zou Guisheng; Wu Aiping; Zhou Fangbing; Ren Jialie [Department of Mechanical Engineering, Tsinghua University and Key Laboratory for Advanced Manufacturing by Materials Processing Technology, Ministry of Education of PR China, Beijing 100084 (China)


    61-Filaments Bi-2223/Ag superconducting tapes have been successfully joined with BSCCO superconducting powder interlayer by diffusion bonding. The electrical properties of the diffusion bonding joints were tested by standard four probe method and the microstructures of the joints were also examined by SEM. Additionally, the phase constituents of the superconducting powders between the tapes before and after bonding process were evaluated by XRD analysis. The result shows that the diffusion bonding joints are superconductive. The microstructures of the joint display a good bonding with no cracks and discontinuities. The joining zones are mainly composed of Bi-2223 phase, Bi-2212 phase and a small amount of CuO, Ca{sub 2}PbO{sub 4}. At last, the phase transformations of the superconducting powders in the bonding process are discussed.

  5. Preparation of YAG:Nd nano-sized powder by co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Li Xia; Liu Hong; Wang Jiyang; Cui Hongmei; Zhang Xudong; Han Feng


    Nd{sup 3+} doped yttrium aluminum garnet Y{sub 3}Al{sub 5}O{sub 12} (YAG) nano-sized powders were prepared by a co-precipitation method using hydroxypropyl cellulose (HPC) as dispersant. The formation process and structure of the as-prepared sample were investigated by means of TG-DTA, XRD, IR, and TEM. It has been found that the YAG powders were amorphous up to 700 deg. C and transformed into pure phase YAG crystallite at 900 deg. C for 2 h, because of the uniformly distribution of Al and Y elements. The size of YAG powder is about 30 nm in diameter and mono-disperse in the presence of HPC. Optical absorption and emission spectra of nano-crystallites versus Nd{sup 3+} concentration and sintering temperature were also studied.

  6. On the Methods to Measure Powder Flow. (United States)

    Tan, Geoffrey; Morton, David A V; Larson, Ian


    The flow of powders can often play a critical role in the manufacturing of pharmaceutical products. Many of these processes require good, consistent and predictable flow of powders to ensure continuous production of pharmaceutical dosages and to ensure their quality. Therefore, the flow of powders is of paramount importance to the pharmaceutical industry and thus the measuring and evaluating of powder flow is of utmost importance. At present, there are numerous methods in which the flow of powders can be measured. However, due to the complex and environment-dependent nature of powders, no one method exists that is capable of providing a complete picture of the behaviour of powders under dynamic conditions. Some of the most commonly applied methods to measure the flow of powders include: density indices, such as the Carr index and Hausner ratio, powder avalanching, the angle of repose (AOR), flow through an orifice, powder rheometry and shear cell testing.

  7. Development of a Reproducible Powder Characterization Method using a Powder Rheometer

    DEFF Research Database (Denmark)

    Søgaard, Søren Vinter; Allesø, Morten; Garnæs, Jørgen


    In this study, a powder rheometer was used to measure flow characteristics of two pharmaceutical model powders. Precise measurements were obtained for one of the model powders whereas the results were less precise for the second powder. In conclusion, further work is needed to increase...... the mechanistic understanding of powder rheological measurements....

  8. Cobalt ferrite nano-composite coated on glass by Doctor Blade method for photo-catalytic degradation of an azo textile dye Reactive Red 4: XRD, FESEM and DRS investigations. (United States)

    Habibi, Mohammad Hossein; Parhizkar, Janan


    Cobalt ferrite nano-composite was prepared by hydrothermal route using cobalt nitrate, iron nitrate and ethylene glycol as chelating agent. The nano-composite was coated on glass by Doctor Blade method and annealed at 300 °C. The structural, optical, and photocatalytic properties have been studied by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and UV-visible spectroscopy (UV-Vis DRS). Powder XRD analysis confirmed formation of CoFe2O4 spinel phase. The estimated particle size from FESEM data was 50 nm. The calculated energy band gaps, obtained by Tauc relation from UV-Vis absorption spectra was 1.3 eV. Photocatalytic degradation of Reactive Red 4 as an azo textile was investigated in aqueous solution under irradiation showed 68.0% degradation of the dye within 100 min. The experimental enhanced activity compare to pure Fe2O3 can be ascribed to the formation of composite, which was mainly attributable to the transfer of electron and hole to the surface of composite and hinder the electron hole recombination. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. XRD applied to the determination of pigments and composition of lithic materials and ceramics from archaeological pre-hispanic sites of the Rio de la Plata

    Energy Technology Data Exchange (ETDEWEB)

    Beovide, Laura [Department of Archeology, National Museum of Anthropology, Montevideo, (Uruguay); Pardo, Helena; Faccio, Ricardo; Mombru, Alvaro [Centro NanoMat, Polo Tecnologico de Pando, Facultad de Quimica, Universidad de la Republica, Pando, Canelones (Uruguay); Crystallography, Solid State and Materials Laboratory (Cryssmat-Lab), DETEMA, Facultad de Quimica, Universidad de la Republica, Gral, Montevideo (Uruguay); Piston, Mariela, E-mail: [Analytical Chemistry, Estrella Campos Department, Facultad de Quimica, Universidad de la Republica, Montevideo (Uruguay)


    Full text: The earliest records of human occupation on the lower basin of Santa Lucia River are dated ca. 4800 {sup 14}C years BP, in the area of one of the major tributaries of the Rio de la Plata on the Uruguayan coast. These societies were basically hunters and gatherers until ca. 3000 {sup 14}C years BP when they incorporated the horticulture. In this multidisciplinary work, two cases of application of XRD analysis of archaeological materials are presented to provide new perspectives in solving various problems related to the technological organization of these societies. In the first case, ceramics and pigments from an archaeological context prior to the hispanic-indian contact were analyzed. The X-ray powder diffraction patterns were obtained using a RIGAKU, Ultima IV with CBO monochromator, CuK{sub {alpha}} radiation was at 40 kV and 20 mA tube power at 0.02 deg/seg, operating in the range from 2{theta}=5.00 to 60.00 deg. According the comparison between the experimental recorded X-ray diffraction pattern to those stored in a X-ray powder diffraction database reveals that the piece of pottery is mainly constitute of quartz (SiO{sub 2}) and hematite (Fe{sub 2}O{sub 3}) while the mineral sample is probably composed mainly of quartz (SiO{sub 2}) and goethite (FeO{sub 3}.H{sub 2}O). The results allow a first approximation to know the inorganic pigments that were part of the decoration of the pottery and pigments used in the archaeological context. In the second case an amphibolite instrument from ca. 2700 {sup 14}C years BP related to a shell midden was analyzed and compared with amphibolites located 15 km of the archaeological site to assess if they were the raw materials for these instruments. Compositional XRD mineralogical analysis shows that the both samples seem to have similar mineral composition, which is mainly quartz (SiO{sub 2}) and a mixed sodium magnesium and calcium silicate (NaCa{sub 2}(Mg{sub 4}Ti)Si{sub 6}Al{sub 2}O{sub 23}(OH){sub 2}). This


    Directory of Open Access Journals (Sweden)

    Z. Sadeghian


    Full Text Available In situ Al2024- Mg2Si composite was fabricated by spark plasma sintering (SPS of reactive powder. Reactive powder was obtained from mechanical alloying (MA of elemental powders. Clad layers of in situ composite were fabricated on Al substrates by spark plasma sintering (SPS. Structural evolution during MA process and after SPS was investigated by X-ray diffractometery (XRD. Scanning electron microscopy (SEM was utilized to study the microstructure of sintered samples. Hardness and tensile behavior of sintered samples were investigated. The results showed that SPS of mechanically alloyed unreacted powder can result in the in situ formation of Mg2Si and Mg2Al3 within the Al matrix. SPSed clad layer showed a sound and clear interface to the Al substrate with a hardness of about 140 HV. Sintered in situ composite exhibited a tensile strength of 288 MPa.

  11. Nano or micro grained alumina powder? A choose before sintering

    Directory of Open Access Journals (Sweden)

    Román, R.


    Full Text Available Two different wet routes have been used to synthesize alumina powders in order to compare the characteristics of the final product and its behaviour during sintering. The Homogeneous Precipitation (HP gives rise to nanoparticulated powders of about 2 nm. However, such particles quickly aggregate and grow with calcination temperature. The Polymerized Organic-Inorganic Synthesis (POI produces homogeneous particle size powders (about 1 micron after resin charring. The characterization of the powder surface is the basis of an efficient process control. Particle characterization parameters (morphology, crystallinity and degree of aggregation are characterized by different techniques, such as DTA/TG, IR, XRD, SEM and TEM, and compared between these synthesis methods. The results show the evolution from the amorphous to the corundum alumina phase for both processes and their ability for sintering, as well discuses the beneficial of nanoparticles obtained by HP during sintering.

    Se han utilizado dos diferentes síntesis por vía húmeda para la preparación de polvos de alúmina con el fin de comparar las características de los productos finales y su comportamiento durante la sinterización. La Precipitación Homogénea (HP da lugar a polvos nanoparticulados de unos 2nm. Se observa sin embargo, como estas partículas se agregan rápidamente y crecen con la temperatura de calcinación. La Síntesis por Polimerización Orgánica-Inorgánica (POI produce polvos de tamaño de partícula homogéneo (en torno a 1 micra después de la descomposión de la resina. La caracterización de la superficie de los polvos es la base de un control eficiente del proceso. Los parámetros de caracterización de las partículas obtenidas (morfología, cristalinidad y grado de agregación se obtienen por diferentes técnicas como DTA/TG, IR, XRD, SEM y TEM, y se comparan entre estos métodos de síntesis. Los resultados muestran la evolución desde el amorfo a la fase

  12. XRD and DTA Analysis of Developed Agglomerated Fluxes for Submerged Arc Welding

    Directory of Open Access Journals (Sweden)

    Ajay Kumar


    Full Text Available A unique study of structural and chemical analysis of crystalline phases in developed agglomerated fluxes was carried out. Thirty-two fluxes were developed by using a mixture of oxides, halides, carbonates, silicates, and ferroalloys for submerged arc welding. The present paper focuses on only ten (out of thirty-two fluxes which were analyzed by X-ray diffraction (XRD to know the different types of oxides formed and changed in oxidation number of metallic centers after sintering process at around 850∘C. To know the effect of temperature over phase transformation and melting of different compounds, differential thermal analysis (DTA was carried out from 1000 to 1400∘C. This study aims to know the quantity of ions present (percentage and melting behavior of developed agglomerated fluxes for submerged arc welding process.

  13. In Situ Synchrotron XRD on a Capillary Li-O2 Battery Cell

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

    In situ studies give an opportunity to explore systems with a minimum of external interference. As Li-air batteries hold the promise for a future battery technology the investigation of the discharge and charge components of the cathode and anode is of importance, as these components may hold...... the key to making a large capacity rechargeable battery[1]. Different design for in situ XRD studies of Li-O2 batteries has been published, based on coin cell like configuration[2] [3] or Swagelok designs [4]. Capillary batteries have been investigated for the Li-ion system since its development[5......], but no capillary batteries of Li-air has yet been designed. Some of the advantage of the capillary battery design lies in its ability to separate the cathode and anode and avoid the use of glass fiber or separators, which may enable ex situ analysis of battery components. The battery design consist...

  14. Investigation of the reactions of chlorides binding to aluminates using XRD and DTA methods

    Directory of Open Access Journals (Sweden)

    Bikić Farzet H.


    Full Text Available The reactions of chlorides binding to aluminates were investigated by analyzing the monochloroaluminate hydrate, product of the reaction. The results show that the product is formed in the fresh concrete, after adding chloride within the stage of the preparation of concrete, as well as adding chlorides by penetration from the environment into the concrete. The obtained results are significant, considering the aspect of preventing corrosion of the steel reinforcement into the concrete. It is known that only free chlorides activate corrosion processes in the steel reinforcement in concrete. The process of chloride bonding is followed by X-ray diffraction (XRD and differential thermal (DTA analysis of samples of the cement paste, which is the process of preparation and care is described in detail in this work.

  15. Rancangan Eksperimen Analisis Struktur Mikro Sampel dengan Prinsip XRD Menggunakan Metode Kristal Berputar

    Directory of Open Access Journals (Sweden)

    Syaiful Rahman


    Full Text Available Pada penelitian ini dibuat rancangan alat peraga yang secara prinsip memiliki kinerja seperti XRD yang dapat digunakan untuk menentukan jenis struktur kristal dari suatu bahan dengan perhitungan indeks bidang melalui puncak-puncak spektrum yang dihasilkan. Laser difungsikan sebagai sinar-x, sedangkan bahan sampel digunakan manik-manik dari plastik yang berbentuk bulat. Untuk memutar sampel digunakan motor stepper. Selanjutnya untuk menangkap cahaya difraksi digunakan sensor cahaya (light sensor yang dihubungkan ke komputer. Data yang diperoleh berupa intensitas pada berbagai waktu dan diolah menggunakan microsoft excel untuk memperoleh posisi puncak dari difraksi serta indeks bidang. Hasil penelitian menunjukan bahwa rancangan alat eksperimen ini telah dapat bekerja dengan baik. Terbukti dapat menunjukkan intensitas puncak difraksi serta indeks bidangnya. Penelitian ini dapat digunakan sebagai pembelajaran fisika di perguruan tinggi, dengan produk berupa panduan praktikum fisika.

  16. Cryogenic Processing of HSS M2: Mechanical Properties and XRD Analysis

    Directory of Open Access Journals (Sweden)

    Sharma Ish Hunar


    Full Text Available The purpose of this study was to reveal the changes in properties of deep cryogenic treatment (DCT processed high speed steel, in comparison to conventional heat treatment for secondary hardness. Tool properties were assessed in terms of hardness, and tensile strength. Statistically significant enhancement in the mechanical properties was observed. Cryogenic processing of HSS tool steel eliminated the retained austenite, and hence increased the hardness of the material. This treatment initiated nucleation sites for precipitation of large numbers of very fine carbide particles.Tensile values for cryogenically treated HSS samples can be attributed to the fact that the tool becomes more brittle after the treatment. XRD analysis illustrated the contraction in lattice of martensite and austenite. Deep cryogenic treatment practically removed all traces of austenite in the sample. The superior performance of cryogenically treated HSS can be attributed to the transformation of almost all retained austenite into martensite, a harder structure and precipitation of fine and hard carbides.

  17. XRD and EPR structural investigation of some zinc borate glasses doped with iron ions (United States)

    Stefan, Razvan; Pascuta, Petru; Popa, Adriana; Raita, Oana; Indrea, Emil; Culea, Eugen


    Glasses in the system xFe2O3·(100-x) [45ZnO·55B2O3] (0≤x≤10 mol%) have been prepared by melting at 1200 °C and rapidly cooling at room temperature. The obtained samples were submitted to an additional thermal treatment at 570 °C for 12 h in order to relax the glass structure as well as to improve the local order. The as cast and heat treated samples were investigated using X-ray diffraction (XRD) and electron paramagnetic resonance (EPR) measurements. The XRD patterns of all the studied samples show their vitreous nature. Structural modifications occurring in the heat treated samples compared to the untreated ones have been pointed out. EPR spectra of untreated and heat treated samples revealed resonance absorptions centered at g≈2.0, g≈4.3 and g≈6.4. The compositional variation of the line intensity and linewidth of the absorptions from g≈4.3 and g≈2.0 have been interpreted in terms of the variation in the concentration of the Fe3+ ions and the interaction between the iron ions. The EPR spectra of the untreated samples containing 5 mol% Fe2O3 have been studied at different temperatures (110-290 K). The line intensity of the resonance signals decreases with increase in temperature whereas the linewidth is found to be independent of temperature. It was also found that the temperature variation of reciprocal line intensity obeys the Boltzmann law.

  18. Thermal decomposition of dolomite under CO2: insights from TGA and in situ XRD analysis. (United States)

    Valverde, Jose Manuel; Perejon, Antonio; Medina, Santiago; Perez-Maqueda, Luis A


    Thermal decomposition of dolomite in the presence of CO2 in a calcination environment is investigated by means of in situ X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The in situ XRD results suggest that dolomite decomposes directly at a temperature around 700 °C into MgO and CaO. Immediate carbonation of nascent CaO crystals leads to the formation of calcite as an intermediate product of decomposition. Subsequently, decarbonation of this poorly crystalline calcite occurs when the reaction is thermodynamically favorable and sufficiently fast at a temperature depending on the CO2 partial pressure in the calcination atmosphere. Decarbonation of this dolomitic calcite occurs at a lower temperature than limestone decarbonation due to the relatively low crystallinity of the former. Full decomposition of dolomite leads also to a relatively low crystalline CaO, which exhibits a high reactivity as compared to limestone derived CaO. Under CO2 capture conditions in the Calcium-Looping (CaL) process, MgO grains remain inert yet favor the carbonation reactivity of dolomitic CaO especially in the solid-state diffusion controlled phase. The fundamental mechanism that drives the crystallographic transformation of dolomite in the presence of CO2 is thus responsible for its fast calcination kinetics and the high carbonation reactivity of dolomitic CaO, which makes natural dolomite a potentially advantageous alternative to limestone for CO2 capture in the CaL technology as well as SO2in situ removal in oxy-combustion fluidized bed reactors.

  19. Effect of Ni content on microwave absorbing properties of MnAl powder

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Zhen-zhong; Lin, Pei-hao, E-mail:; Huang, Wei-chao; Pan, Shun-kang; Liu, Ye; Wang, Lei


    MnAlNi powder was prepared by the process of vacuum levitation melting and high-energy ball milling, The morphology and phase structure of the powder were analyzed by Scanning Electron Microscope(SEM), X-ray diffraction(XRD) and the effect of the Ni content on microwave absorbing properties of MnAl powder was investigated by an vector network analyzer. The addition of Ni, which improved the microwave absorbing properties of MnAl powder but not changed the composition of Al{sub 8}Mn{sub 5} alloy. The minimum reflectivity of (Al{sub 8}Mn{sub 5}){sub 0.95}Ni{sub 0.05} powder with a coating thickness (d) of 1.8 mm was about −40.8 dB and has better bandwidth effect, the absorbing mechanism of AlMnNi powders on the electromagnetic was related to the electromagnetic loss within the absorbing coatings and the effect of coating thickness on the interference loss of electromagnetic wave. - Highlights: • The grain size and cell volume of Al{sub 8}Mn{sub 5} alloy phase were decreased with the increasing of Ni. • ε″ and μ″ of powder moves toward low frequency region at the beginning then moves high. • The minimum reflectivity of (Al{sub 8}Mn{sub 5}){sub 0.95}Ni{sub 0.05} powder was −40.8 dB with 1.8 mm thickness. • The lowest reflection loss peak of (Al{sub 8}Mn{sub 5}){sub 0.95}Ni{sub 0.05} was −46.3 dB with 2.2 mm thickness.

  20. Morphological and structural characterization of the Zn{sub 0,9}Mn{sub 0,1}O powder synthesized by combustion reaction and Pechini; Caracterizacao estrutural e morfologica de pos de Zn{sub 0,9}Mn{sub 0,1}O sintetizados por reacao de combustao e metodo Pechini

    Energy Technology Data Exchange (ETDEWEB)

    Ribeiro, M.A.; Torquato, R.; Simoes, A.N.; Costa, A.C.F.M.; Gama, L., E-mail: [Universidade Federal de Campina Grande (DEMA/UFCG), PB (Brazil). Dept. de Engenharia dos Materiais; Kiminami, R.H.G.A. [Universidade Federal de Sao Carlos (DEMA/UFSCar), SP (Brazil). Dept. de Engenharia de Materiais


    Zinc oxide, due to the piezoelectric and electro-optical characteristics, is used in application such as, chemical sensor, varistor, transparent conductive thin film and DMS. The aim of this work is to evaluate and compare structural and morphological characteristics of nanometric powders of Zn{sub 0,9}Mn{sub 0,1}O prepared by chemical synthesis of combustion reaction and Pechini method. The powders were characterized by XRD, SEM and BET. The XRD data shown to both studied method the presence of ZnO phase with hexagonal structure and without second phase. The powder prepared by combustion reaction presented 9% of reduction in crystallinity and 42% of increase in surface area in comparison with the powder prepared by Pechini method. The morphological analysis of the powder showed that both method produce powders with soft agglomerates constituted by nano size particles. (author)

  1. Combined XRD and Raman studies of coke types found in SAPO-34 after methanol and propene conversion

    DEFF Research Database (Denmark)

    Wragg, David S.; Grønvold, Arne; Voronov, Alexey


    We have used a combination of high resolution powder X-ray diffraction (HRPD), Raman spectroscopy, in situ powder diffraction and nitrogen adsorption measurements to study the effect on and nature of coke in the zeotype catalyst SAPO-34 during the methanol to olefin (MTO) and propene oligomerisat...

  2. Electrodeposition of Fe powder from acid electrolytes

    Directory of Open Access Journals (Sweden)



    Full Text Available Polarization characteristics of the electrodeposition processes of Fe powders from sulfate and chloride electrolytes and the morphology of the obtained powders were investigated. The morphology depended on the anion presence in the electrolyte but not on the current density in the investigated range. A characteristic feature of the dendritic powder with cauliflower endings obtained from sulfate electrolyte is the presence of cone-like cavities and the crystallite morphology of the powders surface. On the other hand, Fe powders electrodeposited from chloride electrolyte appear in the form of agglomerates. A soap solution treatment applied as a method of washing and drying provides good protection from oxidation of the powders.

  3. Characterisation of mineralogical forms of barium and trace heavy metal impurities in commercial barytes by EPMA, XRD and ICP-MS. (United States)

    Ansari, T M; Marr, I L; Coats, A M


    This study was carried out to characterise the mineralogical forms of barium and the trace heavy metal impurities in commercial barytes of different origins using electron probe microanalysis (EPMA), X-ray diffraction (XRD) and inductively coupled plasma mass spectrometry (ICP-MS). Qualitative EPMA results show the presence of typically eight different minerals in commercial barytes including barite (BaSO4), barium feldspar, galena (PbS), pyrite (FeS2), sphalerite (ZnS), quartz (SiO2), and silicates, etc. Quantitative EPMA confirms that the barite crystals in the barytes contain some strontium and a little calcium, whereas trace heavy metals occur in the associated minerals. Analysis of aqua regia extracts of barytes samples by ICP-MS has shown the presence of a large number of elements in the associated minerals. Arsenic, copper and zinc concentrations correlate closely in all 10 samples. The findings suggest that barytes is not, as traditionally thought, an inert mineral, but is a potentially toxic substance due to its associated heavy metal impurities, which can be determined by an aqua regia digest without the need for complete dissolution of the barite itself. X-ray powder diffraction was not informative as the complex barite pattern masks the very weak lines from the small amounts of associated minerals.

  4. Nickel oxide reduction studied by environmental TEM and in situ XRD

    DEFF Research Database (Denmark)

    Jeangros, Q.; Hansen, Thomas Willum; Wagner, Jakob Birkedal


    Nickel oxide reduction and subsequent Ni behaviour under H2 is of practical importance in the field of solid oxide fuel cell (SOFC) technology, as it determines the structure of the electronic conductor on the anode side during operation [1]. Despite extensive coverage in the literature [2......], several questions remain, notably regarding the NiO reduction kinetics and its structural evolution. Here, we perform in situ reduction of an industrial NiO powder from JT Baker™ under 1.3 mbar of H2 (2 mlN/min) in a differentially pumped FEI Titan environmental transmission electron microscope (ETEM) [3......]. Images, diffraction patterns and electron energy-loss spectra are acquired during different temperature ramps (300 to 600°C) in order to monitor the structural and chemical evolution of the system. Similar experiments are performed in a PANalytical X'Pert PRO X-ray diffractometer equipped with an Anton...

  5. The New Method of XRD Measurement of the Degree of Disorder for Anode Coke Material

    Directory of Open Access Journals (Sweden)

    Zhuo Zhang


    Full Text Available Quantitative analysis by X-ray powder diffraction of two cokes (pitch coke and petroleum coke shows that their crystal structure changed with increasing temperature. The crystal data processing of the crystallization degree of disorder is used with further improvement of the proposed microcrystalline-stacking fault calculation method. With this improvement it is now possible to obtain the degree of stacking disorder of two cokes applied as anode materials at different graphitization temperatures. Raman spectroscopy verified the accuracy of this method, which is more reliable than the crystal structure refinement using the d002 method. This paper provides the theoretical analysis and interpretation of the relationship between the microstructure model of the material and quantitative data, discharge capacity, and the first charge-discharge efficiency.

  6. Nanostructured Polypyrrole Powder: A Structural and Morphological Characterization

    Directory of Open Access Journals (Sweden)

    Edgar A. Sanches


    Full Text Available Polypyrrole (PPY powder was chemically synthesized using ferric chloride (FeCl3 and characterized by X-ray diffraction (XRD, Le Bail Method, Fourier Transform Infrared Spectrometry (FTIR, and Scanning Electron Microscopy (SEM. XRD pattern showed a broad scattering of a semicrystalline structure composed of main broad peaks centered at 2θ = 11.4°, 22.1°, and 43.3°. Crystallinity percentage was estimated by the ratio between the sums of the peak areas to the area of amorphous broad halo due to the amorphous phase and showed that PPY has around 20 (1%. FTIR analysis allowed assigning characteristic absorption bands in the structure of PPY. SEM showed micrometric particles of varying sizes with morphologies similar to cauliflower. Crystal data (monoclinic, space group P 21/c, a=7.1499 (2 Å, b=13.9470 (2 Å, c=17.3316 (2 Å, α=90 Å, β=61.5640 (2 Å and γ=90 Å were obtained using the FullProf package program under the conditions of the method proposed by Le Bail. Molecular relaxation was performed using the density functional theory (DFT and suggests that tetramer polymer chains are arranged along the “c” direction. Average crystallite size was found in the range of 20 (1 Å. A value of 9.33 × 10−9 S/cm was found for PPY conductivity.

  7. Mask materials for powder blasting

    NARCIS (Netherlands)

    Wensink, H.; Jansen, Henricus V.; Berenschot, Johan W.; Elwenspoek, Michael Curt

    Powder blasting, or abrasive jet machining (AJM), is a technique in which a particle jet is directed towards a target for mechanical material removal. It is a fast, cheap and accurate directional etch technique for brittle materials such as glass, silicon and ceramics. The particle jet (which

  8. High resolution powder blast micromachining

    NARCIS (Netherlands)

    Wensink, H.; Berenschot, Johan W.; Jansen, Henricus V.; Elwenspoek, Michael Curt


    Powder blasting, or Abrasive Jet Machining (AJM), is a technique in which a particle jet is directed towards a target for mechanical material removal. It is a fast, cheap and accurate directional etch technique for brittle materials like glass, silicon and ceramics. By introducing electroplated

  9. Phonons from neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Dimitrov, D.A.; Louca, D.; Roeder, H. (Los Alamos National Laboratory, Los Alamos, New Mexico 87544 (United States))


    The spherically averaged structure function S([vert bar][bold q][vert bar]) obtained from pulsed neutron powder diffraction contains both elastic and inelastic scattering via an integral over energy. The Fourier transformation of S([vert bar][bold q][vert bar]) to real space, as is done in the pair density function (PDF) analysis, regularizes the data, i.e., it accentuates the diffuse scattering. We present a technique which enables the extraction of off-center ([vert bar][bold q][vert bar][ne]0) phonon information from powder diffraction experiments by comparing the experimental PDF with theoretical calculations based on standard interatomic potentials and the crystal symmetry. This procedure [dynamics from powder diffraction] has been [ital successfully] implemented as demonstrated here for two systems, a simple metal fcc Ni and an ionic crystal CaF[sub 2]. Although computationally intensive, this data analysis allows for a phonon based modeling of the PDF, and additionally provides off-center phonon information from neutron powder diffraction. [copyright] [ital 1999] [ital The American Physical Society

  10. Uranium Carbide Powder Ignition Studies

    Energy Technology Data Exchange (ETDEWEB)

    Berthinier, C.; Coullomb, S.; Rado, C.; Le Guyadec, F. [CEA, DEN, DTEC, SDTC, LEME, F-30207 Bagnols-sur-Ceze (France); Chatillon, C.; Blanquet, E.; Boichot, R. [SIMAP, Sciences et Ingenierie des Materiaux et Procedes, INPG-CNRS-UJF ENSEEG, BP 75, 38402 St Martin-d' Heres (France)


    Mixed (U, Pu) carbide, constituted by means of 80% of uranium monocarbide (UC), is considered as a possible fuel material for future gas fast reactors or sodium fast reactor. However, UC undergoes a strong exothermic reaction with air and fine powders of UC are pyrophoric. Thus, it is necessary to understand this high reactivity in order to determine safe handling conditions for the production and reprocessing of carbide fuels. UC powder was obtained by arc melting and milling. The reactivity of uranium carbide was studied in oxidizing atmosphere and different experimental devices were used to determine ignition temperatures. The phases formed at the various observed stages of the oxidation process were determined by post-mortem X ray diffraction analysis. Studies were first performed using small quantities of UC powder (around 50 mg) in Differential Thermal Analysis / Thermogravimetric Analysis (DTA/TGA) and Differential Scanning Calorimetry (DSC). Experiments were realized using different parameters, such as heating rate and gas flow rate and composition, to determine their influence on pyro-phoricity. Results obtained with small quantities (tens of milligrams) revealed that UC powder is highly reactive in air in the range 200- 250 deg. C. Studies were also performed in the 'Pyro' test facility multi-function furnace allowing CCD camera recording, during heating and ignition, through view-ports. Lower ignition temperatures, around 100 deg. C, were obtained using around 1 g UC powder samples. Results are discussed and analysed with theory of burning curve ignition and numerical simulations. Simulations aim to understand the influence of the different parameters on pyro-phoricity. Small scale simulations (on a spherical grain) confirm the influence of UC grains size, heat rate and gas composition on powder ignition temperature with small quantities. The issue is now to understand the influence of grain pile form factor and volume on the pyro-phoricity of

  11. XRD monitoring of α self-irradiation in uranium-americium mixed oxides. (United States)

    Horlait, Denis; Lebreton, Florent; Roussel, Pascal; Delahaye, Thibaud


    The structural evolution under (241)Am self-irradiation of U(1-x)Am(x)O(2±δ) transmutation fuels (with x ≤ 0.5) was studied by X-ray diffraction (XRD). Samples first underwent a preliminary heat treatment performed under a reducing atmosphere (Ar/H2(4%)) aiming to recover the previously accumulated structural defects. Over all measurements (carried out over up to a full year and for integrated doses up to 1.5 × 10(18) α-decay events·g(-1)), only fluorite U(1-x)Am(x)O(2±δ) solid solutions were observed. Within a few days after the end of the heat treatment, each of the five studied samples was slowly oxidized as a consequence of their move to air atmosphere, which is evidenced by XRD by an initial sharp decrease of the unit cell parameter. For the compounds with x ≤ 0.15, this oxidation occurred without any phase transitions, but for U0.6Am0.4O(2±δ) and U0.5Am0.5O(2±δ), this process is accompanied by a transition from a first fluorite solid solution to a second oxidized one, as the latter is thermodynamically stable in ambient conditions. In the meantime and after the oxidation process, (241)Am α self-irradiation caused a structural swelling up to ∼0.8 vol %, independently of the sample composition. The kinetic constants of swelling were also determined by regression of experimental data and are, as expected, dependent on x and thus on the dose rate. The normalization of these kinetic constants by sample α-activity, however, leads to very close swelling rates among the samples. Finally, evolutions of microstrain and crystallite size were also monitored, but for the considered dose rates and cumulated doses, α self-irradiation was found, within the limits of the diffractometer used, to have almost no impact on these characteristics. Microstrain was found to be influenced instead by the americium content in the materials (i.e., by the impurities associated with americium starting material and the increase of cationic charge heterogeneity with

  12. Synchrotron-based XRD from rat bone of different age groups. (United States)

    Rao, D V; Gigante, G E; Cesareo, R; Brunetti, A; Schiavon, N; Akatsuka, T; Yuasa, T; Takeda, T


    Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca10(PO4)6(OH)2] bone fill with varying composition (60% and 70%) and bone cream (35-48%), has been acquired with 15keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15keV X-rays (λ=0.82666 A0). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P63/m with the lattice parameters of a=9.4328Å and c=6.8842Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100μm resolution. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Data from the Mars Science Laboratory CheMin XRD/XRF Instrument (United States)

    Vaniman, David; Blake, David; Bristow, Tom; DesMarais, David; Achilles, Cherie; Anderson, Robert; Crips, Joy; Morookian, John Michael; Spanovich, Nicole; Vasavada, Ashwin; hide


    The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity uses a Co tube source and a CCD detector to acquire mineralogy from diffracted primary X-rays and chemical information from fluoresced X-rays. CheMin has been operating at the MSL Gale Crater field site since August 5, 2012 and has provided the first X-ray diffraction (XRD) analyses in situ on a body beyond Earth. Data from the first sample collected, the Rocknest eolian soil, identify a basaltic mineral suite, predominantly plagioclase (approx.An50), forsteritic olivine (approx.Fo58), augite and pigeonite, consistent with expectation that detrital grains on Mars would reflect widespread basaltic sources. Minor phases (each <2 wt% of the crystalline component) include sanidine, magnetite, quartz, anhydrite, hematite and ilmenite. Significantly, about a third of the sample is amorphous or poorly ordered in XRD. This amorphous component is attested to by a broad rise in background centered at approx.27deg 2(theta) (Co K(alpha)) and may include volcanic glass, impact glass, and poorly crystalline phases including iron oxyhydroxides; a rise at lower 2(theta) may indicate allophane or hisingerite. Constraints from phase chemistry of the crystalline components, compared with a Rocknest bulk composition from the APXS instrument on Curiosity, indicate that in sum the amorphous or poorly crystalline components are relatively Si, Al, Mg-poor and enriched in Ti, Cr, Fe, K, P, S, and Cl. All of the identified crystalline phases are volatile-free; H2O, SO2 and CO2 volatile releases from a split of this sample analyzed by the SAM instrument on Curiosity are associated with the amorphous or poorly ordered materials. The Rocknest eolian soil may be a mixture of local detritus, mostly crystalline, with a regional or global set of dominantly amorphous or poorly ordered components. The Rocknest sample was targeted by MSL for "first time analysis" to demonstrate that a loose deposit could be scooped, sieved to

  14. Polymer quenched prealloyed metal powder (United States)

    Hajaligol, Mohammad R.; Fleischhauer, Grier; German, Randall M.


    A powder metallurgical process of preparing a sheet from a powder having an intermetallic alloy composition such as an iron, nickel or titanium aluminide. The sheet can be manufactured into electrical resistance heating elements having improved room temperature ductility, electrical resistivity, cyclic fatigue resistance, high temperature oxidation resistance, low and high temperature strength, and/or resistance to high temperature sagging. The iron aluminide has an entirely ferritic microstructure which is free of austenite and can include, in weight %, 4 to 32% Al, and optional additions such as .ltoreq.1% Cr, .gtoreq.0.05% Zr .ltoreq.2% Ti, .ltoreq.2% Mo, .ltoreq.1% Ni, .ltoreq.0.75% C, .ltoreq.0.1% B, .ltoreq.1% submicron oxide particles and/or electrically insulating or electrically conductive covalent ceramic particles, .ltoreq.1% rare earth metal, and/or .ltoreq.3 % Cu. The process includes forming a non-densified metal sheet by consolidating a powder having an intermetallic alloy composition such as by roll compaction, tape casting or plasma spraying, forming a cold rolled sheet by cold rolling the non-densified metal sheet so as to increase the density and reduce the thickness thereof and annealing the cold rolled sheet. The powder can be a water, polymer or gas atomized powder which is subjecting to sieving and/or blending with a binder prior to the consolidation step. After the consolidation step, the sheet can be partially sintered. The cold rolling and/or annealing steps can be repeated to achieve the desired sheet thickness and properties. The annealing can be carried out in a vacuum furnace with a vacuum or inert atmosphere. During final annealing, the cold rolled sheet recrystallizes to an average grain size of about 10 to 30 .mu.m. Final stress relief annealing can be carried out in the B2 phase temperature range.

  15. Solution-combustion synthesis and photoluminescence properties of YBO3:Tb3+ phosphor powders (United States)

    Onani, Martin O.; Okil, Joseph O.; Dejene, Francis B.


    YBO3:Tb3+ nanocrystalline phosphors were successfully deposited by a solution-combustion method, using rare-earth nitrates, urea and boric acid as starting materials. The crystal structure, morphology, chemical composition and photoluminescence properties of the films were investigated by X-ray diffraction (XRD) and atomic force microscopy (AFM). The results of SEM and XRD revealed that the powders were composed of spherical YBO3:Tb3+ nanocrystals with average grain size of between 50 and 100 nm. The electron diffraction spectroscopy (EDS) confirmed the presence of the Y, B, O, and C. The XRD measurements revealed YBO3:Tb3+ (JCPDS:83-1205) structure when annealed at 1000 °C for 2 h. The YBO3:Tb3+ powders exhibited emissions at 490, 545 and 585 nm, which were assigned to the 5D4-7F6, 5D4-7F5 and 5D4-7F4 transitions of Tb3+, respectively. Among them, the green emission at 545 nm (5D4-7F5) was dominant.

  16. Structural and magnetic properties of turmeric functionalized CoFe2O4 nanocomposite powder (United States)

    Mehran, E.; Farjami Shayesteh, S.; Sheykhan, M.


    The structural and magnetic properties of the synthesized pure and functionalized CoFe2O4 magnetic nanoparticles (NPs) are studied by analyzing the results from the x-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR spectroscopy, thermogravimetry (TG), and vibrating sample magnetometer (VSM). To extract the structure and lattice parameters from the XRD analysis results, we first apply the pseudo-Voigt model function to the experimental data obtained from XRD analysis and then the Rietveld algorithm is used in order to optimize the model function to estimate the true intensity values. Our simulated intensities are in good agreement with the experimental peaks, therefore, all structural parameters such as crystallite size and lattice constant are achieved through this simulation. Magnetic analysis reveals that the synthesized functionalized NPs have a saturation magnetization almost equal to that of pure nanoparticles (PNPs). It is also found that the presence of the turmeric causes a small reduction in coercivity of the functionalized NPs in comparison with PNP. Our TGA and FTIR results show that the turmeric is bonded very well to the surface of the NPs. So it can be inferred that a nancomposite (NC) powder of turmeric and nanoparticles is produced. As an application, the anti-arsenic characteristic of turmeric makes the synthesized functionalized NPs or NC powder a good candidate for arsenic removal from polluted industrial waste water. Project supported by the University of Guilan and the Iran Nanotechnology Initiative Council.

  17. Characterization of Ni ferrites powders prepared by plasma arc discharge process (United States)

    Safari, A.; Gheisari, Kh.; Farbod, M.


    The aim of this work was to synthesize a single-phase spinel structure from a mixture of zinc, iron and nickel powders by plasma arc discharge method. A mixture of zinc, iron and nickel powders with the appropriate molar ratio was prepared and formed into a cylindrical shape. The synthesis process was performed in air, oxygen and argon atmospheres with the applied arc current of 400 A and pressure of 1 atm. After establishing an arc between the electrodes, the produced powders were collected and their structure and magnetic properties were examined by XRD and VSM, respectively. ZnO as an impurity was appeared in the as-produced powders owing to the high reactivity of zinc atoms, preventing the formation of Ni-Zn ferrite. A pure spinel structure with the highest saturation magnetization (43.8 emu/g) was observed as zinc powders removed completely from the initial mixture. Morphological evaluations using field emission scanning electron microscopy showed that the mean size of fabricated nanoparticles was in the range 100-200 nm and was dependent on the production conditions.

  18. Correlation between morphology and magnetic properties of electrochemically produced cobalt powder particles

    Directory of Open Access Journals (Sweden)

    Maksimović Vesna M.


    Full Text Available Cobalt 3D powder particles were successfully prepared by the galvanostatic electrodeposition. Electrodeposited cobalt powder were characterized by X-ray diffraction (XRD, scanning electron microscope (SEM, Energy Dispersive Spectroscopy (EDS analysis and SQUID magnetometry. It has been shown that morphology, structure and magnetic properties of cobalt particles are closely associated and can be easily controlled by adjusting process parameters of electrodeposition. Morphology of cobalt powder particles is strongly affected by hydrogen evolution reaction as a parallel reaction to cobalt electrodeposition. Depending on the applied current density, the two types of powder particles were formed: dendrites at lower and spongy-like particles at higher current densities. Morphologies and structures of powder particles are correlated with their magnetic properties, and compared with those of the bulk cobalt. In comparison with the properties of bulk cobalt, the obtained 3D structures exhibited a decreased saturation magnetization (MS, but an enhanced coercivity (HC which is explained by their peculiar morphology. [Projekat Ministarstva nauke Republike Srbije, br. III 45012

  19. A 4-(o-chlorophenyl)-2-aminothiazole: Microwave assisted synthesis, spectral, thermal, XRD and biological studies (United States)

    Rajmane, S. V.; Ubale, V. P.; Lawand, A. S.; Nalawade, A. M.; Karale, N. N.; More, P. G.


    A 4-(o-chlorophenyl)-2-aminothiazole (CPAT) has been synthesized by reacting o-chloroacetophenone, iodine and thiourea under microwave irradiation as a green chemistry approach. The reactions proceed selectively and within a couple of minutes giving high yields of the products. The compound was characterized by elemental, spectral (UV-visible, IR, NMR and GC-MS), XRD and thermal analyses. The TG curve of the compound was analyzed to calculate various kinetic parameters (n, E, Z, ΔS and ΔG) by using Coats-Redfern (C.R.), MacCallum-Tanner (M.T.) and Horowitz-Metzger (H.M.) method. The compound was tested for the evaluation of antibacterial activity against B. subtilis and E. coli and antifungal activity against A. niger and C. albicans. The compound was evaluated for their in vitro nematicidal activity on plant parasitic nematode Meloidogyne javanica and molluscicidal activity on fresh water helminthiasis vector snail Lymnea auricularia. The compound is biologically active in very low concentration. X-ray diffraction study suggests a triclinic crystal system for the compound.

  20. Modeling the PbI2 formation in perovskite solar cells using XRD/XPS patterns (United States)

    Sohrabpoor, Hamed; Elyasi, Majid; Aldosari, Marouf; Gorji, Nima E.


    The impact of prolonged irradiation and air humidity on the stability of perovskite solar cells is modeled using X-ray diffraction and X-ray photoelectron spectroscopy patterns reported in the literature. Light or air-moisture causes the formation of a thin PbI2 or oxide defective layers (in nanoscale) at the interface of perovskite/hole-transport-layer or at the junction with metallic back contact. This thin layer blocks the carrier transport/passivation at the interfaces and cause degradation of device parameters. Variation in thickness of defective layers, changes the XRD and XPS peaks. This allows detection and estimation of the type, crystallinity and thickness of the defective layer. A simple model is developed here to extract the thickness of such thin defective layers formed in nanometer scale at the back region of several perovskite devices. Based on this information, corrected energy band diagram of every device before and after degradation/aging is drawn and discussed in order to obtain insight into the carrier transport and charge collection at the barrier region. In addition, graphene contacted perovskite devices are investigated showing that honey-comb network of graphene contact reduces the effect of aging leading to formation of a thinner defective layer at the perovskite surface compared to perovskite devices with conventional inorganic contacts i.e. Au, Al.

  1. [Spectroscopic analysis of the crystallization mechanism of synthesized zeolite with XRD and FTIR approaches]. (United States)

    Fan, Chun-hui; Ma, Hong-rui; Hua, Li


    Zeolites were synthesized from fly ash using modified one-stage method. The changes in cation exchange capacity (CEC) and chemical elements of zeolite were investigated during the synthesis process to reveal the materials and elements transformation in solid-liquid system. The approaches of XRD, SEM and FTIR were used to indicate the crystallization characteristics and mechanism. The zeolite NaP1 was synthesized, and the CEC value reached to the maximum of 135 mmol/100g at 24 h. After the hydrothermal reaction for 12 h, the characteristic peak and metastable crystalline structure of zeolite NaP1 appeared, then the hydroxy sodalite products formed at 48 h. The crystallization process was the result of materials transformation: the elements of fly ash released into the liquid system for the melting effect of alkali solution, and the solid system played the role of skeleton in crystallization process, being the "source" and the "sink" of the reaction, respectively, and the achievements presented the crystallization mechanism of liquid-phase and solid-phase transformation.

  2. Synthesis, XRD, TEM, EPR, and Optical Absorption Spectral Studies of CuZnO2 Nanocompound

    Directory of Open Access Journals (Sweden)

    T. Ravindra Reddy


    Full Text Available Synthesis of nano CuZnO2 compound is carried out by thermal decomposition method. The crystalline phase of the material is characterized by XRD. The calculated unit cell constants are a=3.1 Å and c=3.4786 Å and are of tetragonal structure. The unit cell constants are different from wurtzite (hexagonal which indicate that a nanocompound is formed. Further TEM images reveal that the metal ion is in tetragonal structure with oxygen ligands. The prepared CuZnO2 is then characterized for crystallite size analysis by employing transmission electron microscopy (TEM. The size is found to be 100 nm. Uniform bright rings are noticed in the TEM picture suggesting that the nanocrystals have preferential instead of random orientations. The selected-area electron diffraction (SAED pattern clearly indicates the formation of CuO-ZnO nanocompound. The nature of bonding is studied by electron paramagnetic resonance (EPR. The covalency character is about 0.74 and thus the compound is electrically less conductive. Optical absorption spectral studies suggest that Cu(II is placed in tetragonal elongation crystal field. The spin-orbit coupling constant, λ, is calculated using the EPR and optical absorption spectral results suggest some covalent bond between metal and ligand. Near infrared (NIR spectra are due to hydroxyl and water fundamentals.

  3. Structural investigations of (La,Pu)PO4 monazite solid solutions: XRD and XAFS study (United States)

    Arinicheva, Yulia; Popa, Karin; Scheinost, Andreas C.; Rossberg, André; Dieste-Blanco, Oliver; Raison, Philippe; Cambriani, Andrea; Somers, Joseph; Bosbach, Dirk; Neumeier, Stefan


    A solid state method was used to synthesize La1-xPuxPO4 (x = 0.01, 0.05, 0.10, 0.15, (0.5)) solid solutions with monazite structure. XRD measurements of the compounds with x = 0.50 revealed the formation of two phases: (La,Pu)PO4-monazite and a cubic phase (PuO2). Pure-phase La1-xPuxPO4-monazite solid solutions were obtained for materials with x = 0.00-0.15 and confirmed by a linear dependence of the lattice parameters on composition according to Vegard's law. X-ray absorption spectroscopy (XAS) analysis at the Pu-LIII and La-LIII edges confirmed the +III valence state of plutonium in the monazite solid solutions. The local environment of Pu is PuPO4-like along the solid solution series, except for the longest fitted cation-cation distance, which may be an indication of cluster formation consisting of a few Pu-atoms in the La-Pu-monazite lattice.

  4. Radiation Crosslinking of Polyurethanes: Characterization by FTIR, TGA, SEM, XRD, and Raman Spectroscopy

    Directory of Open Access Journals (Sweden)

    Mohamed Mohamady Ghobashy


    Full Text Available Gamma radiation can be used for enhancing the physical properties of polyurethane (PU. Radiation was used to crosslink a polyurethane at room temperature; four samples of the PU solid film are irradiated at variable four radiation doses 0, 50, 100, and 150 kGy under vacuum conditions. Crosslinking radiation is more common than oxidative degradation and crosslinking is believed to be more efficient in the soft segment of PU. The structure of the PUs is performed by Fourier transform infrared (FTIR-ATR, Thermogravimetric Analysis (TGA-DTG, and X-ray Diffraction (XRD which have been used to investigate the effect of gamma radiation on the polyurethane (PU. The results showed that the radiation crosslinking of polyurethanes improved the thermal stability and the crystallinity. The microstructure modifications of polyurethane samples have also been studied as a function of the dose using the scanning electron microscope (SEM. The effects of gamma irradiation on the color changes of polyurethane were observed. The irradiated PUs have conjugated structure and are capable of emitting purple fluorescence.

  5. Mössbauer, XRD, and Complex Thermal Analysis of the Hydration of Cement with Fly Ash

    Directory of Open Access Journals (Sweden)

    Vili Lilkov


    Full Text Available Hydration of cement with and without fly ash is studied with Mössbauer spectroscopy, XRD, and thermal analysis. Iron in cement is present as Fe3+-ions and occupies two octahedral positions, with close isomer shifts and quadrupole splittings. Iron in fly ash is present as Fe2+ and Fe3+, and the Mössbauer spectra display three doublets—two for Fe3+ in octahedral coordination and one for Fe2+. A third doublet was registered in the hydrating plain cement pastes after the 5th day, due to Fe3+ in tetrahedral coordination in the structure of the newly formed monosulphate aluminate. In cement pastes with fly ash, the doublet of tetrahedral iron is formed earlier because the quantity of ettringite and portlandite is low and more monosulphate crystallizes. No Fe(OH3 phase forms during hydration of C4AF. The fly ash displays pozzolanic properties, which lead to lowering of the portlandite quantity in the cement mixtures and increasing of the high temperature products.

  6. The Potential Impact of Biofield Energy Treatment on the Physical and Thermal Properties of Silver Oxide Powder


    Mahendra, Trivedi; Alice, Branton; Dahryn, Trivedi; Gopal, Nayak


    Silver oxide has gained significant attention due to its antimicrobial activities. The purpose of this study was to evaluate the impact of biofield energy treatment on the physical and thermal properties of silver oxide (Ag2O). The silver oxide powder was divided into two parts, one part was kept as control and another part was received Mr. Trivedi's biofield energy treatment. The control and treated samples were analyzed using X-ray diffraction (XRD), differential scanning calorimetry (DSC),...

  7. 21 CFR 73.2645 - Aluminum powder. (United States)


    ... 21 Food and Drugs 1 2010-04-01 2010-04-01 false Aluminum powder. 73.2645 Section 73.2645 Food and... ADDITIVES EXEMPT FROM CERTIFICATION Cosmetics § 73.2645 Aluminum powder. (a) Identity and specifications. The color additive aluminum powder shall conform in identity and specifications to the requirements of...

  8. 21 CFR 73.1645 - Aluminum powder. (United States)


    ... 21 Food and Drugs 1 2010-04-01 2010-04-01 false Aluminum powder. 73.1645 Section 73.1645 Food and... ADDITIVES EXEMPT FROM CERTIFICATION Drugs § 73.1645 Aluminum powder. (a) Identity. (1) The color additive aluminum powder shall be composed of finely divided particles of aluminum prepared from virgin aluminum. It...

  9. Metallurgical Characterization of Aluminum Powder Consolidation. (United States)


    theoretical density could be obtained by cold compacting Al powder. The apparent lack of inter- particle bonding in Figure 13 is due to heavy etching of the...34 ring seal Crimp hold Figure 39. Powder pack as assembled. 47 • .U % . * .,Z . % Ignition PVC tube (21.6 cm O.D., 20 cm l.D.) ON 30cm Powder pack ANFO

  10. 21 CFR 520.1696a - Buffered penicillin powder, penicillin powder with buffered aqueous diluent. (United States)


    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Buffered penicillin powder, penicillin powder with... FORM NEW ANIMAL DRUGS § 520.1696a Buffered penicillin powder, penicillin powder with buffered aqueous diluent. (a) Specifications. When reconstituted, each milliliter contains penicillin G procaine equivalent...

  11. [Impact of directly compressed auxiliary materials on powder property of fermented cordyceps powder]. (United States)

    Chen, Li-Hua; Yue, Guo-Chao; Guan, Yong-Mei; Yang, Ming; Zhu, Wei-Feng


    To investigate such physical indexes as hygroscopicity, angle of repose, bulk density, fillibility of compression of mixed powder of directly compressed auxiliary materials and fermented cordyceps powder by using micromeritic study methods. The results showed that spray-dried lactose Flowlac100 and microcrystalline cellulose Avicel PH102 had better effect in liquidity and compressibility on fermented cordyceps powder than pregelatinized starch. The study on the impact of directly compressed auxiliary materials on the powder property of fermented cordyceps powder had guiding significant to the research of fermented cordyceps powder tablets, and could provide basis for the development of fermented cordyceps powder tablets.

  12. Mechanical stimulated reaction of metal/polymer mixed powders; Kinzoku/kobunshi kongo funmatsu no kikaiteki reiki hanno

    Energy Technology Data Exchange (ETDEWEB)

    Tobita, M.; Sakakibara, A.; Takemoto, Y. [Okayama University, Okayama (Japan). Faculty of Engineering; Iwabu, H. [Kurare Co. Ltd., Osaka (Japan)


    Mechanical grinding (MG) with mechanically stimulated reaction was performed on metal/polymer mixed powders. The starting materials used in this study were the metals of Mg, Ti and Mg{sub 2}Ni powders, arid polymer of PTFE, PVC and PE powders. The MG process was investigated using XRD, IR, SEM and TEM. According to XRD results, magnesium fluoride (MgF{sub 2}, TiF{sub 2}) and chloride (MgCl{sub 2}) were detected from MG products of the Mg/PTFE, Ti/PTFE and Mg/PVC blending systems, respectively. Explosive reaction was found during MG of both Mg/PTFE and Ti/PTFE. It was also confirmed by XRD results that the production of MgF{sub 2} had already been formed just before the explosive reaction in Mg/PTFE system. It was found from IR analysis that C-C single bond in the polymers, not only both in PTFE and PVC but also in PE, changed to double bond C=C. Hydrogen produced due to decomposition of PE on blending Mg{sub 2}Ni/PE was absorbed into C-Mg{sub 2}Ni-H as amorphous solutes. These mechanically stimulated reaction was powerful method for decomposition of engineering plastics. (author)

  13. Synthesis of La{sup 3+} doped nanocrystalline ceria powder by urea-formaldehyde gel combustion route

    Energy Technology Data Exchange (ETDEWEB)

    Biswas, M. [Central Glass and Ceramic Research Institute, Kolkata 700 032 (India); Bandyopadhyay, S., E-mail: [Central Glass and Ceramic Research Institute, Kolkata 700 032 (India)


    Highlights: Black-Right-Pointing-Pointer Nano LC synthesized by gel combustion, using urea-formaldehyde fuel for first time. Black-Right-Pointing-Pointer Largely single crystals were produced in average range of 20-30 nm. Black-Right-Pointing-Pointer La{sup 3+} doping increases cell dimension linearly. Black-Right-Pointing-Pointer La{sup 3+} doping introduces ionic point defects but does not change electronic band gap. Black-Right-Pointing-Pointer Presence of Ce{sup 3+} indicates that this synthesis route produces reactive powders. -- Abstract: Nanocrystalline ceria powders doped with various concentrations of lanthanum oxide have been prepared following gel combustion route using for the first time urea-formaldehyde as fuel. The synthesized products were characterized by XRD, FESEM, TEM, PL and UV-vis spectroscopy. Peak positions of XRD were refined and the lattice parameters were obtained by applying Cohen's method. Unit cell parameter increases with concentration of La{sup 3+} ion and the variation is consistently linear. XRD calculations showed the dependence of crystallite size on dopant concentrations at lower level. TEM observation revealed unagglomerated particles to be single crystals in the average range of 20-30 nm. Band gap of the La{sup 3+} doped ceria materials does not change with doping. Spectroscopic experiments proved the existence of Ce{sup 3+} in the formed powder.

  14. Structural determination of Co/TiO2 nanocomposite: XRD technique and simulation analysis

    Directory of Open Access Journals (Sweden)

    Mostaghni F.


    Full Text Available Synthesis and complex theoretical and experimental studies of Co/TiO2 anatase have been reported. The preparation of Co/TiO2 was carried out by sol-gel method. Distribution of cations among the two tetrahedral and octahedral sites was estimated by analyzing the powder X-ray diffraction patterns by employing Rietveld refinement technique, and the results revealed the existence of tetragonal structure. Band structure and density of states calculations were performed using the first-principles methods. The structural and electronic properties of Co/TiO2 were calculated in the general gradient approximation (GGA. An additional comparison with pure TiO2 anatase allowed us to clarify cobalt doping effect on the electronic structure and the band gap. The band gap of Co/TiO2 was decreased by broadening the valence band as a result of the overlap among Co 3d, Ti 3d, and O 2p states, which made it respond better to visible and solar light.

  15. Data from the Mars Science Laboratory CheMin XRD/XRF instrument (United States)

    Vaniman, David; Bristow, , David Blake, Tom; Des Marais, David; Achilles, Cherie; Spanovich, Ashwin Vasavada, , Robert Anderson, Joy Crisp, John Michael Morookian, Nicole; Yen, Albert; Bish, David; Chipera, Steve; Downs, Robert; Morrison, Shaunna; Farmer, Jack; Grotzinger, John; Stolper, Edward; Morris, , Douglas Ming, Richard; Rampe, Elizabeth; Treiman, Allan; Sarrazin, Philippe; MSL Science Team


    The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity uses a Co tube source and a CCD detector to acquire mineralogy from diffracted primary X-rays and chemical information from fluoresced X-rays. CheMin has been operating at the MSL Gale Crater field site since August 5, 2012 and has provided the first X-ray diffraction (XRD) analyses in situ on a body beyond Earth. Data from the first sample collected, the Rocknest eolian soil, identify a basaltic mineral suite, predominantly plagioclase (~An50), forsteritic olivine (~Fo58), augite and pigeonite, consistent with expectation that detrital grains on Mars would reflect widespread basaltic sources. Minor phases (each allophane or hisingerite. Constraints from phase chemistry of the crystalline components, compared with a Rocknest bulk composition from the APXS instrument on Curiosity, indicate that in sum the amorphous or poorly crystalline components are relatively Si, Al, Mg-poor and enriched in Ti, Cr, Fe, K, P, S, and Cl. All of the identified crystalline phases are volatile-free; H2O, SO2 and CO2 volatile releases from a split of this sample analyzed by the SAM instrument on Curiosity are associated with the amorphous or poorly ordered materials. The Rocknest eolian soil may be a mixture of local detritus, mostly crystalline, with a regional or global set of dominantly amorphous or poorly ordered components. The Rocknest sample was targeted by MSL for "first time analysis" to demonstrate that a loose deposit could be scooped, sieved to <150 µm, and delivered to instruments in the body of the rover. A drilled sample of sediment in outcrop is anticipated. At the time of writing this abstract, promising outcrops are in range and this talk will provide an update on data collected with the CheMin instrument.

  16. Changes in selected oxysterols in powdered foodstuffs

    Directory of Open Access Journals (Sweden)

    Sylwia Chudy


    Full Text Available The present research consisted of producing 3 types of powdered concentrates: the dairy, the egg and the dairy-egg (produced from a blend of raw liquid milk and liquid eggs. The dairy-egg powder was produced in order to facilitate formulation of dry food mixes. Powders were vacuumpackaged and packaged in air atmosphere and stored for 24 months. Changes in contents of selected oxysterols (determined by gas chromatography were recorded. Regardless of the packaging type, the predominant oxysterol in the dairy-egg powder was α-epoxy-C (7.679 and 5.600 μg/g powder, respectively.

  17. [Advances in studies on bear bile powder]. (United States)

    Zhou, Chao-fan; Gao, Guo-jian; Liu, Ying


    In this paper, a detailed analysis was made on relevant literatures about bear bile powder in terms of chemical component, pharmacological effect and clinical efficacy, indicating bear bile powder's significant pharmacological effects and clinical application in treating various diseases. Due to the complex composition, bear bile powder is relatively toxic. Therefore, efforts shall be made to study bear bile powder's pharmacological effects, clinical application, chemical composition and toxic side-effects, with the aim to provide a scientific basis for widespread reasonable clinical application of bear bile powder.

  18. Preparation of antimony trioxide powder

    Energy Technology Data Exchange (ETDEWEB)

    Park, Hyung Kyu; Jang, Hee Dong; Km, Joon Soo; Lim, Young Woong; Kim, Sung Don; Yoon, Ho Sung; Lee, Hoo In; Kim, Chul Joo [Korea Institute of Geology Mining and Materials, Taejon (Korea)


    Antimony trioxide is used as flame retardant material in plastic, rubber, and textile industries. It was carried out to establish processing technology of antimony trioxide, and provide for smelting of metallic antimony by domestic industries. Also, domestic market of antimony trioxide was surveyed. Commercial antimony trioxide has been manufactured through two steps : the first is to extract antimony metal from Stibnite ore, and the second is to evaporate and oxidize metallic antimony. In this study, it was focused on the second step because primary antimony has not been produced domestically. An equipment for melting and vaporizing of metallic antimony was experimentally prepared. Antimony metal was melted in magnesia crucible, and reacted with air to oxidize into antimony trioxide powder in the equipment by use of suction blower. The powder was collected through bag filter. The crystal form of the antimony trioxide sample was senarmontite. The shape of the powder was widely spherical. It is considered that antimony trioxide could be prepared effectively through the experiment. (author). 9 figs.

  19. Dynamic compaction of ceramic powders

    Energy Technology Data Exchange (ETDEWEB)

    Cline, C.F.


    Dynamic consolidation is a technique for densifying powder ensembles to near theoretical with or without external application of heat. The technique itself is simple: the confined powder, initially at a green density of approx. 50% encounters a high pressure shock wave which exceeds the yield strength and densifies as the wave proceeds through the compact. The time scales and pressure range from 1-10's of microseconds and 10-100's of kilobars (10 Kb = 1 GPa). The short time scale of the pressure pulse during the compaction stage inhibits kinetic processes which have longer time constants. The pressure pulse can be delivered to the green compact by a number of techniques, i.e. high explosive, projectile. The methods differ in the degree that one can control the amplitude, duration, and nature of the pressure pulse. The lecture compares powders compacted by explosive and light gas guns and when possible characterize their resulting structures and properties, using AlN as example. 14 figures.

  20. 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: [Zoz GmbH, D-57482, Wenden (Germany)


    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)


    respectively. Late in the program, a fourth powder ( egg albumin ) was added to the list of powders to be investigated. The preparation of powders including...effects of ad sorbed foreign vapors on powder properties, (7) effects of removal of adsorbed gases and vapors, (8) energy required to disperse a powder sample, (9) properties of compacted powders, and (10) egg albumin studies.

  2. Effect of C and milling parameters on the synthesis of WC powders by mechanical alloying

    CSIR Research Space (South Africa)

    Bolokang, S


    Full Text Available of Refractory Metals & Hard Materials xxx (2009) xxx–xxx Contents lists availabl Int. Journal of Refractory Metal ls ARTICLE IN PRESS E-mail address: (S. Bolokang). avoided [1]. Although MA can produce a non-equilibrium, super....09.006 s & Hard Materials xxx (2009) xxx–xxx Fig. 3 shows a decrease in powder crystallite size with increas- ing milling times. After 12 h milling time, 11 nm WC crystallite size was obtained. Fig. 2. XRD pattern for the production of WC from interrupted high...

  3. Complex Impedance of Manganese Ferrite Powders Obtained by Two Different Methods

    Directory of Open Access Journals (Sweden)

    Mălăescu I.


    Full Text Available Two samples of manganese ferrite powder were obtained by the calcination method (sample A and hydrothermal method (sample B. The crystal structure of the samples has been determined using X-ray diffraction analysis (XRD. The results shown that the sample A has three phases (FeMnO3, Mn2O3 and Fe2O3 and the prevailing phase is FeMnO3 with perovskite structure and the sample B has only a single phase (MnFe2O4.

  4. The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars (United States)

    Blake, David F.


    The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50µm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish

  5. Preparation of nanocrystalline Fe-Si-Ni soft magnetic powders by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Madaah Hosseini, H.R. [Materials Science and Engineering Department, Sharif University of Technology, P.O. Box 11365-9466, Tehran (Iran, Islamic Republic of)]. E-mail:; Bahrami, A. [Materials Science and Engineering Department, Sharif University of Technology, P.O. Box 11365-9466, Tehran (Iran, Islamic Republic of)


    In this study, structural and magnetic properties of nanocrystalline Fe-Si-Ni powders produced by mechanical alloying (Ma) have been investigated. The samples with different chemical compositions and milling times were characterized by X-ray diffraction (XRD) and scanning electron microscope (Sem). The alloy powders with average grain size 8-19 nm were synthesized by milling for 35-100 h. Coercivity (H {sub c}) and crystallite size exhibited a similar decrease by increasing the mechanical alloying time. Maximum saturation magnetization (M {sub s}) and minimum H {sub c} were obtained at the composition of Fe{sub 87}Si{sub 10}Ni{sub 5} after 70 h milling.

  6. Preparation and Study of morphological properties of ZnO nano Powder

    Directory of Open Access Journals (Sweden)

    Mohammed Salab Hamza


    Full Text Available In this work, ZnO nanostructures for powder ZnO were synthesized by Hydrothermal Method. Size and shape of ZnO nanostructureas can be controlled by change ammonia concentration. In the preparation of ZnO nanostructure, zinc nitrate hexahydrate [Zn(NO32·6H2O] was used as a precursor. The structure and morphology of ZnO nanostructure have been characterized by scanning electron microscopy (SEM, atomic force microscopy (AFM, X-ray diffraction (XRD. The synthesized ZnO nanostructures have a hexagonal wurtzite structure. Also using Zeta potential and Particle Size Analyzers and size distribution of the ZnO powder

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

    Directory of Open Access Journals (Sweden)

    Romański A.


    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.

  8. Effects of copper content on the shell characteristics of hollow steel spheres manufactured using an advanced powder metallurgy technique (United States)

    Sazegaran, Hamid; Kiani-Rashid, Ali-Reza; Khaki, Jalil Vahdati


    Metallic hollow spheres are used as base materials in the manufacture of hollow sphere structures and metallic foams. In this study, steel hollow spheres were successfully manufactured using an advanced powder metallurgy technique. The spheres' shells were characterized by optical microscopy in conjunction with microstructural image analysis software, scanning electron microscopy (SEM), energy- dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). The microscopic evaluations revealed that the shells consist of sintered iron powder, sintered copper powder, sodium silicate, and porosity regions. In addition, the effects of copper content on various parameters such as shell defects, microcracks, thickness, and porosities were investigated. The results indicated that increasing the copper content results in decreases in the surface fraction of shell porosities and the number of microcracks and an increase in shell thickness.

  9. Effect of ball to powder ratio on the ZrO{sub 2} phase transformations during milling

    Energy Technology Data Exchange (ETDEWEB)

    Zakeri, M.; Razavi, M., E-mail:; Rahimipour, M.R.; Jamal Abbasi, B.


    Effect of milling time and ball to powder weight ratio (BPR) were investigated on the phase transformation of monoclinic zirconia during high energy ball milling. Degree of phase transformation was studied by X-ray diffraction (XRD) and quantitative phase analysis (Rietveld refinement). Morphology and microstructure were monitored by scanning and transmission electron microscopy, respectively. Higher milling time and BPR led to the more transformation, smaller mean grain size and larger strain. There was approximately 80% tetragonal zirconia in the 80 h milled powder with the BPR 25:1. A nanostructure powder with the mean grain size less than 10 nm was obtained in both BPRs that were in consistence with TEM images. Stress and strain inducing in the lattice of m-ZrO{sub 2} was proposed as the main mechanism of its transformation.

  10. Roller compaction of moist pharmaceutical powders. (United States)

    Wu, C-Y; Hung, W-L; Miguélez-Morán, A M; Gururajan, B; Seville, J P K


    The compression behaviour of powders during roller compaction is dominated by a number of factors, such as process conditions (roll speed, roll gap, feeding mechanisms and feeding speed) and powder properties (particle size, shape, moisture content). The moisture content affects the powder properties, such as the flowability and cohesion, but it is not clear how the moisture content will influence the powder compression behaviour during roller compaction. In this study, the effect of moisture contents on roller compaction behaviour of microcrystalline cellulose (MCC, Avicel PH102) was investigated experimentally. MCC samples of different moisture contents were prepared by mixing as-received MCC powder with different amount of water that was sprayed onto the powder bed being agitated in a rotary mixer. The flowability of these samples were evaluated in terms of the poured angle of repose and flow functions. The moist powders were then compacted using the instrumented roller compactor developed at the University of Birmingham. The flow and compression behaviour during roller compaction and the properties of produced ribbons were examined. It has been found that, as the moisture content increases, the flowability of moist MCC powders decreases and the powder becomes more cohesive. As a consequence of non-uniform flow of powder into the compaction zone induced by the friction between powder and side cheek plates, all produced ribbons have a higher density in the middle and lower densities at the edges. For the ribbons made of powders with high moisture contents, different hydration states across the ribbon width were also identified from SEM images. Moreover, it was interesting to find that these ribbons were split into two halves. This is attributed to the reduction in the mechanical strength of moist powder compacts with high moisture contents produced at high compression pressures. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  11. Influence of the powder preparation on the sintering of Yb-doped Sc 2O 3 transparent ceramics (United States)

    Bravo, A. C.; Longuet, L.; Autissier, D.; Baumard, J. F.; Vissie, P.; Longuet, J. L.


    We report the preparation and the sintering of high quality Yb:Sc 2O 3 powders with the ultimate intent to make transparent Yb:Sc 2O 3 ceramics for laser applications. The aim of the study is to compare two routes of powder preparation and observe the influence of the powder processing on the sintering of Yb-doped Sc 2O 3 ceramics. The powders were prepared (i) either from commercial oxides by a classical ceramic way (solid state reaction process) (ii) or by a wet chemical route. In that case, a carbonate precursor was synthesized by a coprecipitation method from a mixed solution of scandium and ytterbium nitrates using aqueous ammonium hydrogen carbonate as a precipitating agent. The Yb:Sc 2O 3 powder was obtained after heat treatment of the carbonate precursor at 700 °C. The powders prepared by these two methods were characterized by BET measurements, XRD and SEM and their sintering behaviour was investigated by dilatometry. The effects of a grinding step and of the addition of a sintering aid addition (TEOS) were investigated. The microstructures of the vacuum sintered materials were observed by scanning electron microscopy. Electron probe microanalysis allowed to characterize the repartition of the dopant Yb 3+ in the Sc 2O 3 matrix. Translucent ceramics with densities close to 99% were obtained in the best conditions.

  12. Synthesis and electromagnetic absorption properties of micro-nano nickel powders prepared with liquid phase reduction method

    Directory of Open Access Journals (Sweden)

    Ying Yu


    Full Text Available Monodisperse micro-nano nickel powders have been prepared by chemical reduction of aqueous solution NiSO4, NaOH and NaH2PO2, and the influence of pH value and initial concentration of NiSO4 on the size, structure, morphology and microwave absorption properties of nickel powders were investigated. The crystal structure of nickel powders was characterized by X-ray diffraction (XRD. And the morphology of the as-synthesized products was characterized by scanning electron microscopy (SEM and transmission electron microscopy (TEM. The microwave absorption properties of the composite materials were characterized by network analyzer. The result indicates that the growth of nickel powders produced by NiSO4 and NaH2PO2 at alkaline condition deeply relies on pH value and initial concentration of NiSO4 in reaction system. Different sizes of nickel powders with the diameter of 1.5μm and 180nm were produced at the pH value of 10 and initial concentration of NiSO4 at 0.5mol/L. The network analyzer showed definite microwave absorption properties of nickel powders with different sizes in the range of 0.5–18.0GHz.

  13. Studying the melting behavior of coal, biomass, and coal/biomass ash using viscosity and heated stage XRD data

    DEFF Research Database (Denmark)

    Arvelakis, Stelios; Folkedahl, B.; Dam-Johansen, Kim


    by the cocombustion tests appeared to be somewhat different compared to that of the laboratory-prepared ash samples. The heated stage XRD data provide useful information regarding the reactions among the various ash compounds and the phase transformations during the heating and cooling of the ash samples and helped...... the explanation of the produced viscosity curves....

  14. XRD and UV-Vis diffuse reflectance analysis of CeO 2-ZrO 2 solid ...

    Indian Academy of Sciences (India)

    The products were characterized by XRD and UV-Vis-NIR diffuse reflectance spectroscopy. The materials are crystalline in nature and the lattice parameters of the solid solution series follow Vegard's law. Diffuse reflectance spectra of the solid solutions in the UV region show two intense bands at 250 and 297 nm which are ...

  15. Co-precipitation synthesis and characterization of NiO-Ce0.8Sm0.2O1.9 nanocomposite powders: effect of precipitation agents. (United States)

    Ding, Changsheng; Lin, Hongfei; Sato, Kazuhisa; Hashida, Toshiyuki


    NiO-Ce0.8Sm0.2O1.9 (NiO-SDC) nanocomposite powders applied as promising anode material for low-temperature solid oxide fuel cells (SOFCs) were synthesized by hydroxide co-precipitation method using NH3 x H2O, NaOH and NH3 x H2O + NaOH as precipitation agents. The crystal phases, morphologies and sintering behavior of the synthesized NiO-SDC nanocomposite powders were investigated by means of X-ray diffraction (XRD), transmission electron microscopy (TEM) and sintering experiments. The effect of precipitation agents on the synthesis of the NiO-SDC nanocomposite powders was discussed. Results show that different precipitation agents influence greatly the synthesis and characteristics of the NiO-SDC nanocomposite powders. The NiO-SDC nanocomposite powders synthesized with NH3 x H2O deviate from the original composition due to the loss of Ni. The loss of Ni is avoided and nano-sized NiO-SDC composite powders are synthesized, when NaOH and NH3 x H2O + NaOH are used as precipitation agents. The NiO-SDC nanocomposite powders can be synthesized at relatively low temperature using NH3 x H2O + NaOH as precipitation agent, and the synthesized NiO-SDC nanocomposite powders show good sintering characteristics.

  16. L-Leucine as an excipient against moisture on in vitro aerosolization performances of highly hygroscopic spray-dried powders. (United States)

    Li, Liang; Sun, Siping; Parumasivam, Thaigarajan; Denman, John A; Gengenbach, Thomas; Tang, Patricia; Mao, Shirui; Chan, Hak-Kim


    L-Leucine (LL) has been widely used to enhance the dispersion performance of powders for inhalation. LL can also protect powders against moisture, but this effect is much less studied. The aim of this study was to investigate whether LL could prevent moisture-induced deterioration in in vitro aerosolization performances of highly hygroscopic spray-dried powders. Disodium cromoglycate (DSCG) was chosen as a model drug and different amounts of LL (2-40% w/w) were added to the formulation, with the aim to explore the relationship between powder dispersion, moisture protection and physicochemical properties of the powders. The powder formulations were prepared by spray drying of aqueous solutions containing known concentrations of DSCG and LL. The particle sizes were measured by laser diffraction. The physicochemical properties of fine particles were characterized by X-ray powder diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and dynamic vapor sorption (DVS). The surface morphology and chemistry of fine particles were analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (ToF-SIMS). In vitro aerosolization performances were evaluated by a next generation impactor (NGI) after the powders were stored at 60% or 75% relative humidity (RH), and 25°C for 24h. Spray-dried (SD) DSCG powders were amorphous and absorbed 30-45% (w/w) water at 70-80% RH, resulting in deterioration in the aerosolization performance of the powders. LL did not decrease the water uptake of DSCG powders, but it could significantly reduce the effect of moisture on aerosolization performances. This is due to enrichment of crystalline LL on the surface of the composite particles. The effect was directly related to the percentage of LL coverage on the surface of particles. Formulations having 61-73% (molar percent) of LL on the particle surface (which correspond to 10-20% (w

  17. Structural, optical and magnetic properties of Sn doped ZnS nano powders prepared by solid state reaction (United States)

    Kumar, K. Chaitanya; Rao, N. Madhusudhana; Kaleemulla, S.; Rao, G. Venugopal


    Tin doped ZnS powders (Zn1-xSnxS, x = 0.00, 0.02, 0.05&0.08) were synthesized by a simple Solid state reaction and were characterized by Powder X-ray diffractometer (XRD), UV-Vis-NIR diffuse reflectance spectrophotometer, fluorescence spectrophotometer, scanning electron microscope (SEM) and vibrating sample magnetometer (VSM). The XRD studies revealed that no change in crystal structure was observed by the substitution of Sn into ZnS lattice. The crystallite size was calculated by Scherrer's formula and found that the crystallize size of Sn doped ZnS powders were in the range of 35-45 nm. From the diffused reflectance spectra, the band gap values of Zn1-xSnxS powders were estimated, and they were found to be in the range of 3.53-3.58 eV. The pure ZnS particles showed higher optical absorption in visible region than that of Sn doped ZnS nano particles. The Photoluminescence (PL) spectra of Zn1-xSnxS powders were recorded in the range of 400-700 nm with an excitation wavelength of 360 nm. The Zn1-xSnxS powders exhibited ferromagnetism at low temperature (100 K) and super paramagnetism at room temperature (300 K). The strength of magnetization increased with increase of Sn doping concentration from 0.015 emu/g to 0.18 emu/g, when x increased from 0.00-0.05.

  18. Feasibility of Plasma Treated Clay in Clay/Polymer Nanocomposites Powders for use Laser Sintering (LS) (United States)

    Almansoori, Alaa; Seabright, Ryan; Majewski, C.; Rodenburg, C.


    The addition of small quantities of nano-clay to nylon is known to improve mechanical properties of the resulting nano-composite. However, achieving a uniform dispersion and distribution of the clay within the base polymer can prove difficult. A demonstration of the fabrication and characterization of plasma-treated organoclay/Nylon12 nanocomposite was carried out with the aim of achieving better dispersion of clay platelets on the Nylon12 particle surface. Air-plasma etching was used to enhance the compatibility between clays and polymers to ensure a uniform clay dispersion in composite powders. Downward heat sintering (DHS) in a hot press is used to process neat and composite powders into tensile and XRD specimens. Morphological studies using Low Voltage Scanning Electron Microscopy (LV-SEM) were undertaken to characterize the fracture surfaces and clay dispersion in powders and final composite specimens. Thermogravimetric analysis (TGA) testing performed that the etched clay (EC) is more stable than the nonetched clay (NEC), even at higher temperatures. The influence of the clay ratio and the clay plasma treatment process on the mechanical properties of the nanocomposites was studied by tensile testing. The composite fabricated from (3% EC/N12) powder showed ~19 % improvement in elastic modulus while the composite made from (3% NEC/N12) powder was improved by only 14%). Most notably however is that the variation between tests is strongly reduced when etch clay is used in the composite. We attribute this to a more uniform distribution and better dispersion of the plasma treated clay within polymer powders and ultimately the composite.

  19. Bioactive and Antibacterial Glass Powders Doped with Copper by Ion-Exchange in Aqueous Solutions

    Directory of Open Access Journals (Sweden)

    Marta Miola


    Full Text Available In this work, two bioactive glass powders (SBA2 and SBA3 were doped with Cu by means of the ion-exchange technique in aqueous solution. SBA2 glass was subjected to the ion-exchange process by using different Cu salts (copper(II nitrate, chloride, acetate, and sulphate and concentrations. Structural (X-ray diffraction-XRD, morphological (Scanning Electron Microscopy-SEM, and compositional (Energy Dispersion Spectrometry-EDS analyses evidenced the formation of crystalline phases for glasses ion-exchanged in copper(II nitrate and chloride solutions; while the ion-exchange in copper(II acetate solutions lead to the incorporation of higher Cu amount than the ion-exchange in copper(II sulphate solutions. For this reason, the antibacterial test (inhibition halo towards S. aureus was performed on SBA2 powders ion-exchanged in copper(II acetate solutions and evidenced a limited antibacterial effect. A second glass composition (SBA3 was developed to allow a greater incorporation of Cu in the glass surface; SBA3 powders were ion-exchanged in copper(II acetate solutions (0.01 M and 0.05 M. Cu-doped SBA3 powders showed an amorphous structure; morphological analysis evidenced a rougher surface for Cu-doped powders in comparison to the undoped glass. EDS and X-ray photoelectron spectroscopy (XPS confirmed the Cu introduction as Cu(II ions. Bioactivity test in simulated body fluid (SBF showed that Cu introduction did not alter the bioactive behaviour of the glass. Finally, inhibition halo test towards S. aureus evidenced a good antimicrobial effect for glass powders ion-exchanged in copper(II acetate solutions 0.05 M.

  20. Adsorption of lignosulfonate compounds using powdered eggshell

    Directory of Open Access Journals (Sweden)

    Muhammad Ali Zulfikar


    Full Text Available Batch adsorption of lignosulfonates using untreated powdered eggshell under the influences of mixing time, pH,particle size and dose of powdered eggshell was investigated. Adsorption isotherms of lignosulfonates onto powder eggshellwere also studied. Eggshells were collected from the Balubur traditional market in Bandung, Indonesia, washed with distilledwater, air dried, and then ground into powder of different particle sizes. Kinetic studies found that equilibrium time was ashigh as 90 minutes. From experiments carried out at different pH, it was observed that pH plays an important role in theadsorption of lignosulfonate compounds. It was also observed that particles size has no significant effect on the adsorptionof lignosulfonate compounds. The optimum dosage of powdered eggshell was 30 g/100 mL of 500 mg/L lignosulfonatesolution. Adsorption isotherms studied through the use of graphical methods revealed that the adsorption of lignosulfonatesonto powdered eggshell follows the Langmuir model.

  1. Indigenous tooth powders = covert lead poisoning? (United States)

    Hegde, Sapna; Shubha, A B; Rao, B Dinesh


    The present study aimed to measure the concentration of lead in various indigenous preparations of tooth powders available and used locally in and around Udaipur, Rajasthan, India. Seven different brands of tooth powders manufactured and/or marketed locally were obtained from stores all over Udaipur city. Some home-made powders commonly used for cleaning teeth were also collected. The tooth powders were analyzed for lead content by atomic absorption spectrophotometry. All tooth powders tested were found to contain high levels of lead ranging from 21 ppm to 82 ppm, above the maximum permissible level of 20 ppm prescribed by the Bureau of Indian Standards. Indigenous tooth powders contain high levels of lead and thus may be a source of lead poisoning that is often overlooked.

  2. Modification of the structural and optical properties of commercial ZnO powder by mechanical activation

    Directory of Open Access Journals (Sweden)

    Šćepanović M.


    Full Text Available Mechanical activation was used as a method for modification of the structural and optical properties of commercial ZnO powder. For this purpose zinc oxide powder was mechanically treated by grinding in a high-energy vibro-mill in a continual regime in air up to 300 minutes. Starting and modified ZnO samples were characterized using XRD, BET and TEM measurements. Optical properties of these samples were investigated by Raman and photoluminescence (PL spectroscopy. The color of commercial ZnO powder was white while mechanically activated ZnO powder was dark yellow, indicating the presence of nonstoichiometry. In the Raman spectra of non-activated sample Raman modes of bulk ZnO were observed, while the spectra of modified samples point out structural and stoichiometric changes. The PL spectra of modified samples excited by 325 and 442 nm lines of a He-Cd laser show great difference with respect to the spectra of the original sample. This study confirms that change in the defect structure of the ZnO crystal lattice introduced by mechanical activation affects the optical properties of this material.

  3. Synthesis of yttria-doped bismuth oxide powder by carbonate coprecipitation for IT-SOFC electrolyte. (United States)

    Lee, J G; Kim, S H; Yoon, H H


    Yttria-doped bismuth oxide (YBO) powders were synthesized by ammonium carbonate coprecipitation for the preparation of electrolytes of an intermediate temperature solid oxide fuel cell (IT-SOFC). The starting salts were yttrium and bismuth nitrate. The crystal structures and the morphological characteristics of the particles were analyzed by XRD and SEM, respectively. The ionic conductivity of the sintered pellet was measured by an electrochemical impedance analyzer. The size of the calcined YBO powders were in the range of 20-100 nm as measured by SEM images. The YBO pellets had a face-centered cubic structure, and their crystallite size was about 54-88 nm. The ionic conductivity of the YBO pellets sintered at 800 degrees C was observed to be 2.7 x 10(-1) Scm-(-1) at 700 degrees C. The ball-milling of the YBO powder before it was pelletized was found to have been unrequired probably because of a good sinterability of the YBO powders that was prepared via the ammonium carbonate coprecipitation method. The results showed that the ammonium carbonate coprecipitation process could be used as the cost-efficient method of producing YBO electrolytes for IT-SOFC.

  4. Preparation and Characterization of Amorphous B Powders by Salt-Assisted SHS Technique

    Directory of Open Access Journals (Sweden)

    Yujing Ou


    Full Text Available To use the salt-assisted SHS technique to prepare B powders was proposed. Calculation results found that the adiabatic combustion temperature of the B2O3-Mg reaction system was 2604 K, higher than the 1800 K criterion of self-propagating temperature, which meant that the SHS application was feasible. When 0, 10%, 20%, 30%, 40%, 50%, and 60% NaCl content were added, the adiabatic combustion temperature of the reaction system decreased linearly. When 60% NaCl content was added, the adiabatic combustion temperature was 1799 K (lower than 1800 K, unsuitable for self-propagating reaction, which was consistent with the experimental results. Through scanning electron microscope (SEM, energy disperse spectroscopy (EDS, and particle size analysis, the influence of different addition of NaCl on the morphology, average particle size, and purity of prepared B powder was investigated. EDS and chemical analysis indicated that the purity of prepared B powder was over 96% and the average particle size was within the range of 0.4~0.8 μm when the content of NaCl was 50%. The analysis of X-ray diffraction (XRD and selected area electron diffraction (SAED proved that the prepared B powder was amorphous.

  5. Preparation of niobium carbide powder by electrochemical reduction in molten salt

    Energy Technology Data Exchange (ETDEWEB)

    Song, Qiushi [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110819 (China); Xu, Qian, E-mail: [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110819 (China); School of Materials Science and Engineering, Shanghai University, Shanghai 200072 (China); Meng, Jingchun; Lou, Taiping; Ning, Zhiqiang [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110819 (China); Qi, Yang [College of Science, Northeastern University, Shenyang 110819 (China); Yu, Kai [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110819 (China)


    The niobium carbide powder was prepared via electrochemical reduction of the mixture of Nb{sub 2}O{sub 5} and carbon in molten CaCl{sub 2}–NaCl. The reaction pathway from the sintered precursor to the final product has been investigated. The effect of the working temperature on the reduction of the Nb{sub 2}O{sub 5}/C composite precursor was considered. The role of carbon during the electrochemical reduction of the composite pellet was discussed. The samples were analysed by XRD and SEM. The results indicated that the NbC powder was approximately 200 nm after the reduction. Nb{sub 2}O{sub 5} was gradually reduced to Nb, and NbC was subsequently obtained by the reaction of carbon with Nb metal. In addition, Nb{sub 2}O{sub 5} could spontaneously react with CaO in the melt to form a serious of calcium niobates. The participation of carbon was available for the efficiency of electro-reduction of Nb{sub 2}O{sub 5}. - Graphical abstract: Niobium carbide powder was electrochemically prepared in molten salt, and the reduction pathway was illustrated schematically. - Highlights: • NbC powder was prepared electrochemically in molten salt. • The working temperature was lower than that of carbothermic reduction. • The reduction pathway was discussed compared to direct electro-deoxidation of Nb{sub 2}O{sub 5}.

  6. Sintering of B{sub 4}C powder obtained by a modified carbo-thermal reaction

    Energy Technology Data Exchange (ETDEWEB)

    Rocha, R.M.; Kazumi, M.H.; Goncalves, D.P.; Melo, F.C.L. [Centro Tecnico Aeroespacial (CTA) - Instituto de Aeronautica e Espaco, Praca Marechal Eduardo Gomes, 50 Campus do CTA - Vila das Acacias, 12228-904 Sao Jose dos Campos-SP (Brazil)


    Boron carbide is one of the hardest materials and a highly refractory material that is of great interest for structural, electronic and nuclear applications. B{sub 4}C is commercially manufactured by the carbo-thermal reduction of a mixture of boron oxide (B{sub 2}O{sub 3}) in an batch electric arc furnace process. However the carbo-thermal reaction on the stoichiometric starting composition results an excess carbon residue because of the boron loss in the form of B{sub 2}O{sub 2}. Thus, a modified carbo-thermal reaction is applied with an excess B{sub 2}O{sub 3} to compensate the loss and to obtain stoichiometric powders. The aim of this work is to study the sinterability of this powder with the lower carbon residue acting as sintering additive. Pressureless sintering in the temperatures of 1900 deg. C/30 min and 2100 deg. C/30 min in argon atmosphere were applied. The synthesized powders were analysed by XRD and SEM. Density of 94% of theoretical density was achieved for sample prepared with the powder obtained with 50% B{sub 2}O{sub 3} excess synthesized at 1700 deg. C/15 min. (authors)

  7. Preparation of single phase {beta}-spodumene powders by sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Wen, Shawbing; Yang, Sheng [National Cheng-Kung University, Tainan (Taiwan). Dept. of Resources Engineering; Chen, Jenmin; Wu, Nangchung [National Cheng-Kung University, Tainan (Taiwan). Dept. of Material Science and Engineering; Wang, Moochin [National Kaohsiung Institute of Technology, Kaohsiung (Taiwan). Dept. of Mechanical Engineering


    The {beta}-spodumene (Li{sub 2}O{center_dot}Al{sub 2}O{sub 3}{center_dot}4SiO{sub 2}, LAS) powders were prepared by the sol-gel process using a mixture of silica sol, alumina sol and lithium nitrate solution. Si(OC{sub 2}H{sub 5}){sub 4}, Al(OC{sub 4}H{sub 9}{sup 8ec}){sub 3} and LiNO{sub 3} were used as the starting compounds. Thermogravimetric and differential thermal analyses (TG/DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), wavelength-dispersive spectroscopy (WDS), transmission electron microscopy (TEM) and electron diffraction (ED) analysis were utilized to characterize the {beta}-spodumene powders prepared by the sol-gel process. The crystallization temperature of the LAS gel powder estimated by TG/DTA was about 630 degree C. When the LAS dried gel was heated from 600 to 850 degree C, the crystallized powders of the single phase {beta}-spodumene were obtained. (author)

  8. Sun drying of residual annatto seed powder


    Dyego da Costa Santos; Alexandre José de Melo Queiroz; Rossana Maria Feitosa de Figueirêdo; Emanuel Neto Alves de Oliveira


    Residual annatto seeds are waste from bixin extraction in the food, pharmaceutical and cosmetic industries. Most of this by-product is currently discarded; however, the use of these seeds in human foods through the elaboration of powder added to other commercial powders is seen as a viable option. This study aimed at drying of residual annatto powder, with and without the oil layer derived from the industrial extraction of bixin, fitting different mathematical models to experimental data and ...

  9. In-house characterization of protein powder

    DEFF Research Database (Denmark)

    Hartmann, Christian Grundahl; Nielsen, Ole Faurskov; Ståhl, Kenny


    X-ray powder diffraction patterns of lysozyme and insulin were recorded on a standard in-house powder diffractometer. The experimental powder diffraction patterns were compared with patterns calculated from Protein Data Bank coordinate data. Good agreement was obtained by including straightforward...... to include calculated H-atom positions did not improve the overall fit and was abandoned. The method devised was shown to be a quick and convenient tool for distinguishing precipitates and polymorphs of proteins....

  10. The Influence of Synthesis Temperature on Manufacturing and Properties of SrSi2O2N2:Eu2+ Powders

    Directory of Open Access Journals (Sweden)

    Pawlik T.


    Full Text Available This paper presents the results of the synthesis temperature on the properties of the ceramic powders of SrSi2O2N2:Eu2+ obtained by the solid-phase reaction. Synthesis was carried out in the temperature range of 1250-1650°C for 2 hours in nitrogen flow in the reducing atmosphere of the graphite furnace. The phases present in the resultant powders were identified by X-ray structural analysis (XRD. Scanning electron microscopy (SEM was used to examine the changes in the powder morphology as a result of the synthesis. The excitation and emission spectra measurements let to study phosphor photoluminescence properties. The results show the strong influence of temperature synthesis on the formation and purity of expected phases. The synthesis temperature also affects the luminescent properties of SrSi2O2N2:Eu2+ ceramic powders.

  11. CVD carbon powders modified by ball milling

    Directory of Open Access Journals (Sweden)

    Kazmierczak Tomasz


    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.

  12. Synthesis, characterization and formation mechanism of single-phase nanostructure bredigite powder

    Energy Technology Data Exchange (ETDEWEB)

    Mirhadi, S.M., E-mail: [Department of Ceramic Engineering, Shahreza Branch, Islamic Azad University, 86145-311, Shahreza, Isfahan (Iran, Islamic Republic of); Tavangarian, F.; Emadi, R. [Department of Materials Engineering, Isfahan University of Technology (IUT), Isfahan 84156-83111 (Iran, Islamic Republic of)


    Single-phase nanocrystalline bredigite powder was successfully synthesized by mechanical activation of talc, calcium carbonate, and amorphous silica powder mixture followed by annealing. Simultaneous thermal analysis (STA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), dynamic light scattering (DLS),and Fourier transform infrared spectroscopy (FT-IR) techniques were employed to characterize various powders. Single-phase nanostructure bredigite powder with crystallite size of about 65 nm was synthesized by 20 h of mechanical activation with subsequent annealing at 1200 Degree-Sign C for 1 h. The bredigite formation mechanism was studied. During the formation process of nanostructure bredigite powder some intermediate compounds such as wollastonite (CaSiO{sub 3}), larnite (Ca{sub 2}SiO{sub 4}), merwinite (Ca{sub 3}MgSi{sub 2}O{sub 8}), and calcium magnesium silicate (Ca{sub 5}MgSi{sub 3}O{sub 12}) were formed. It was found that bredigite was not produced directly and that the formation of merwinite, enstatite and Ca{sub 5}MgSi{sub 3}O{sub 12}was unavoidable during the synthesis of bredigite. - Graphical abstract: This paper reports the successful synthesis of nanostructure bredigite powder by mechanical activation with subsequent annealing. The results showed that during the formation of bredigite powder some transition compounds such as wollastonite (CaSiO{sub 3}), larnite (Ca{sub 2}SiO{sub 4}), merwinite (Ca{sub 3}MgSi{sub 2}O{sub 8}), and calcium magnesium silicate (Ca{sub 5}MgSi{sub 3}O{sub 12}) were formed. Highlights: Black-Right-Pointing-Pointer Mechanical activation improved the kinetics of bredigite formation. Black-Right-Pointing-Pointer A mechanism was suggested for the nanostructure bredigite formation. Black-Right-Pointing-Pointer During the formation of bredigite powder some intermediate compounds were formed. Black-Right-Pointing-Pointer The nanostructure bredigite powder had a mean crystallite

  13. Preparation of High Quality Ti-6.5Al-1.4Si-2Zr-0.5Mo-2Sn Alloy Powder by Plasma Rotating Electrode Process

    Directory of Open Access Journals (Sweden)

    KUANG Quan-bo


    Full Text Available This research aims to prepare high quality powder of Ti-6.5Al-1.4Si-2Zr-0.5Mo-2Sn,which lays foundation for the following preparation of powder high temperature titanium alloy component.Ti-6.5Al-1.4Si-2Zr-0.5Mo-2Sn alloy ingots were prepared by vacuum arc remelting (VAR. The chemical compositions of ingots were examined. The loss of alloy elements, uniformity of composition, phase composition and microstructure of titanium alloy ingots were analyzed. Then powders were prepared by plasma rotating electrode process (PREP with different rotating speeds. Alloy powders were sieved into different particle sizes. The relationship between rotating speed and physical and chemical properties of powder was studied. X-ray diffraction(XRD, scanning electron microscope(SEM and metallurgical microscope(OM were used to investigate the phase composition, morphology and microstructure of the powder. The results show that the composition distribution of titanium alloy ingot prepared by VAR is uniform and the content of alloy elements meets the requirements of national standard, through a unique pressing electrode. Microstructure of the ingot is lamellar structure with small amounts of silicide particles disperse in the matrix. The size distribution of the powders made by PREP method exhibits the normal distribution. The sphericity of the powder is excellent,and no hollow ball and satellite ball exists. With the increase of rotating speed, the proportion of small particles increases dramatically,the proportion of large particles decreases greatly. The phase composition of powder is mainly α' phase,and it is mainly composed of peritectic and small amount of dendrite structures. Compared with the alloy ingot, the elements of the powders have a slight loss, the content of O is less than 0.1%,which is beneficial to obtain high-performance powder titanium alloy.

  14. Enzyme-linked immunosorbent assay for the detection of bovine rennet whey powder in milk powder and buttermilk powder

    NARCIS (Netherlands)

    Bremer, M.G.E.G.; Kemmers-Voncken, A.; Boers, E.A.M.; Frankhuizen, R.; Haasnoot, W.


    An inhibition enzyme-linked immunosorbent assay (ELISA) for the detection of bovine rennet whey (BRW) solids in skim milk powders (SMP) and buttermilk powders is presented. The BRW content was determined in a neutralised trichloroacetic acid sample extract by binding of the dissolved

  15. Characterization of pre-Hispanic pottery from Teotihuacan, Mexico, by a combined PIXE-RBS and XRD analysis (United States)

    Ruvalcaba-Sil, J. L.; Ontalba Salamanca, M. A.; Manzanilla, L.; Miranda, J.; Cañetas Ortega, J.; López, C.


    A combined analysis of IBA techniques (Proton Induced X-ray Emission (PIXE) and Rutherford Backscattering Spectroscopy (RBS)) and a complementary study by X-ray Diffraction (XRD) were performed to characterize pottery corresponding to the Epiclassic period (A.D. 700-900) from Teotihuacan, Mexico. Elemental compositions of pottery samples were measured by simultaneous PIXE and RBS using 2.6 MeV protons. Red, white and brown pottery pigments were studied by non-vacuum PIXE and a proton beam of 3 MeV. The various mineralogical phases of the pottery were identified by XRD. From pottery elemental compositions and its mineralogical phases, some differences among the pottery samples and groups were established.

  16. Characterization of pre-Hispanic pottery from Teotihuacan, Mexico, by a combined PIXE-RBS and XRD analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ruvalcaba-Sil, J.L.; Ontalba Salamanca, M.A.; Manzanilla, L.; Miranda, J.; Canetas Ortega, J.; Lopez, C


    A combined analysis of IBA techniques (Proton Induced X-ray Emission (PIXE) and Rutherford Backscattering Spectroscopy (RBS)) and a complementary study by X-ray Diffraction (XRD) were performed to characterize pottery corresponding to the Epiclassic period (A.D. 700-900) from Teotihuacan, Mexico. Elemental compositions of pottery samples were measured by simultaneous PIXE and RBS using 2.6 MeV protons. Red, white and brown pottery pigments were studied by non-vacuum PIXE and a proton beam of 3 MeV. The various mineralogical phases of the pottery were identified by XRD. From pottery elemental compositions and its mineralogical phases, some differences among the pottery samples and groups were established.

  17. Leonardo da Vinci's drapery studies: characterization of lead white pigments by µ-XRD and 2D scanning XRF (United States)

    Gonzalez, Victor; Calligaro, Thomas; Pichon, Laurent; Wallez, Gilles; Mottin, Bruno


    This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of µ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Département des Arts Graphiques, Musée du Louvre and in the Musée des Beaux- Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special µ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique.

  18. In-Situ Study of Gaseous Reduction of Magnetite Doped with Alumina Using High-Temperature XRD Analysis (United States)

    Kapelyushin, Yury; Sasaki, Yasushi; Zhang, Jianqiang; Jeong, Sunkwang; Ostrovski, Oleg


    The reduction of magnetite of technical grade and magnetite doped with 3 mass pct Al2O3 was studied in situ using high-temperature XRD (HT-XRD) analysis. Magnetite was reduced by CO-CO2 gas (80 vol pct CO) at 1023 K (750 °C). Reduction of magnetite doped with alumina occurred from the Fe3O4-FeAl2O4 solid solution which has a miscibility gap with critical temperature of 1133 K (860 °C). The degree of reduction of magnetite was derived using Rietveld refinement of the HT-XRD spectra; the compositions of the Fe3O4-FeAl2O4 solid solution and the concentrations of carbon in γ-iron were determined from the lattice constants of the solutions. The reduction of magnetite progressed topochemically with the formation of a dense iron shell. The reduction of alumina-containing magnetite started along certain lattice planes with the formation of a network-like structure. Reduction of alumina-containing magnetite was faster than that of un-doped magnetite; this difference was attributed to the formation of the network-like structure. Hercynite content in the Fe3O4-FeAl2O4 solid solution in the process of reduction of magnetite doped with 3 mass pct Al2O3 increased from 5.11 to 20 mass pct, which is close to the miscibility gap at 1023 K (750 °C). The concentration of carbon in γ-Fe (0.76 mass pct) formed in the reduced sample of magnetite doped with 3 mass pct Al2O3 was close to the equilibrium value with 80 vol pct CO to 20 vol pct CO2 gas used in the HT-XRD experiments.

  19. Study of Gadolinium-doped cerium oxide by XRD, TG-DTA, impedance analysis, and positron lifetime spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ohta, S; Kosaka, T [Department of Chemistry, Tokyo Gakugei University, Nukuikita 4-1-1, Koganei, Tokyo 184-8501 (Japan); Sato, K, E-mail: [Department of Environmental Sciences, Tokyo Gakugei University, Nukuikita 4-1-1, Koganei, Tokyo 184-8501 (Japan)


    X-ray diffraction, thermogravimetry differential thermal analysis, impedance analysis, and positron lifetime spectroscopy were conducted for Gadolinium-doped cerium oxides (GDC) prepared using oxalate coprecipitation method. XRD revealed the fluorite structure indicating that gadolinium is successfully doped into cerium oxide. Prior to sintering, the vacancy-sized free volume and nanovoid were observed at grain boundaries. The vacancy-sized free volumes shrank with increasing sintering temperatures and finally got dominant.

  20. Combined use of SEM-EDS, OM and XRD for the characterization of corrosion products grown on silver roman coins (United States)

    Ingo, G. M.; Balbi, S.; de Caro, T.; Fragalà, I.; Angelini, E.; Bultrini, G.


    In the framework of the PROMET project (European Commission contract No. 509126) aimed to develop new analytical techniques and materials for monitoring and protecting metal artefacts and monuments from the Mediterranean region, the corrosion products grown on silver Roman coins during archaeological burial is studied by means of scanning electron microscopy combined with energy dispersive spectrometry (SEM-EDS), X-ray diffraction (XRD) and optical microscopy (OM) techniques.

  1. Experimental Equipment for Powder Processing (United States)


    Al2O3/ZrO2 FGM samples. 3.3.4 CTEs measurement [29, 30] By in situ reaction of WO3 to ZrO2, we fabricated various ZrW2O8 /ZrO2 composites, as listed in...Table 6. Table 6 The WO3/ZrO2 mass ratios of various green samples and the corresponding resultant ZrW2O8 /ZrO2 volume ratios in the sintered...samples. # WO3/ZrO2 mass ratio in reactant powder ZrW2O8 /ZrO2 volume ratios in the sintered sample Final relative density 1 0.159:1 20:80 77% 2

  2. Crystal Structure and Morphology Dependence of the Phase of Mollusc Shell: A Case Study of XRD, SEM and ESR

    Energy Technology Data Exchange (ETDEWEB)

    Siriprom, W [Faculty of Resources and Environment, Kasetsart University, Sriracha Campus, Chonburi, 20230 (Thailand); Kaewkhao, J [Center of Excellence in Glass Technology and Materials Science (CEGM), Nakhon Pathom Rajabhat University, 73000 (Thailand); Phachana, K [Department of Chemistry, Faculty of Science, Burapha University, Chonburi, 20131 (Thailand); Limsuwan, P, E-mail: [Department of Physics, King Mongkut' s University of Technology Thonburi, Bangkok, 10140 (Thailand)


    The aim of this study is to investigate the physical properties in the Paphia undulate and Amusium pleuronectes shells collected from the coastal area of Chonburi province, Thailand. The crystal structure of the shells was studied by x-ray diffraction (XRD). The XRD patterns spectra reveal that the Paphia undulate shells and Amusium pleuronectes shells are made of a pure aragonite phase, and a mixture phase of aragonite and calcite, respectively, the identification and quantitative analysis were performed by using the Rietveld method. In this study, we also used the scanning electron microscope (SEM) to study the Morphology of the Paphia undulate shells and Amusium pleuronectes shells. The results on SEM micrographs agree well with those of XRD. In addition, the ions in the shell samples were also studied by Electron Spin Resonance Spectroscopy (ESR). The ESR spectra show that the samples of both shells were consisting of Mn{sup 2+} ions. The pattern of the ESR spectrum is thus strongly influenced by the environment of the paramagnetic ions, and then it can be used to identification of crystal structure of mollusc shell

  3. AFM and XRD characterization of silver nanoparticles films deposited on the surface of DGEBA epoxy resin by ion sputtering

    Directory of Open Access Journals (Sweden)

    José Elisandro de Andrade


    Full Text Available In this work, silver atoms were deposited by ion sputtering on the surface of diglycidyl ether of bisphenol A (DGEBA epoxy resin cured at 150 °C for 6 hours in air. The films of DGEBA and its precursors were characterized by Raman spectroscopy to identify the main functional groups and their relationship with the deposited silver atoms. Silver thin films of 5, 10, 15 and 20 nm were deposited on the epoxy resin at room temperature. Both the initial film of DGEBA and the subsequent silver thin film were analyzed by Atomic Force Microscopy (AFM in the non-contact mode. Silver thin films were also analyzed using X-ray diffraction (XRD at room temperature. The AFM results showed the formation of silver crystallites on the surface of DGEBA at very low coverage whereas XRD indicated that most of them had their main axis aligned to the normal of the surface. An increase in the coverage led to an increase in the grain size as indicated by AFM. However, XRD results indicated that the crystallite size remained almost constant while the appearance of peaks corresponding to other crystalline orientations suggests the coalescence of the original crystallites and an increase in size of the more dense planes, namely [111].

  4. AFM and XRD characterization of silver nanoparticles films deposited on the surface of DGEBA epoxy resin by ion sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, Jose Elisandro de; Machado, Rogerio; Macedo, Marcelo Andrade; Cunha, Frederico Guilherme Carvalho [Clinica de Medicina Nuclear e Radiologia de Maceio (MedRadiUS), Radiology and Imaging Diagnosis at Universidade Federal de Alagoas (UFAL), Maceio, AL (Brazil)


    In this work, silver atoms were deposited by ion sputtering on the surface of diglycidyl ether of bisphenol A (DGEBA) epoxy resin cured at 150 deg C for 6 hours in air. The films of DGEBA and its precursors were characterized by Raman spectroscopy to identify the main functional groups and their relationship with the deposited silver atoms. Silver thin films of 5, 10, 15 and 20 nm were deposited on the epoxy resin at room temperature. Both the initial film of DGEBA and the subsequent silver thin film were analyzed by Atomic Force Microscopy (AFM) in the non-contact mode. Silver thin films were also analyzed using X-ray diffraction (XRD) at room temperature. The AFM results showed the formation of silver crystallites on the surface of DGEBA at very low coverage whereas XRD indicated that most of them had their main axis aligned to the normal of the surface. An increase in the coverage led to an increase in the grain size as indicated by AFM. However, XRD results indicated that the crystallite size remained almost constant while the appearance of peaks corresponding to other crystalline orientations suggests the coalescence of the original crystallites and an increase in size of the more dense planes, namely [111]. (author)

  5. AFM and XRD characterization of silver nanoparticles films deposited on the surface of DGEBA epoxy resin by ion sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, Jose Elisandro de; Machado, Rogerio; Macedo, Marcelo Andrade [Universidade Federal de Sergipe (UFSE), Aracaju, SE (Brazil). Programa de Pos-graduacao em Fisica; Cunha, Frederico Guilherme Carvalho [Universidade Federal de Sergipe (UFSE), Aracaju, SE (Brazil). Programa de Pos-graduacao em Ciencia e Engenharia de Materiais


    In this work, silver atoms were deposited by ion sputtering on the surface of diglycidyl ether of bisphenol A (DGEBA) epoxy resin cured at 150 Degree-Sign C for 6 hours in air. The films of DGEBA and its precursors were characterized by Raman spectroscopy to identify the main functional groups and their relationship with the deposited silver atoms. Silver thin films of 5, 10, 15 and 20 nm were deposited on the epoxy resin at room temperature. Both the initial film of DGEBA and the subsequent silver thin film were analyzed by Atomic Force Microscopy (AFM) in the non-contact mode. Silver thin films were also analyzed using X-ray diffraction (XRD) at room temperature. The AFM results showed the formation of silver crystallites on the surface of DGEBA at very low coverage whereas XRD indicated that most of them had their main axis aligned to the normal of the surface. An increase in the coverage led to an increase in the grain size as indicated by AFM. However, XRD results indicated that the crystallite size remained almost constant while the appearance of peaks corresponding to other crystalline orientations suggests the coalescence of the original crystallites and an increase in size of the more dense planes, namely [111]. (author)

  6. Hydrothermal synthesis of fine oxide powders

    Indian Academy of Sciences (India)


    Inorganic powders are among the most important factors in many fields of materials such as ceramics, catalysts, medicines, food, etc. There are many papers and books related to powders preparation by many authors (Veale. 1972; Kato and Yamaguchi 1983; Vincenzini 1983;. Brinker et al 1984; Johnson Jr. 1987; Messing ...

  7. Evaluating the Johanson theory for titanium powder

    CSIR Research Space (South Africa)

    Chikosha, S


    Full Text Available . In this study, the Johanson theory was used to determine the rolling parameters of titanium powder. Preliminary results of the nip angle, nip pressures and maximum horizontal pressures of the mill for the powder rolled on a 55mm diameter roll with roll gap sizes...

  8. Autoclave heat treatment for prealloyed powder products (United States)

    Freche, J. C.; Ashbrook, R. L.


    Technique could be applied directly to loose powders as part of hot pressing process of forming them to any required shapes. This would eliminate initial extrusion step commonly applied to prealloyed powders, substantially reduce cost of forming operation, and result in optimum properties.

  9. Jetting formation of the explosively loaded powders (United States)

    Xue, Kun; Yu, Qiqi


    The formation of jet-like structures is widely reported in the explosive dispersal of powders surrounding high explosive charges. The jetting of powder beds initiates upon the shock wave reaches the outer edge of the charge. Opposed to the interface instability theory, a hollow sphere based bulk fragmentation model is established to account for the jetting of powders. A two-phase process, namely the nucleation and free expansion of hollow spheres, corresponds to the unloading process of the powder compact caused by the rarefaction waves which governs the fragmentation of the powders. The separation between adjacent hollow spheres dictates the size of the particle clusters, which would evolve into particle jets in later times. The predicted breakup time and the size of particle jets agree well with the experimental results. The increased moisture content in powders results in an increased number of particle jets. This moisture effect can be understood in light of the varied energy distribution due to the incompressibility of the interstitial liquids trapped inside the inter-grain pores. The portion of shock energy which is not consumed in the shock compaction of the wet powders would be dissipated through the viscous shear flows during the unloading of the wet powder compact. The excessive viscous energy requires to activate more localized shear flows, accordingly leading to an increased number of particle jets.

  10. Characterization of mock high-explosive powder

    Energy Technology Data Exchange (ETDEWEB)

    Schmitt, C.R.; Dorsey, G.F.


    Analytical characterization and explosibility tests were made on a simulative high-explosive powder consisting of cyanuric acid, melamine, nitrocellulose, and tris-(..beta..-chloroethyl)-phosphate. Tests indicated that the powder presents no unusual safety or health hazards in isostatic-pressing and dry-machining operations.

  11. Preparation of silver powder through glycerol process

    Indian Academy of Sciences (India)

    High purity fine silver powder with uniform particle morphology was prepared through glycerol process. The process involves reduction of silver nitrate by glycerol under atmospheric conditions at a temperature below 175°C. Glycerol, in this process, acts as a solvent as well as a reducing agent. The powders prepared ...

  12. A breath actuated dry powder inhaler

    NARCIS (Netherlands)

    de Boer, Anne; Frijlink, Henderik W.; Hagedoorn, Paul


    A breath actuated dry powder inhaler with a single air circulation chamber for de-agglomeration of entrained powdered medicament using the energy of the inspiratory air stream. The chamber has a substantially polygonal sidewall, a plurality of air supply channels entering the chamber substantially

  13. Slip casting and nitridation of silicon powder (United States)

    Seiko, Y.


    Powdered Silicon was slip-cast with a CaSO4 x 0.5H2O mold and nitrided in a N atm. containing 0 or 5 vol. % H at 1000 to 1420 deg. To remove the castings, the modeling faces were coated successively with an aq. salt soap and powdered cellulose containing Na alginate, and thus prevented the sticking problem.

  14. Computational modelling for dry-powder inhalers

    NARCIS (Netherlands)

    Kröger, Ralf; Woolhouse, Robert; Becker, Michael; Wachtel, Herbert; de Boer, Anne; Horner, Marc


    Computational fluid dynamics (CFD) is a simulation tool used for modelling powder flow through inhalers to allow optimisation both of device design and drug powder. Here, Ralf Kröger, Consulting Senior CFD Engineer, ANSYS Germany GmbH; Marc Horner, Lead Technical Services Engineer, Healthcare,

  15. Wet powder seal for gas containment (United States)

    Stang, Louis G.


    A gas seal is formed by a compact layer of an insoluble powder and liquid filling the fine interstices of that layer. The smaller the particle size of the selected powder, such as sand or talc, the finer will be the interstices or capillary spaces in the layer and the greater will be the resulting sealing capacity, i.e., the gas pressure differential which the wet powder layer can withstand. Such wet powder seal is useful in constructing underground gas reservoirs or storage cavities for nuclear wastes as well as stopping leaks in gas mains buried under ground or situated under water. The sealing capacity of the wet powder seal can be augmented by the hydrostatic head of a liquid body established over the seal.

  16. Electronic Nose Study of Powdered Garlic

    Directory of Open Access Journals (Sweden)

    Rosa E. Baby


    Full Text Available An electronic nose was used to study the odour profile of garlic, separating the powered samples of eight cultivars and proving to be useful to discriminate garlic specimen dried by lyophilization and oven-dried and humidified specimen (before dried by both techniques for each cultivar. Pattern recognition and multivariate analysis of the electronic nose data has enabled to easily separate the garlic cultivars, to clearly discriminate the lyophilized or oven-dried specimen and the non humidified samples from the humidified powders maintaining, in every case, the cultivars identification. The humidification of lyophilized powders has shown a sharp separation of cultivars, otherwise, in the humidified oven-dried powders, their identification resulted less precise. This fact enabled to infer that lyophilized powders (either dry or humidified better retained their odour profile than oven-dried powders, maintaining the properties of each cultivar.

  17. Sun drying of residual annatto seed powder

    Directory of Open Access Journals (Sweden)

    Dyego da Costa Santos


    Full Text Available Residual annatto seeds are waste from bixin extraction in the food, pharmaceutical and cosmetic industries. Most of this by-product is currently discarded; however, the use of these seeds in human foods through the elaboration of powder added to other commercial powders is seen as a viable option. This study aimed at drying of residual annatto powder, with and without the oil layer derived from the industrial extraction of bixin, fitting different mathematical models to experimental data and calculating the effective moisture diffusivity of the samples. Powder containing oil exhibited the shortest drying time, highest drying rate (≈ 5.0 kg kg-1 min-1 and highest effective diffusivity (6.49 × 10-12 m2 s-1. All mathematical models assessed were a suitable representation of the drying kinetics of powders with and without oil, with R2 above 0.99 and root mean square error values lower than 1.0.

  18. Characterizing the Phyllosilicates and Amorphous Phases Found by MSL Using Laboratory XRD and EGA Measurements of Natural and Synthetic Materials (United States)

    Rampe, Elizabeth B.; Morris, Richard V.; Chipera, Steve; Bish, David L.; Bristow, Thomas; Archer, Paul Douglas; Blake, David; Achilles, Cherie; Ming, Douglas W.; Vaniman, David; hide


    The Curiosity Rover landed on the Peace Vallis alluvial fan in Gale crater on August 5, 2012. A primary mission science objective is to search for past habitable environments, and, in particular, to assess the role of past water. Identifying the minerals and mineraloids that result from aqueous alteration at Gale crater is essential for understanding past aqueous processes at the MSL landing site and hence for interpreting the site's potential habitability. X-ray diffraction (XRD) data from the CheMin instrument and evolved gas analyses (EGA) from the SAM instrument have helped the MSL science team identify phases that resulted from aqueous processes: phyllosilicates and amorphous phases were measure in two drill samples (John Klein and Cumberland) obtained from the Sheepbed Member, Yellowknife Bay Fm., which is believed to represent a fluvial-lacustrine environment. A third set of analyses was obtained from scoop samples from the Rocknest sand shadow. Chemical data from the APXS instrument have helped constrain the chemical compositions of these secondary phases and suggest that the phyllosilicate component is Mg-enriched and the amorphous component is Fe-enriched, relatively Si-poor, and S- and H-bearing. To refine the phyllosilicate and amorphous components in the samples measured by MSL, we measured XRD and EGA data for a variety of relevant natural terrestrial phyllosilicates and synthetic mineraloids in laboratory testbeds of the CheMin and SAM instruments. Specifically, Mg-saturated smectites and vermiculites were measured with XRD at low relative humidity to understand the behavior of the 001 reflections under Mars-like conditions. Our laboratory XRD measurements suggest that interlayer cation composition affects the hydration state of swelling clays at low RH and, thus, the 001 peak positions. XRD patterns of synthetic amorphous materials, including allophane, ferrihydrite, and hisingerite were used in full-pattern fitting (FULLPAT) models to help

  19. Powder strength distributions for understanding de-agglomeration of lactose powders. (United States)

    Das, Shyamal C; Behara, Srinivas Ravindra Babu; Bulitta, Jurgen B; Morton, David A V; Larson, Ian; Stewart, Peter J


    The purpose was to calculate distributions of powder strength of a cohesive bed to explain the de-agglomeration of lactose. De-agglomeration profiles of Lactohale 300(®) (L300) and micronized lactose (ML) were constructed by particle sizing aerosolised plumes dispersed at air flow rates of 30-180 l/min. The work of cohesion distribution was determined by inverse gas chromatography. The primary particle size and tapped density distributions were determined. Powder strength distributions were calculated by Monte Carlo simulations from distributions of particle size, work of cohesion and tapped density measurements. The powder strength distribution of L300 was broader than that of ML. Up to 85th percentile, powder strength of L300 was lower than ML which was consistent with the better de-agglomeration of L300 at low flow rates. However, ~15% of L300 particles had higher powder strength than ML which likely to cause lower de-agglomeration for L300 at high air flow rates. Cohesive lactose powders formed matrices of non-homogenous powder strength. De-agglomeration of cohesive powders has been shown to be related to powder strength. This study provided new insights into powder de-agglomeration by a new approach for calculating powder strength distributions to better understand complex de-agglomeration behaviour.

  20. Application of powder rheometer to determine powder flow properties and lubrication efficiency of pharmaceutical particulate systems. (United States)

    Navaneethan, Charu V; Missaghi, Shahrzad; Fassihi, Reza


    The objective of this study was to understand the behavior of particulate systems under different conditions of shear dynamics before and after granulation and to investigate the efficiency of powder lubrication. Three drug powders, metronidazole, colloidal bismuth citrate, and tetracycline hydrochloride, were chosen as model drugs representing noncohesive and cohesive powder systems. Each powder was individually granulated with microcrystalline cellulose and 5%PVP as a binder. One portion from each granulation was lubricated with different levels of magnesium stearate for 5 minutes. The powder characterization was performed on the plain powders, nonlubricated and lubricated granules using powder rheometer equipped with a helical blade rotating and moving under experimentally fixed set of parameters. The profiles of interaction during the force-distance measurements indicate that powder compresses, expands, and shears many times in a test cycle. Test profiles also clearly reveal existence of significant differences between cohesive and noncohesive powders. In all cases lubrication normalized the overall interactive nature of the powder by reducing peaks and valleys as observed from the profiles and reduced the frictional effect. The developed methods are easy to perform and will allow formulation scientists to better understand powder behavior and help in predicting potential impact of processing factors on particulate systems.

  1. Improving powder flow properties of a cohesive lactose monohydrate powder by intensive mechanical dry coating. (United States)

    Zhou, Qi; Armstrong, Brian; Larson, Ian; Stewart, Peter J; Morton, David A V


    The objective of this study was to improve the cohesive lactose powder flowability. A cohesive lactose monohydrate powder was processed in either a tumbling blender or an intensive mechanical processor with either magnesium stearate or fumed silica. No substantial changes in particle size were detected by laser diffraction following either treatment. The untreated lactose sample exhibited very poor powder flow. Only limited improvements in powder flowability were indicated after the tumbling blending, intensive mechanical processing with the fumed silica or without additives. However, the intensive mechanical processing of the lactose sample with magnesium stearate demonstrated exceptionally large increases in both poured and tapped density as well as notable improvements in all powder flowability indicators examined. Our findings support the use of intensive mechanical processing technique as an effective method to coat cohesive pharmaceutical powders with selected additives, modify the surface nature of the particles, reduce the interparticle cohesive forces and hence improve powder flowability. The subtle differences in powder flow behaviour of lactose samples between the untreated and tumbling blended powders with magnesium stearate were only detected by the powder rheometer using its dynamic mode, indicating its potential advantages over traditional powder flow characterisation approaches. (c) 2009 Wiley-Liss, Inc. and the American Pharmacists Association.

  2. Measurement of powder bed density in powder bed fusion additive manufacturing processes (United States)

    Jacob, G.; Donmez, A.; Slotwinski, J.; Moylan, S.


    Many factors influence the performance of additive manufacturing (AM) processes, resulting in a high degree of variation in process outcomes. Therefore, quantifying these factors and their correlations to process outcomes are important challenges to overcome to enable widespread adoption of emerging AM technologies. In the powder bed fusion AM process, the density of the powder layers in the powder bed is a key influencing factor. This paper introduces a method to determine the powder bed density (PBD) during the powder bed fusion (PBF) process. A complete uncertainty analysis associated with the measurement method was also described. The resulting expanded measurement uncertainty, U PBD (k  =  2), was determined as 0.004 g · cm-3. It was shown that this expanded measurement uncertainty is about three orders of magnitude smaller than the typical powder bed density. This method enables establishing correlations between the changes in PBD and the direction of motion of the powder recoating arm.

  3. Effect of the order and disorder of BaMoO4 powders in photoluminescent properties. (United States)

    Marques, Ana Paula A; Picon, Francini C; Melo, Dulce M A; Pizani, Paulo S; Leite, Edson R; Varela, José A; Longo, Elson


    The study of the photoluminescent properties affected by order and disorder of the BaMoO(4) powders is the principal objective in this work. BaMoO(4) compounds were prepared using soft chemical process called Complex Polymerization Method. In this work, different deagglomeration types and different heating rates were used to promote different disorder degrees. Scheelite type phase (BaMoO(4)) was determined by X-ray Diffraction (XRD), Fourier Transformed Infra-Red (FTIR) and Raman spectroscopy after heat treating the sample at 400 degrees C. The room temperature luminescence spectra revealed an intense single-emission band in the visible region. Based on XRD and Raman data it was observed that the transition between the completely disordered structure to completely ordered structure is a good condition for photoluminescence (PL) emission. The best PL emission is obtained when the material possesses short range disorder, i.e., is periodically ordered (XRD), but some disorder as measured by Raman spectroscopy. The excellent optical properties observed for disordered BaMoO(4) suggested that this material is a highly promising candidate for optical applications.

  4. Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders. (United States)

    Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong; Zheng, Feng


    Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH₄)₂C₂O₄·H₂O and Na₂CO₃) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7-10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na₂CO₃ precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed.

  5. Fabrication of Yb:Sc2O3 laser ceramics by vacuum sintering co-precipitated nano-powders (United States)

    Liu, Qiang; Dai, Zhengfa; Hreniak, Dariusz; Li, Shanshan; Liu, Wenbin; Wang, Wei; Luo, Wei; Li, Chaoyu; Dai, Jiawei; Chen, Haohong; Kou, Huamin; Shi, Yun; Pan, Yubai; Li, Jiang


    Ytterbium doped scandium oxide (Yb:Sc2O3) nano-powders were synthesized by a co-precipitation method. Ammonium hydrogen carbonate (NH4HCO3) and ammonia sulfate ((NH4)2SO4) were used in the precipitation process as the precipitant and dispersing agent, respectively. Structural properties and morphology of the precursor and nano-powders were investigated by BET, XRD, and SEM measurements. Ultra-fine and low agglomerated 5 at%Yb:Sc2O3 powders with the average particle size of 86 nm were obtained after calcination of the precipitate at 1100 °C for 5 h, that was found to be the optimal temperature for preparation of 5 at%Sc2O3 powders for further sintering. 5 at%Yb:Sc2O3 transparent ceramics with in-line transmittance of 73.9% at 1100 nm and average grain size of 182 μm were fabricated by vacuum sintering of the optimal powder at 1850 °C for 10 h. The microstructure, the spectroscopic properties and the gain characteristics of obtained 5 at%Yb:Sc2O3 ceramics were also studied and discussed.

  6. Combustion synthesis of nanocrystalline ceria (CeO{sub 2}) powders by a dry route

    Energy Technology Data Exchange (ETDEWEB)

    Hwang, C.-C. [Department of Applied Chemistry, Chung Cheng Institute of Technology, NDU, Dashi, Taoyuan 335, Taiwan (China)]. E-mail:; Huang, T.-H. [Department of Applied Chemistry, Chung Cheng Institute of Technology, NDU, Dashi, Taoyuan 335, Taiwan (China); Tsai, J.-S. [Department of Applied Chemistry, Chung Cheng Institute of Technology, NDU, Dashi, Taoyuan 335, Taiwan (China); Lin, C.-S. [School of Defense Science, Chung Cheng Institute of Technology, NDU, Dashi, Taoyuan 335, Taiwan (China); Peng, C.-H. [Chemical Systems Research Division, Chung Shan Institute of Science and Technology, Lungtan, Taoyuan 325, Taiwan (China)


    In this study, ceria (CeO{sub 2}) powders were synthesized with 50 g per batch via a combustion technique using two kinds of starting materials-urea [(NH{sub 2}){sub 2}CO] (as a fuel) and ceric ammonium nitrate [Ce(NH{sub 4}){sub 2}(NO{sub 3}){sub 6}] (acting as both the source of cerium ion and an oxidizer). The starting materials were mixed thoroughly without adding water, and then ignited in the air at room temperature. It underwent a self-combustion process with a large amount of smoke, a voluminous loose product. The as-synthesized powders were characterized by X-ray diffraction (XRD) analysis, transmission electron microscope (TEM), scanning electron microscope (SEM), CHN elemental analyzer, surface area measurements, and sinterability. Experimental results revealed that the nanocrystalline CeO{sub 2} powders with low impurity content (<0.2 wt%) can be obtained after combustion. Specific surface area and primary crystallite particle size of the ceria powder were {approx}50 m{sup 2}/g and {approx}25 nm, respectively, through the stoichiometric fuel/oxidizer ratio reaction. The powder, when cold pressed and sintered in the air at 1250 deg. C for 1 h, was measured to attain the sintered density {approx}92% of theoretical density having submicron grain size. In addition, the thermal decomposition and combustion process of the reactant mixture were investigated using thermogravimetry (TG), differential scanning calorimetry (DSC), and mass spectrometry (MS) techniques simultaneously. Based on the results of thermal analysis, a possible mechanism concerning the combustion reaction is proposed.

  7. Inhalable Lactose-Based Dry Powder Formulations of Low Molecular Weight Heparin (United States)

    Bai, Shuhua; Gupta, Vivek


    Abstract Background Currently low molecular weight heparin (LMWH) is administered as subcutaneous injection. This study sought to investigate the feasibility of LMWH as an inhalable dry powder (DPI) formulation and evaluate the interaction of the drug with lactose when used as a carrier. The study also compares the extent of pulmonary absorption of LMWH administered as a dry powder with that administered as an aerosolized aqueous solution. Methods The formulations were prepared by mixing LMWH in an aqueous solution of lactose followed by lyophilization of the resulting solution. The lyophilized preparation was then ground and sieved. Physical characterization of the formulations was performed by Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), particle size analysis, and determination of aerodynamic diameter. For in vivo studies, formulations were administered to anesthetized rats, and drug absorption was monitored by measuring plasma antifactor Xa activity. Results and Conclusions In the FTIR scan, all characteristic peaks of lactose and LMWH were observed, suggesting that there was no strong interaction between lactose and LMWH. Although the aerodynamic diameter of the formulation (DPI-2) that was sieved through 170- and 230-mesh screens was similar to that of the formulation (DPI-1) sieved through 120- and 170-mesh screens, the particle sizes of the two formulations were significantly different. Dry powder formulations of LMWH were better absorbed compared to an inhalable solution of LMWH. One of the dry powder formulations (DPI-2) produced an almost 1.5-fold increase in the relative bioavailability (41.6%) compared to the liquid formulation of LMWH (32.5%). Overall, the data presented here suggest that lactose does not adversely affect the physical-chemical characteristics of the drug, and that lactose can be used as a carrier for pulmonary delivery of LMWH. PMID:19778265

  8. [Preparation and characterization of zirconium hydroxide powder for fluoride adsorption]. (United States)

    Yang, Shuo; Dou, Xiao-min; Liang, Wen-yan; Wang, Yi-li; Lin, Wei


    The method co-precipitation was applied to preparation the zirconium hydroxide as a type drinking-water defluoridation adsorbent. The effect of the preparation conditions on the adsorptive capacity was studied. The optimization of preparation condition for zirconium hydroxide concludes that co-precipitation time is 10 h, pH value is 7.0, drying time is 72 h, calcination temperature is below 100 degrees C. Also, the adsorbent samples were characterized. SEM measurements reveal that zirconium hydroxide powder are constructed by several small particles, with a diameter about 20-30 microm. XRD and TG/DTA measurements show that the zirconium hydroxide samples have amorphous phase and converse to tetragonal phase when calcined at 600 degrees C. Nitrogen adsorption/desorption measurements show that samples have large surface areas of 138.4 m2/g and a 2 nm average pore size distribution in the mesopore region. The performance of zirconium hydroxide regeneration process was investigated. The results show that the regeneration techniques are very suitable to restore the fluorine-removal ability for zirconium hydroxide.

  9. Effect of waste rubber powder as filler for plywood application

    Directory of Open Access Journals (Sweden)

    Ong Huei Ruey


    Full Text Available The study investigated the suitability of waste rubber powder (WRP use as filler in adhesive formulation for plywood application. Melamine Urea Formaldehyde (MUF was employed as resin for formulating the wood adhesive. To improve chemical properties and bonding quality of adhesive, WRP was treated by different chemicals like 20% nitric acid, 30% hydrogen peroxide and acetone solution. The treated WRP were analysed by XRD and it showed that inorganic compounds were removed and carbon was remained as major component under the treatment of 20% HNO3. The treatment improved the mechanical properties like shear strength and formaldehyde emission of plywood (high shear strength and low formaldehyde emission. The physico-chemical interaction between the wood, resin and filler was investigated using fourier transform infrared spectroscopic (FTIR technique and the interactions among N-H of MUF and C=O of wood and WRP were identified. The morphology of wood-adhesive interface was studied by field emission scanning electron microscope (FESEM and light microscope (LM. It showed that the penetration of adhesives and fillers through the wood pores was responsible for mechanical interlocking. Therefore, chemically treated WRP proved its potential use as filler in MUF based adhesive for making plywood.

  10. Nanostructural Features of Silver Nanoparticles Powder Synthesized through Concurrent Formation of the Nanosized Particles of Both Starch and Silver

    Directory of Open Access Journals (Sweden)

    A. Hebeish


    Full Text Available Green innovative strategy was developed to accomplish silver nanoparticles formation of starch-silver nanoparticles (St-AgNPs in the powder form. Thus, St-AgNPs were synthesized through concurrent formation of the nanosized particles of both starch and silver. The alkali dissolved starch acts as reducing agent for silver ions and as stabilizing agent for the formed AgNPs. The chemical reduction process occurred in water bath under high-speed homogenizer. After completion of the reaction, the colloidal solution of AgNPs coated with alkali dissolved starch was cooled and precipitated using ethanol. The powder precipitate was collected by centrifugation, then washed, and dried; St-AgNPs powder was characterized using state-of-the-art facilities including UV-vis spectroscopy, Transmission Electron Microscopy (TEM, particle size analyzer (PS, Polydispersity index (PdI, Zeta potential (ZP, XRD, FT-IR, EDX, and TGA. TEM and XRD indicate that the average size of pure AgNPs does not exceed 20 nm with spherical shape and high concentration of AgNPs (30000 ppm. The results obtained from TGA indicates that the higher thermal stability of starch coated AgNPS than that of starch nanoparticles alone. In addition to the data obtained from EDX which reveals the presence of AgNPs and the data obtained from particle size analyzer and zeta potential determination indicate that the good uniformity and the highly stability of St-AgNPs.

  11. Nano-sized ZnO powders prepared by co-precipitation method with various pH (United States)

    Purwaningsih, S. Y.; Pratapa, S.; Triwikantoro, Darminto


    In this work, nano-sized ZnO powders have been synthesized by the co-precipitation method with Zn(CH3COOH)2.2H2O, HCl, and NH3.H2O as raw materials in various pH ranging from 8 to 10. The purity, microstructure, chemical group analysis, morphology of the prepared ZnO powders were studied by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), energy dispersive X-ray spectrometry (EDX), and scanning electron microscope (SEM), respectively. Rietveld refinement of XRD data showed that ZnO crystallizes in the wurtzite structure with high purity. The obtained powders were nano-sized particles with the average crystallite size about 17.9 ± 2.1 nm synthesized with pH of 9.5, at 85°C, and stirring time of 6 h. The SEM results have visualied the morphology of ZnO nanoparticles with spherical-like shape. The effect of processing conditions on morphology of ZnO was also discussed.

  12. 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


    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.

  13. Hygroscopic behavior of lyophilized acerola pulp powder

    Directory of Open Access Journals (Sweden)

    Luciana C. Ribeiro


    Full Text Available ABSTRACT Powder products are characterized by their practicality and long life. However, fruit powders have high hygroscopicity and tend to agglomerate due to its hydrophilic nature. The isotherms of equilibrium moisture content apply to the study of dehydrated food preservation potential. Acerola is a nutritionally rich fruit, with great economic and industrial potential. The objective of this study was to analyse acerola powder adsorption isotherms obtained by lyophilization and characterize the powder obtained from lyophilized acerola pulp. Analysis of hygroscopicity, solubility and degree of caking were performed. Isotherms were represented by the mathematical models of GAB, BET, Henderson and Oswin, at temperatures of 25, 35 and 45 °C. According to the results, the obtained powder showed hygroscopicity of 5.96 g of absorbed water 100g-1 of solids, solubility of 95.08% and caking of 14.12%. The BET model showed the best fit to the adsorption isotherms of the acerola pulp powder obtained by lyophilization. The obtained isotherm was of type III, with a "J" shape. There was an inversion of the effect of temperature on the isotherms of acerola powders.

  14. Interfacial reactions and wetting in Al-Mg sintered by powder metallurgy process

    Energy Technology Data Exchange (ETDEWEB)

    Faisal, Heny, E-mail:; Darminto,; Triwikantoro,; Zainuri, M. [Physics Department, Math and Science Faculty, Institute of Technology Sepuluh Nopember (ITS) Jl. Arief Rahman Hakim, Surabaya 60111 (Indonesia)


    Was conducted to analyze the effect of temperature variation on the bonding interface sintered composite Al-Mg and analyze the effect of variations of the density and hardness sinter. Research carried out by the base material powders of Al, Mg powder and solvent n-butanol. The method used in this study is a powder metallurgy, with a composition of 60% volume fraction of Al - 40% Mg. Al-Mg mixing with n-butanol for 1 hour at 500 rpm. Then the emphasis (cold comression) with a size of 1.4 cm in diameter dies and height of 2.8 cm, is pressed with a force of 20 MPa and held for 15 minutes. After the sample into pellets, then sintered at various temperatures 300 °C, 350 °C, 400 °C and 450 °C. Characterization is done by using the testing green density, sintered density, X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), vickers microhardness, and press test. XRD data analysis done by using X’Pert High Score Plus (HSP) to determine whether there is a new phase is formed. Test results show that the sintered density increasing sintering temperature, the resulting density is also increasing (shrinkage). However, at a temperature of 450 °C decreased (swelling). With the increased sinter density, interfacial bonding getting Kuta and more compact so that its hardness is also increased. From the test results of SEM / EDX, there Mg into Al in the border area. At temperatures of 300 °C, 350 °C, 400 °C, the phase formed is Al, Mg and MgO. While phase is formed at a temperature of 450 °C is aluminum magnesium (Al{sub 3}Mg{sub 2}), Aluminum Magnesium Zinc (AlMg{sub 2}Zn).

  15. Dustiness of fine and nanoscale powders. (United States)

    Evans, Douglas E; Turkevich, Leonid A; Roettgers, Cynthia T; Deye, Gregory J; Baron, Paul A


    Dustiness may be defined as the propensity of a powder to form airborne dust by a prescribed mechanical stimulus; dustiness testing is typically intended to replicate mechanisms of dust generation encountered in workplaces. A novel dustiness testing device, developed for pharmaceutical application, was evaluated in the dustiness investigation of 27 fine and nanoscale powders. The device efficiently dispersed small (mg) quantities of a wide variety of fine and nanoscale powders, into a small sampling chamber. Measurements consisted of gravimetrically determined total and respirable dustiness. The following materials were studied: single and multiwalled carbon nanotubes, carbon nanofibers, and carbon blacks; fumed oxides of titanium, aluminum, silicon, and cerium; metallic nanoparticles (nickel, cobalt, manganese, and silver) silicon carbide, Arizona road dust; nanoclays; and lithium titanate. Both the total and respirable dustiness spanned two orders of magnitude (0.3-37.9% and 0.1-31.8% of the predispersed test powders, respectively). For many powders, a significant respirable dustiness was observed. For most powders studied, the respirable dustiness accounted for approximately one-third of the total dustiness. It is believed that this relationship holds for many fine and nanoscale test powders (i.e. those primarily selected for this study), but may not hold for coarse powders. Neither total nor respirable dustiness was found to be correlated with BET surface area, therefore dustiness is not determined by primary particle size. For a subset of test powders, aerodynamic particle size distributions by number were measured (with an electrical low-pressure impactor and an aerodynamic particle sizer). Particle size modes ranged from approximately 300 nm to several micrometers, but no modes below 100 nm, were observed. It is therefore unlikely that these materials would exhibit a substantial sub-100 nm particle contribution in a workplace.

  16. Microstructure of as-fabricated UMo/Al(Si) plates prepared with ground and atomized powder (United States)

    Jungwirth, R.; Palancher, H.; Bonnin, A.; Bertrand-Drira, C.; Borca, C.; Honkimäki, V.; Jarousse, C.; Stepnik, B.; Park, S.-H.; Iltis, X.; Schmahl, W. W.; Petry, W.


    fuelplate is sealed. After this step, the UMo particles are tightly covered with Al as shown in Fig. 1. To access the meat layer, small samples have been cut from the fuel plates. The AlFeNi cladding has been removed using abrasive paper and diamond polishing paste. Cross sections were prepared from each sample and examined using SEM/EDX and XRD. Laboratory scale XRD Laboratory sealed-tube XRD on a STOE-STADIP diffractometer equipped with an incident beam focusing monochromator and used in reflection geometry with respect to the sample. MoK-α radiation has been used. Details on the systems used can be found in [39]. mu;-XRD using micro-focused synchrotron radiation at the Swiss Light Source μ-XAS beamline (PSI, Switzerland). At SLS, the beam size was 3 × 3 μm2, the energy was 19.7 keV. Further details on the experimental procedure can be found in [40]. Only very small sample volumes are probed with this technique, therefore the results may not be representative for the whole miniplate. The standard deviation of the lattice parameters obtained with this method is ±0.01 Å in case not different given. High-energy XRD (HE-XRD) in transmission mode using synchrotron radiation at the "High Energy Diffraction and Scattering Beamline ID15B" of ESRF. An X-ray energy of 87 keV has been used, the beam size was 0.3 × 0.3 mm2. Details on the experimental procedure are presented in [41,42]. It was possible to determine the average mass fractions of the phases present inside the sample using this technique. The standard deviation of the lattice parameters obtained with this method is ±0.001 Å in case not different given. laser granulometry to determine the size distribution of the particles, XRD for phase identification. Granulometry measurements showed that a significant amount of very fine particles of a few μm to 10 μm size are present in the first class of powder.In both cases, laboratory XRD analyses evidenced only two phases: γ-UMo and UO2. In contrast to observations on

  17. Fire hazard of titanium powder layers mixed with inert nano TiO2 powder. (United States)

    Yuan, Chunmiao; Cai, Jingzhi; Amyotte, Paul; Li, Chang; Bu, Yajie; Liu, Kangfu; Li, Gang


    Metallic dust layers are highly sensitive to ignition from common ignition sources, even when mixed with high percentages of inert solids. In turn, dust layer fires are a potential ignition source for dust explosions or other damaging fires. Flame spread velocity (FSV), as a potential parameter for evaluating fire hazard, was investigated for titanium powder layers mixed with inert nano TiO2 powder in both natural convection and in forced airflow conditions. Increased mass percentage of nano TiO2 powder decreased FSV of Ti powder mixtures as expected. The mixing ratio of nano TiO2 to fully suppress layer fires was 80% and 90% for micro and nano Ti powder, respectively. Mechanisms governing flame spread across a layer of nano Ti powder differed from those of a layer of micro Ti powder. FSV in no airflow conditions was higher than in aided airflow for micro Ti powder because conduction was the dominant heat transfer mechanism. However, FSV in no airflow was lower than in opposed airflow for nano Ti powder because convection/radiation was the dominant heat transfer mechanism. A fly fire phenomenon contributed to greater FSVs and higher fire hazard with nano Ti powder mixtures under aided airflow conditions. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Use of whey powder and skim milk powder for the production of fermented cream

    Directory of Open Access Journals (Sweden)

    Ceren AKAL


    Full Text Available Abstract This study is about the production of fermented cream samples having 18% fat by addition of starter cultures. In order to partialy increase non-fat solid content of fermented cream samples, skim milk powder and demineralized whey powder in two different rates (50% and 70% were used. Samples were analyzed for changes in their biochemical and physicochemical properties (total solid, ash, fat, titratable acidity, pH value, total nitrogen, viscosity, tyrosine, acid number, peroxide and diacetyl values during 29-day of storage period. Samples tested consisted of 7 different groups; control group (without adding any powder, skim milk powder, 50% demineralized whey powder and 70% demineralized whey powder samples were in two different addition rate (2% and 4%. Also samples were analyzed for sensory properties. According to the results obtained, the addition of milk powder products affected titratable acidity and tyrosine values of fermented cream samples. Although powder addition and/or storage period didn’t cause significant variations in total solid, ash, fat, pH value, viscosity, acid number, peroxide, tyrosine and diacetyl values; sensory properties of fermented cream samples were influenced by both powder addition and storage period. Fermented cream containing 2% skim milk powder gets the top score of sensory evaluation among the samples.

  19. Sintering of Cu–Al2O3 nano-composite powders produced by a thermochemical route

    Directory of Open Access Journals (Sweden)



    Full Text Available This paper presents the synthesis of nano-composite Cu–Al2O3 powder by a thermochemical method and sintering, with a comparative analysis of the mechanical and electrical properties of the obtained solid samples. Nano-crystalline Cu–Al2O3 powders were produced by a thermochemical method through the following stages: spray-drying, oxidation of the precursor powder, reduction by hydrogen and homogenization. Characterization of powders included analytical electron microscopy (AEM coupled with energy dispersive spectroscopy (EDS, differenttial thermal and thermogravimetric (DTA–TGA analysis and X-ray diffraction (XRD analysis. The size of the produced powders was 20–50 nm, with a noticeable presence of agglomerates. The composite powders were characterized by a homogenous distribution of Al2O3 in a copper matrix. The powders were cold pressed at a pressure of 500 MPa and sintered in a hydrogen atmosphere under isothermal conditions in the temperature range from 800 to 900 °C for up to 120 min. Characterization of the Cu–Al2O3 sintered system included determination of the density, relative volume change, electrical and mechanical properties, examination of the microstructure by SEM and focused ion beam (FIB analysis, as well as by EDS. The obtained nano-composite, the structure of which was, with certain changes, presserved in the final structure, provided a sintered material with a homogenеous distribution of dispersoid in a copper matrix, with exceptional effects of reinforcement and an excellent combination of mechanical and electrical properties.

  20. Preparation and Evaluation of Herbal Shampoo Powder (United States)

    Dubey, Sachin; Nema, Neelesh; Nayak, S.


    Two preparations of herbal shampoo powder were formulated using some common traditional drugs used by folk and traditional people of Bundelkhand region (M.P) India, for hair care. The preparations were formulated using bahera, amla, neem tulsi, shikakai henna & brahmi evaluated for organoleptic, powder charecterestics, foam test and physical evaluation. As the selected drugs being used since long time as single drug or in combination, present investigations will further help to establish a standard formulation and evaluation parameters, which will certainly help in the standardization for quality and purity of such type of herbal powder shampoos. PMID:22557149

  1. Comparative investigation of Fourier Transform Infrared (FT-IR) spectroscopy and X-ray Diffraction (XRD) in the determination of cotton fiber crystallinity (United States)

    Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI) from the X-ray diffraction (XRD) measurement, in its present state XRD procedure can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous po...

  2. Astrobiological Significance of Definitive Mineralogical Analysis of Martian Surface Samples Using the CheMin XRD/XRF Instrument (United States)

    Feldman, S. M.; Blake, D. F.; Sarrazin, P.; Bish, D. L.; Chipera, S. J.; Vaniman, D. T.; Collins, S.


    The search for evidence of habitability, or of extant or extinct life on Mars, will initially be a search for evidence of past or present conditions supportive of life. The three key requirements for the emergence of life are thought to be liquid water; a suitable energy source; and chemical building blocks. CheMin is a miniaturized XRD/XRF (X-Ray diffraction / X-ray fluorescence) instrument which has been developed for definitive mineralogic analysis of soils and rocks on the Martian surface. The CheMin instrument can provide information that is highly relevant to each of these habitability requirements as summarized below.

  3. Titania nanotube powders obtained by rapid breakdown anodization in perchloric acid electrolytes

    Energy Technology Data Exchange (ETDEWEB)

    Ali, Saima, E-mail:; Hannula, Simo-Pekka


    Titania nanotube (TNT) powders are prepared by rapid break down anodization (RBA) in a 0.1 M perchloric acid (HClO{sub 4}) solution (Process 1), and ethylene glycol (EG) mixture with HClO{sub 4} and water (Process 2). A study of the as-prepared and calcined TNT powders obtained by both processes is implemented to evaluate and compare the morphology, crystal structure, specific surface area, and the composition of the nanotubes. Longer TNTs are formed in Process 1, while comparatively larger pore diameter and wall thickness are obtained for the nanotubes prepared by Process 2. The TNTs obtained by Process 1 are converted to nanorods at 350 °C, while nanotubes obtained by Process 2 preserve tubular morphology till 350 °C. In addition, the TNTs prepared by an aqueous electrolyte have a crystalline structure, whereas the TNTs obtained by Process 2 are amorphous. Samples calcined till 450 °C have XRD peaks from the anatase phase, while the rutile phase appears at 550 °C for the TNTs prepared by both processes. The Raman spectra also show clear anatase peaks for all samples except the as-prepared sample obtained by Process 2, thus supporting the XRD findings. FTIR spectra reveal the presence of O-H groups in the structure for the TNTs obtained by both processes. However, the presence is less prominent for annealed samples. Additionally, TNTs obtained by Process 2 have a carbonaceous impurity present in the structure attributed to the electrolyte used in that process. While a negligible weight loss is typical for TNTs prepared from aqueous electrolytes, a weight loss of 38.6% in the temperature range of 25–600 °C is found for TNTs prepared in EG electrolyte (Process 2). A large specific surface area of 179.2 m{sup 2} g{sup −1} is obtained for TNTs prepared by Process 1, whereas Process 2 produces nanotubes with a lower specific surface area. The difference appears to correspond to the dimensions of the nanotubes obtained by the two processes. - Graphical abstract

  4. Thermal evolution of CaO-doped HfO{sub 2} films and powders

    Energy Technology Data Exchange (ETDEWEB)

    Barolin, S A; Sanctis, O A de [Lab. Materiales Ceramicos, FCEIyA, Universidad Nacional de Rosario, IFIR-CONICET (Argentina); Caracoche, M C; Martinez, J A; Taylor, M A; Pasquevich, A F [Departamento de Fisica, FCE, Universidad Nacional de La Plata, IFLP-CONICET (Argentina); Rivas, P C, E-mail: [Facultad de Ciencias Agronomicas y Forestales, Universidad Nacional de La Plata, IFLP (Argentina)


    Solid solutions of ZrO2 and HfO2 are potential electrolyte materials for intermediate-temperature SOFC because both are oxygen-ion conductors. The main challenge for these compounds is to reduce the relatively high value of the activation energies vacancies diffusion, which is influenced by several factors. In this work the thermal evolution of CaO-HfO{sub 2} materials have been investigated. (CaO)y-Hf(1-y)O(2-y) (y = 0.06, 0.14 y 0.2) coatings and powders were synthesized by chemical solution deposition (CSD). Films were deposited onto alumina substrates by Dip Coating technique, the burning of organic waste was carried out at 500 deg. C under normal atmosphere and then the films were thermally treated at intervals of temperature rising to a maximum temperature of 1250 deg. C. By means Glazing Incidence X-ray Diffraction (rho-2theta configuration) the phases were studied in the annealed films. On the other hand, the thermal evolution and crystallization process of powders were analyzed in-situ by HT-XRD. The phenomena crystallization occurred in films and powders were analyzed. The activation energies of diffusion of oxygen vacancies of HfO2-14 mole% CaO and HfO2-20 mole% CaO films were measured from the thermal evolution of the relaxation constant measured by Perturbed Angular Correlation Technique.

  5. White light emission from Er2O3 nano-powder excited by infrared radiation (United States)

    Tabanli, Sevcan; Eryurek, Gonul; Di Bartolo, Baldassare


    Phosphors of Er2O3 nano-crystalline powders were synthesized by the thermal decomposition method. The structural properties of the nano-powders were investigated with XRD and HRTEM measurements. The cubic phase with a = 10.540 Å was the only phase observed. The average crystalline sizes and the widths of the grain size distribution curves were determined to be 27.2, 18.7 and 9.7 nm, respectively. The spectroscopic properties of the Er2O3 nano-powder were studied by measuring the luminescence, decay and rise patterns under 808 and 975 nm diode laser excitations. A peculiar effect of the pressure was observed since an optically active ion (Er) is part of the complex and not a dopant. A broad band of the white light emission combined with blue, green and red up-conversion emission bands of Er3+ ions were observed at 0.03 mbar pressure under both excitation wavelengths. Only, an intense broad band white light emission was observed from these nanocrystals at atmospheric pressure. Rising patterns show that the white light intensity reaches its maximum value more rapidly under 975 nm excitation although it decays slower than that of 808 nm excitation. The color quality parameters such as the color coordinate (CRI), correlated color temperature and the color rendering index were found to vary with both the excitation wavelength and the ambient pressure indicating that these nanocrystals could be considered good white light emitting source under the infrared excitations.

  6. Comparison of characteristics of hydroxyapatite powders synthesized from cuttlefish bone via precipitation and ball milling techniques (United States)

    Faksawat, K.; Kaewwiset, W.; Limsuwan, P.; Naemchanthara, K.


    The aim of this work was to compare characteristics of hydroxyapatite synthesized by precipitation and ball milling techniques. The cuttlefish bone powder was a precursor in calcium source and the di ammonium hydrogen orthophosphate powders was a precursor in phosphate source. The hydroxyapatite was synthesized by the both techniques such as precipitation and ball milling techniques. The phase formation, chemical structure and morphology of the both hydroxyapatite powders have been examined by X-ray diffractometer (XRD), Fourier transform infrared spectroscope (FTIR) and field emission scanning electron microscope (FESEM), respectively. The results show that the hydroxyapatite synthesized by precipitation technique formed hydroxyapatite phase slower than the hydroxyapatite synthesized by ball milling technique. The FTIR results show the chemical structures of sample in both techniques are similar. The morphology of the hydroxyapatite from the both techniques were sphere like shapes and particle size was about in nano scale. The average particle size of the hydroxyapatite by ball milling technique was less than those synthesized by precipitation technique. This experiment indicated that the ball milling technique take time less than the precipitation technique in hydroxyapatite synthesis.

  7. Laser Powder Cladding of Ti-6Al-4V α/β Alloy (United States)

    Al-Sayed Ali, Samar Reda; Hussein, Abdel Hamid Ahmed; Nofal, Adel Abdel Menam Saleh; Elgazzar, Haytham Abdelrafea; Sabour, Hassan Abdel


    Laser cladding process was performed on a commercial Ti-6Al-4V (α + β) titanium alloy by means of tungsten carbide-nickel based alloy powder blend. Nd:YAG laser with a 2.2-KW continuous wave was used with coaxial jet nozzle coupled with a standard powder feeding system. Four-track deposition of a blended powder consisting of 60 wt % tungsten carbide (WC) and 40 wt % NiCrBSi was successfully made on the alloy. The high content of the hard WC particles is intended to enhance the abrasion resistance of the titanium alloy. The goal was to create a uniform distribution of hard WC particles that is crack-free and nonporous to enhance the wear resistance of such alloy. This was achieved by changing the laser cladding parameters to reach the optimum conditions for favorable mechanical properties. The laser cladding samples were subjected to thorough microstructure examinations, microhardness and abrasion tests. Phase identification was obtained by X-ray diffraction (XRD). The obtained results revealed that the best clad layers were achieved at a specific heat input value of 59.5 J·mm−2. An increase by more than three folds in the microhardness values of the clad layers was achieved and the wear resistance was improved by values reaching 400 times. PMID:29036935

  8. Waste Fiber Powder Functionalized with Silver Nanoprism for Enhanced Raman Scattering Analysis (United States)

    Tang, Bin; Zeng, Tian; Liu, Jun; Zhou, Ji; Ye, Yong; Wang, Xungai


    Biomass disks based on fine powder produced from disposed wool fibers were prepared for surface-enhanced Raman scattering (SERS). The wool powders (WPs) were modified by silver nanoprisms via an assembly method and then pressed into disks using a hydraulic laboratory pellet press. Scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were used to characterize the WPs and disks before and after treatment with silver nanoparticles (AgNPs). The WPs retained porous structures after treatment with AgNPs. The silver nanoprisms on WPs were observed clearly and the localized surface plasmon resonance (LSPR) properties of silver nanoprisms led to blue color of wool powder (WP). The obtained WP disks with AgNPs were confirmed to enhance greatly the Raman signal of thiram. The SERS disks are low-cost and convenient to use, with high sensitivity. The characteristic SERS bands of 10-8 M thiram can be identified from WP disks containing silver nanoparticles.

  9. Laser Powder Cladding of Ti-6Al-4V α/β Alloy

    Directory of Open Access Journals (Sweden)

    Samar Reda Al-Sayed Ali


    Full Text Available Laser cladding process was performed on a commercial Ti-6Al-4V (α + β titanium alloy by means of tungsten carbide-nickel based alloy powder blend. Nd:YAG laser with a 2.2-KW continuous wave was used with coaxial jet nozzle coupled with a standard powder feeding system. Four-track deposition of a blended powder consisting of 60 wt % tungsten carbide (WC and 40 wt % NiCrBSi was successfully made on the alloy. The high content of the hard WC particles is intended to enhance the abrasion resistance of the titanium alloy. The goal was to create a uniform distribution of hard WC particles that is crack-free and nonporous to enhance the wear resistance of such alloy. This was achieved by changing the laser cladding parameters to reach the optimum conditions for favorable mechanical properties. The laser cladding samples were subjected to thorough microstructure examinations, microhardness and abrasion tests. Phase identification was obtained by X-ray diffraction (XRD. The obtained results revealed that the best clad layers were achieved at a specific heat input value of 59.5 J·mm−2. An increase by more than three folds in the microhardness values of the clad layers was achieved and the wear resistance was improved by values reaching 400 times.

  10. Co-precipitation synthesis of lutetium aluminum garnet (LuAG) powders: The influence of ethanol (United States)

    Pan, Liangjie; Jiang, Benxue; Fan, Jintai; Zhang, Pande; Mao, Xiaojian; Zhang, Long


    Aluminum Garnet (LuAG) precursors were co-precipitated by using ethanol-water as the precipitant solvent. The effect of different volume ratios of ethanol to water (R) on the preparation of pure-phase LuAG powders has been mainly studied. The evolution of phase, composition and micro-structure of the as-synthesized LuAG powders were characterized by TG/DTA, FTIR, XRD, BET, and SEM. The BET-equivalent diameter of LuAG nano particles increased with R. The ethanol-water solvent does not change the main composition of the LuAG precursors, but has great influence on the morphology of the final LuAG nano particles. Uniformly dispersed LuAG powders calcined at 1200 °C for 3 h with a particle size of approximately 120 nm were obtained by using ethanol-water solvent with proper R = 1. The mechanism of ethanol in the preparation process was discussed.

  11. Oxalate co-precipitation synthesis of calcium zirconate and calcium titanate powders.

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez-Sanchez, Bernadette A.; Tuttle, Bruce Andrew


    Fine powders of calcium zirconate (CaZrO{sub 3}, CZ) and calcium titanate (CaTiO{sub 3}, CT) were synthesized using a nonaqueous oxalate co-precipitation route from Ca(NO{sub 3}){sub 2}{center_dot}4 H{sub 2}O and group(IV) n-butoxides (Ti(OBu{sup n}){sub 4} or Zr(OBu{sup n}){sub 4}). Several reaction conditions and batch sizes (2-35 g) were explored to determine their influence on final particle size, morphology, and phase. Characterization of the as-prepared oxalate precursors, oven dried oxalate precursors (60-90 C), and calcined powders (635-900 C) were analyzed with TGA/DTA, XRD, TEM, and SEM. Densification and sintering studies on pressed CZ pellets at 1375 and 1400 C were also performed. Through the developed oxalate co-precipitation route, densification temperatures for CZ were lowered by 125 C from the 1500 C firing temperature required for conventional mixed oxide powders. Low field electrical tests of the CZ pellets indicated excellent dielectric properties with dielectric constants of {approx}30 and a dissipation factor of 0.0004 were measured at 1 kHz.

  12. Effect of Limestone Powder on Acid Attack Characteristics of Cement Pastes

    Directory of Open Access Journals (Sweden)

    Shuhua LIU


    Full Text Available The acid resistance of cement pastes containing limestone powder with two different water-binder (w/b ratios exposed to acetic (pH = 4 and sulfuric acid (pH = 2 solutions respectively were investigated in this paper. Limestone powder, fly ash and silica fume were also added to the cement paste mixture at different proportions. Static and flowing aqueous environments were set in this experiment. Strength and microstructure of the pastes after acid attack were investigated by using strength test, X-ray diffractometer (XRD and scanning electron microscopy (SEM. The experimental results show that the erosion degree depends not only on pH value of the solution and w/b ratio of the pastes, but also on the content of limestone powder. Acetic acid reacts with calcium hydroxide and carbonate thus dissolving the pastes, while sulfuric acid consumed calcium hydroxide, and generated gypsum and ettringite. The consumption of calcium hydroxide in the flowing solution group is higher than that in the static solution because the flowing sulfuric acid solution has negative effect upon the gypsum crystallization. Fly ash and silica fume are beneficial to limestone cement paste because of the less calcium hydroxide formation, which is among the hydrates vulnerable to acid erosion. DOI:

  13. Physicochemical and antibacterial characterization of ionocity Ag/Cu powder nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Nowak, A., E-mail: [A. Chełkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1A, 41-500 Chorzów (Poland); Szade, J. [A. Chełkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1A, 41-500 Chorzów (Poland); Talik, E. [A. Chełkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Zubko, M. [Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1A, 41-500 Chorzów (Poland); Institute of Material Science, University of Silesia, 75 Pułku Piechoty 1a, 41-500 Chórzow (Poland); Wasilkowski, D. [Department of Biochemistry, University of Silesia, Jagiellońska 28, 40-032 Katowice (Poland); Dulski, M. [Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1A, 41-500 Chorzów (Poland); Institute of Material Science, University of Silesia, 75 Pułku Piechoty 1a, 41-500 Chórzow (Poland); Balin, K. [A. Chełkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1A, 41-500 Chorzów (Poland); and others


    Metal ion in bimetallic nanoparticles has shown vast potential in a variety of applications. In this paper we show the results of physical and chemical investigations of powder Ag/Cu nanoparticles obtained by chemical synthesis. Transmission electron microscopy (TEM) experiment indicated the presence of bimetallic nanoparticles in the agglomerated form. The average size of silver and copper nanoparticles is 17.1(4) nm (Ag) and 28.9(2) nm (Cu) basing on the X-ray diffraction (XRD) data. X-ray photoelectron (XPS) and Raman spectroscopies revealed the existence of metallic silver and copper as well as Cu{sub 2}O and CuO being a part of the nanoparticles. Moreover, UV–Vis spectroscopy showed surface alloy of Ag and Cu while Time of Flight Secondary Ion Mass Spectroscopy (ToF-SIMS) and Energy Dispersive X-ray Spectroscopy (EDX) showed heterogeneously distributed Ag structures placed on spherical Cu nanoparticles. The tests of antibacterial activity show promising killing/inhibiting growth behaviour for Gram positive and Gram negative bacteria. - Highlights: • Ag/Cu nanoparticles were obtained in the powder form. • The average size of nanoparticles is 17.1(4) nm (Ag) and 28.9(2) nm (Cu). • Ag/Cu powder nanoparticle shows promising antibacterial properties.

  14. Application of SnO2 Nano-powder on MEMS Type Gas Sensors

    Directory of Open Access Journals (Sweden)

    E. Abbaspour-Sani


    Full Text Available This paper describes a cost effective and new method for preparing SnO2 sol-gel as the basic material for the Micro-Electro-Mechanical System (MEMS type gas sensors. The SnO2 sol-gel was prepared by mixing SnCl4, propanol and isopropanol in a specified ratio. The produced sol-gel was exposed to two different decomposition temperatures of 600°C and 1200°C. Thermal treatment of the sol-gel resulted in formation of nano-crystalline single phase SnO2 powder having two different grain sizes. The grain size of the nano-powder calcinated at 600°C was about 10 nm and increased to about 80nm when the treatment temperature increased to 1200°C. The samples analyzed by XRD and TEM methods and both confirmed the grain size dependency on temperature. The prepared SnO2 sol-gels were applied on alumina substrates and the prepared samples were tested for sensitivity and selectivity using hydrogen, air and natural gas. The measurement results indicate a decrease in both selectivity and sensitivity of the gas sensor for increased nano-powder grain size.

  15. Hydrothermal synthesis of fine oxide powders

    Indian Academy of Sciences (India)

    The authors describe. hydrothermal decomposition,; hydrothermal metal oxidation,; hydrothermal reaction,; hydrothermal precipitation and hydrothermal hydrolysis,; hydrothermal electrochemical,; reactive electrode submerged arc,; hydrothermal microwave,; hydrothermal sonochemical,. etc and also ideal and real powders ...

  16. 30 CFR 56.6901 - Black powder. (United States)


    ...) Containers of black powder shall be— (1) Nonsparking; (2) Kept in a totally enclosed cargo space while being transported by a vehicle; (3) Securely closed at all times when— (i) Within 50 feet of any magazine or open...

  17. Toxicology evaluation of selenium protein powder

    Directory of Open Access Journals (Sweden)

    Qin Shunyi


    Full Text Available The experiment was conducted to evaluate the safety of selenium protein powder, a novel organic selenium nutritional supplement, and reported corresponding data and results based on a series of toxicological tests. It was examined to evaluate oral acute toxicity by median lethal dose test and mutagenic potential by bone marrow cell micronucleus test and sperm abnormality test using Kun-Ming mice. The results showed that the oral LD50 of selenium protein powder exceeded 31.25 g/kg body weight in mice. No mutagenicity was found by mouse bone marrow cell micronucleus test and mouse sperm abnormality test. The results suggested greater safety of selenium protein powder as a nutritional selenium supplement, and selenium protein powder has the potential for development and application in food systems or functional foods.

  18. Surface chemistry and microscopy of food powders (United States)

    Burgain, Jennifer; Petit, Jeremy; Scher, Joël; Rasch, Ron; Bhandari, Bhesh; Gaiani, Claire


    Despite high industrial and scientific interest, a comprehensive review of the surface science of food powders is still lacking. There is a real gap between scientific concerns of the field and accessible reviews on the subject. The global description of the surface of food powders by multi-scale microscopy approaches seems to be essential in order to investigate their complexity and take advantage of their high innovation potential. Links between these techniques and the interest to develop a multi-analytical approach to investigate scientific questions dealing with powder functionality are discussed in the second part of the review. Finally, some techniques used in others fields and showing promising possibilities in the food powder domain will be highlighted.

  19. Structural characterization of plasma nitrided interstitial-free steel at different temperatures by SEM, XRD and Rietveld method

    Directory of Open Access Journals (Sweden)

    Ana Paula de Andrade Manfridini


    Full Text Available Plasma nitriding processes are widely used to improve surface properties of several steels and alloys. In this work, the formation of nitrides in the surface of plasma nitrided IF steels as a function of the temperature was investigated. Three cold-rolled IF steel plates were nitrided for 4 h after shot peening at three different temperatures: 450 °C, 475 °C, and 500 °C. The resultant nitrided layers were then characterized by scanning electron microscopy (SEM, X-ray diffraction (XRD, Rietveld method, and hardness measurements. Through SEM images, it was possible to visualize two main sublayers: a compound layer and a diffusion zone. Through XRD, two phases were identified in the compound layer, which were ɛ-Fe2–3N and γ′-Fe4N. The diffusion zone presented a ferritic matrix with fine precipitates, possibly α″-Fe16N2. By Rietveld, the calculated quantity of γ′-Fe4N was 68 wt.% for the sample treated at 475 °C and 58 wt.% for the one treated at 500 °C. These values were consistent with the hardness measurements. Thus, it is suggested that higher nitriding temperatures facilitate the decreasing of γ′-Fe4N and, consequently, the increasing of ɛ-Fe2–3N in the compound layer.

  20. [Use of powder metallurgy for development of implants of Co-Cr-Mo alloy powder]. (United States)

    Dabrowski, J R


    This paper discusses the application of powder metallurgy for the development of porous implantation materials. Powders obtained from Co-Cr-Mo alloy with different carbon content by water spraying and grinding, have been investigated. Cold pressing and rotary re-pressing methods were used for compressing the powder. It was found that the sintered materials obtained from water spraying have the most advantageous properties.

  1. A Comprehensive Review of Black Powder (United States)


    second role is to prevent absorption of water. From high speed cinematography of a single burning grain, it appears that the coating acts as an...graphite film thickness. C. Internal Structure of Black Powder S.E.M. microphotographs of class one black powder were obtained by first cleaving the...ground in the Indiana pilot plant jet-mill. They were burned in air at atmospheric pressure and photographed by cinematography at 2000 frames per

  2. Additive Technologies Based on Composite Powder Nanomaterials (United States)

    Gorynin, I. V.; Oryshchenko, A. S.; Malyshevskii, V. A.; Farmakovskii, B. V.; Kuznetsov, P. A.


    The possibilities of application of promising adaptive technologies of bulk laser deposition and selective laser sintering in machine building with the aim of creation of complex-configuration parts and reconditioning of worn components of various-purpose articles from metallic powder materials are considered. The possibilities of the production chain from making of metallic powders to creation of ready coatings and articles on the base of a single unit are described.

  3. Powder Characterization and Optimization for Additive Manufacturing


    Cordova, Laura; Campos, Mónica; Tinga, Tiedo


    Achieving the optimal quality for Additive Manufactured (AM) parts does not only depend on setting the right process parameters. Material feedstock also plays an important role when aiming for high performance products. The metal AM processes that are most applicable to industry, Powder Bed Fusion and Directed Energy Deposition, use metal powder as raw material. Therefore, controlling the quality and correctly characterizing the particles used in the process is a key step to successfully appl...

  4. Advanced powder metallurgy aluminum alloys and composites (United States)

    Lisagor, W. B.; Stein, B. A.


    The differences between powder and ingot metallurgy processing of aluminum alloys are outlined. The potential payoff in the use of advanced powder metallurgy (PM) aluminum alloys in future transport aircraft is indicated. The national program to bring this technology to commercial fruition and the NASA Langley Research Center role in this program are briefly outlined. Some initial results of research in 2000-series PM alloys and composites that highlight the property improvements possible are given.

  5. Powder metallurgy in aerospace research: A survey (United States)

    Blakeslee, H. W.


    The various techniques by which powders can be produced, as pure metals or as alloys, are discussed; the methods by which these powders can be formed into the final parts are explained as well as further processing that may be necessary to meet specific requirements. The NASA developments are detailed, and references are provided for those who wish to obtain further information characteristic of any methodology.

  6. Structural, electronic and optical properties of monoclinic Na{sub 2}Ti{sub 3}O{sub 7} from density functional theory calculations: A comparison with XRD and optical absorption measurements

    Energy Technology Data Exchange (ETDEWEB)

    Araújo-Filho, Adailton A. [Departamento de Física, Universidade Federal do Ceará, Caixa Postal 6030, 60455-760 Fortaleza, CE (Brazil); Silva, Fábio L.R.; Righi, Ariete [Departamento de Física, Universidade Federal de Minas Gerais, Belo Horizonte, MG 31270-901 (Brazil); Silva, Mauricélio B. da; Silva, Bruno P. [Departamento de Física, Universidade Federal do Ceará, Caixa Postal 6030, 60455-760 Fortaleza, CE (Brazil); Caetano, Ewerton W.S., E-mail: [Instituto Federal de Educação, Ciência e Tecnologia do Ceará, 60040-531 Fortaleza, CE (Brazil); Freire, Valder N. [Departamento de Física, Universidade Federal do Ceará, Caixa Postal 6030, 60455-760 Fortaleza, CE (Brazil)


    Powder samples of bulk monoclinic sodium trititanate Na{sub 2}Ti{sub 3}O{sub 7} were prepared carefully by solid state reaction, and its monoclinic P2{sub 1}/m crystal structure and morphology were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), respectively. Moreover, the sodium trititanate main energy band gap was estimated as E{sub g}=3.51±0.01 eV employing UV–Vis spectroscopy, which is smaller than the measured 3.70 eV energy gap published previously by other authors. Aiming to achieve a better understanding of the experimental data, density functional theory (DFT) computations were performed within the local density and generalized gradient approximations (LDA and GGA, respectively) taking into account dispersion effects through the scheme of Tkatchenko and Scheffler (GGA+TS). Optimal lattice parameters, with deviations relative to measurements Δa=−0.06 Å, Δb=0.02 Å, and Δc=−0.09 Å, were obtained at the GGA level, which was then used to simulate the sodium trititanate electronic and optical properties. Indirect band transitions have led to a theoretical gap energy value of about 3.25 eV. Our results, however, differ from pioneer DFT results with respect to the specific Brillouin zone vectors for which the indirect transition with smallest energy value occurs. Effective masses for electrons and holes were also estimated along a set of directions in reciprocal space. Lastly, our calculations revealed a relatively large degree of optical isotropy for the Na{sub 2}Ti{sub 3}O{sub 7} optical absorption and complex dielectric function. - Graphical abstract: Monoclinic sodium trititanate Na2Ti3O7 was characterized by experiment and dispersion-corrected DFT calculations. An indirect gap of 3.5 eV is predicted, with heavy electrons and anisotropic holes ruling its conductivity. - Highlights: • Monoclinic Na2Ti3O7 was characterized by experiment (XRD, SEM, UV–Vis spectroscopy). • DFT GGA+TS optimized geometry and

  7. La2O3 Nano powders by mixture of fuels approach through chemical combustion for dielectric studies (United States)

    Nithesh Sharma, G.; Venkateswara Rao, K.; Sesha Sai Kumar, V.; Shilpa Chakra, Ch; Rajendar, V.; Ranjith Reddy, P.


    La2O3 which is considered as a promising substitute for present SiO2 Gate oxide material in CMOS devices has been synthesized by mixture of fuel method . The method involves the mixing of the Lanthanum Nitrate with, mixture 1:1 of Urea and Glycine. The fuel to oxidizer ratio (Ψ) has been maintained as 1.25. The powders were studied by several physical characterization techniques such as X-ray diffraction (XRD), Thermo gravimetric analysis (TGA) and Differential Thermal analysis (DTA) and dielectric properties have been studied using LCR meter. Surface morphology has been studied by SEM. Particle size has been analysed using Particle analyzer.


    Directory of Open Access Journals (Sweden)

    Mustafa Tuncer


    Full Text Available Alumina – 20 vol% zirconia (ZTA nanocomposites were synthesized by the tartaric acid sol-gel method. The precursors gelled from solutions at different pH were prepared and then calcined from 1000 to 1500°C. Surface area measurement (BET, X-ray diffraction (XRD, scanning electron microscopy (SEM and transmission electron microscopy (TEM were used to characterize the synthesized powders. Control of agglomeration state was carried out by changing the pH of the solution. Weakly agglomerated powders were obtained at pH=6, whereas the solution at pH=1 revealed hard agglomerated powders, (agglomeration degrees, N, were found to be 16425 at pH=1 and 102 at pH=6, respectively. The pH dependence of agglomeration was explained by the dissociation behavior of tartaric acid at various pH environments. XRD results showed that the powders have been fully tetragonal phase at 1000°C, while they exhibited tetragonal zirconia with minor monoclinic phase as well as a-Al2O3 at 1500°C. The presence of a-Al2O3 in the nanocrystalline composite contributes the wide range of temperature stability for t-ZrO2 up to 1500°C. TEM micrograph confirmed that alumina and zirconia were dispersed homogenously. Mechanical properties (hardness and indentation fracture toughness of sintered samples were also determined.

  9. Plasma spheroidization of nickel powders in a plasma reactor

    Indian Academy of Sciences (India)

    The technique involves injection of the powder into a plasma flame, melting, acceleration of the powder particles, impact and bonding with the substrate. Feedstock powders of metals, alloys and ceramics for thermal spray applications have to meet several requirements. Particle shape, size and its distribution, powder flow ...

  10. Plant Mediated Synthesis of Silver Nanoparticles by Using Dried Stem Powder of Tinospora Crispa, And Study of Its Photoluminiscence Activity

    Directory of Open Access Journals (Sweden)



    Full Text Available The Tinospora Crispa is an important medicinal plant to synthesize silver Nanoparticles provides environmentally benign and a feasible alternative to the most of the chemical, physical and biological methods. Utilizing the reduced property of Tinospora Crispa dried stem powder from 1mM aqueous silver nitrate, the average size of 40nm silver nanoparticles were synthesized at room temperature. The stem powder extracts mixed with silver nitrate showed a gradual change in the color of the extracts from yellow to dark brown. The formation of silver nanoparticles was confirmed by UV-Visible spectrophotometer, X-Ray diffraction (XRD, Fourier transform infrared (FTIR, Energy dispersive spectroscopy (EDAX and Transmission electron microscopy (TEM. The photoluminescence studies of silver nanoparticles shows that they are efficient fluorescence emitting probes.

  11. Synthesis of (Mo{sub 1-x}-Cr{sub x})Si{sub 2} nanostructured powders via mechanical alloying and following heat treatment

    Energy Technology Data Exchange (ETDEWEB)

    Yazdani-rad, R.; Mirvakili, S.A. [Materials and Energy Research Center, Tehran (Iran, Islamic Republic of); Zakeri, M., E-mail: [Islamic Azad University (Saveh Branch), P.O. Box: 39187/366, Saveh (Iran, Islamic Republic of)


    MoSi{sub 2}-CrSi{sub 2} nanocomposite powder was successfully synthesized by ball milling of Mo, Si and Cr elemental powders. Effects of the Cr content, milling time and annealing temperature were studied. X-ray diffraction (XRD) was used to characterize the milled and annealed powders. The morphological and microstructural evolutions were studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). High temperature polymorph (HTP) of MoSi{sub 2} begins to form after 50 h of milling and completes after 70 h of milling. MoSi{sub 2}-CrSi{sub 2} composite powder was also prepared with a combination of short milling time (50 h) and low temperature annealing (850 {sup o}C). Annealing led to the HTP to low temperature polymorph (LTP) transformation of MoSi{sub 2}. MoSi{sub 2}-CrSi{sub 2} nanocomposite powder with the mean grain size less than 50 nm was obtained at the end of milling. This composite maintained its nanocrystalline nature after annealing. A spherical morphology was procured for 50 h milled powder with 0.25 mole Cr.

  12. Phase, crystal struture and sintering behavior of shock-synthesized Pb(Zr 0.95Ti 0.05)O 3 powders (United States)

    Wang, Junxia; Yang, Shiyuan; Wang, Jin; He, Hongliang; Xiong, Ying; Chen, Feng


    With a cylindrical shock-wave-loading technique, the single perovskite-phase Pb(Zr 0.95Ti 0.05)O 3 powders (PZT 95/5) were synthesized by shock-induced chemical reactions in heterogeneous multi-material powder mixtures of Pb 3O 4, ZrO 2 and TiO 2. The phase and crystal structure of as-synthesized powders were characterized by X-ray diffraction (XRD) and fourier transform infrared (FT-IR) analysis. And the microstructure and electrical properties of PZT 95/5 ceramics prepared with as-synthesized PZT powders at different sintering temperature were analyzed. The results showed that the shock-wave-induced a large quantity of lattice defects and distortion of the crystal structure in the shock-synthesized PZT powders, which could enhance the sintering activity. Thus, the optimal density and electrical properties of PZT ceramics prepared with as-synthesized powders could be obtained at a sintering temperature of 1200-1225 °C for 3 h, significantly lower than the sintering temperature of PZT 95/5 ceramics prepared by conventional solid-state reaction.

  13. Frontal Dynamics of Powder Snow Avalanches (United States)

    Louge, M. Y.; Carroll, C. S.; Turnbull, B.


    We model the dynamics of the head of dilute powder snow avalanches sustained by a massive frontal blow-out, arising as a weakly cohesive snow cover is fluidized by the very pore pressure gradients that the avalanche induces within the snow pack. Such material eruption just behind the front acts as a source of denser fluid thrust into a uniform ambient air flow at high Reynolds number. In such "eruption current", fluidization depth is inversely proportional to a bulk Richardson number representing avalanche height. By excluding situations in which the snow cover is not fluidized up to its free surface, we derive a criterion combining snow pack friction and density indicating which avalanches can produce a sustainable powder cloud. A mass balance involving snow cover and powder cloud sets avalanche height and mean density. By determining which solution of the mass balance is stable, we find that avalanches reach constant growth and acceleration rates for fixed slope and avalanche width. Under these conditions, we calculate the fraction of the fluidized cover that is actually scoured and blown-out into the cloud, and deduce from a momentum balance on the head that the avalanche accelerates at a rate only 14% of the gravitational component along the flow. We also calculate how far a powder cloud travels until its mean density becomes constant. Finally, we show that the dynamics of powder snow avalanches are crucially affected by the rate of change of their width, for example by reaching an apparent steady speed as their channel widens. If such widening is rapid, or if slope inclination vanishes, we calculate where and how powder clouds collapse. Predictions agree well with observations of powder snow avalanches carried out at the Vallee de la Sionne (Switzerland).

  14. Pure insulin highly respirable powders for inhalation. (United States)

    Balducci, Anna Giulia; Cagnani, Stefano; Sonvico, Fabio; Rossi, Alessandra; Barata, Pedro; Colombo, Gaia; Colombo, Paolo; Buttini, Francesca


    The aim of the present research was to investigate the possibility to obtain by spray drying an insulin pulmonary powder respirable and stable at room temperature without the use of excipients. Several insulin spray-dried powders were prepared with or without the addition of excipients (mannitol, bovine serum albumin, aspartic acid) from water dispersions or from acidic aqueous solutions. Each formulation was characterized using laser diffraction, scanning electron microscopy and in vitro aerosol performance with a Turbospin DPI device. Stability was assessed by the quantification of impurities with a molecular mass greater than that of insulin (HMWP) and related proteins (A21+ORP). Insulin powders prepared without excipients from an acid solution showed a shrivelled, raisin-like shape of non-aggregated microparticles and a high respirability (FPF>65%). The optimal result with respect to respirability and stability was reached when the pH of the insulin acetic acid solution to spray dry was adjusted at pH 3.6 with ammonium hydroxide. The median volume diameter of the obtained powder was 4.04 μm, insulin content 95%, emitted dose of 89.5%, MMAD 1.79 μm and fine particle fraction of 83.6%. This powder was stable at room temperature over a period of eighteen months with respect to the content of A21+ORP. As far as the HMWP content was concerned, the powder complied with the specification limits for a period of five months. The insulin acetic powder opens up the possibility of a more effective pulmonary therapy less dependent on refrigerated storage. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Slip casting nano-particle powders for making transparent ceramics (United States)

    Kuntz, Joshua D [Livermore, CA; Soules, Thomas F [Livermore, CA; Landingham, Richard Lee [Livermore, CA; Hollingsworth, Joel P [Oakland, CA


    A method of making a transparent ceramic including the steps of providing nano-ceramic powders in a processed or unprocessed form, mixing the powders with de-ionized water, the step of mixing the powders with de-ionized water producing a slurry, sonifing the slurry to completely wet the powder and suspend the powder in the de-ionized water, separating very fine particles from the slurry, molding the slurry, and curing the slurry to produce the transparent ceramic.

  16. Methods for production of aluminium powders and their application fields

    Energy Technology Data Exchange (ETDEWEB)

    Gopienko, V.G.; Kiselev, V.P.; Zobnina, N.S. (Vsesoyuznyj Nauchno-Issledovatel' skij i Proektnyj Inst. Alyuminievoj, magnievoj i ehlektrodnoj promyshlennosti (USSR))


    Different types of powder products made of alluminium and its alloys (powder, fine powders, granules and pastes) as well as their basic physicochemical properties are briefly characterized. The principle methods for alluminium powder production are outlined: physicochemical methods, the melt spraying by compressed gas being the mostly developed among them, and physico-mechanical ones. Main application spheres for powder productions of aluminium and its alloys are reported in short.

  17. Platinum incorporation in the Na Y zeolite through impregnation method, and characterization by XRD, FTIR and nitrogen adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Araujo, A.S.; Sousa, B.V.; Andrade, A.C.C.; Rodrigues, M.G.F. [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Centro de Ciencias e Tecnologia. Unidade Academica de Engenharia Quimica], e-mail:, e-mail:, e-mail:; Rangel, M.C. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica. Grupo de Estudos em Cinetica e Catalise


    Supported metal catalysts are widely used in petroleum refining, chemical and petroleum industries. These catalysts are important in ammonia synthesis, conversion of hydrocarbons with water vapor to synthesis gas, reforming, hydrocracking, ... Platinum has long been used in cracking, hydrogenation and dehydrogenation processes. The aim of this project is the Na Y zeolitic sample preparation through impregnation for incipient humidity, with 0,5% concentration of platinum, aiming its use as a catalyst in the steam reforming reaction. The characterization techniques used were: X Rays Diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR) and Nitrogen Adsorption (BET Method). From the obtained results through the techniques mentioned previously it is possible to evidence that the platinum impregnation process did not change the Na Y zeolite structure. Through the superficial specific area (BET) it was possible to observe that the platinum impregnation process caused a decrease in the specific area due to the reduction to the accessibility to the micropores of the zeolitic structure. (author)

  18. XPS, FTIR, EDX, and XRD Analysis of Al2O3 Scales Grown on PM2000 Alloy

    Directory of Open Access Journals (Sweden)

    K. Djebaili


    Full Text Available This work is an original example to compare the results obtained after calcination of Al2O3 hydroxides and oxidation of alumino-formers alloys. FTIR and XPS signatures were obtained for various oxidation temperatures and compared with those known from the literature about calcination of Al2O3 precursors. The aim of this work is to evaluate the use of IR spectroscopy and XPS analysis to probe the structural varieties of Al2O3. For this objective, a study of the PM2000 oxidation at various temperatures was conducted by means of XRD, IR spectroscopy, XPS analysis, EDX analysis, and SEM observations. This allowed us to clearly differentiate the transition Al2O3 from the α-Al2O3 and, amongst the transition Al2O3, to differentiate the characteristic of the IR spectrum of γ-δ phases from that of the θ phase.

  19. Determination of stoichiometry from polycrystalline powders of ...

    African Journals Online (AJOL)

    Polycrystalline molybdenum and tungsten (MoSe2, WSe2) diselenides were synthesized at 1323 K for 168 hours in silica tubes sealed secondary vacuum. They were haracterized by diffraction with X-Ray diffraction (XRD), Scanning Electron Microscopy (SEM) and gravimetric analysis show that they are homogeneous and ...

  20. The use of combined synchrotron radiation micro FT-IR and XRD for the characterization of Romanesque wall paintings

    Energy Technology Data Exchange (ETDEWEB)

    Salvado, N.; Buti, S. [Universitat Politecnica de Catalunya, Dpt. d' Enginyeria Quimica, EPSEVG, Vilanova i la Geltru, Barcelona (Spain); Pantos, E.; Bahrami, F. [CCLRC, Daresbury Laboratory, Warrington (United Kingdom); Labrador, A. [LLS, BM16-ESRF, BP 220, Grenoble Cedex (France); Pradell, T. [Universitat Politecnica de Catalunya, Dpt. Fisica i Enginyeria Nuclear, ESAB, Castelldefels, Barcelona (Spain)


    The high analytical sensitivity and high spatial resolution of synchrotron radiation-based techniques, in particular SR-XRD and SR-FT-IR, allows the identification of complex micrometric mixtures of compounds that constitute the different layers of ancient paintings. The reliability of the measurements even with an extremely small amount of sampled material is very high, and this is particularly important when analyzing art works. Furthermore, the micro size (10 x 10{mu}m for FT-IR and 30 to 50 {mu}m squared spot size for XRD) of the beam enables one to obtain detailed compositional profiles from the different chromatic and preparation layers. The sensitivity of the techniques is high enough for the determination of minor and trace compounds, such as reaction and weathering compounds. We report here the identification of pigments in the Romanesque wall paintings found in situ in the church of Saint Eulalia of Unha place in the Aran valley (central Pyrenees). During the first centuries of the second millennium numerous religious buildings were built in Western Europe in the Romanesque style. In particular, a great number of churches were built in the Pyrenees, most of which were decorated with wall paintings. Although only a few of these paintings have survived, they represent one of the most important collections of Romanesque art, both for their quantity and quality. A full identification of the pigments, binder, supports, and reaction and weathering compounds has been obtained. The results obtained, in particular aerinite as a pigment, indicate a clear connection between the paintings found in this Occitanian church and the Catalan Romanesque paintings from the south bound of the Pyrenees. (orig.)

  1. Caracterización de nanocompuestos de poliuretano-urea/montmorillonita por XRD y µ-Raman

    Directory of Open Access Journals (Sweden)

    Alneira Cuéllar Burgos


    Full Text Available En este trabajo se ha utilizado un copolímero de poliuretano urea (PUU y una montmorillonita (MMT modificada para obtener un nanocompuesto. El silicato modificado fue exfoliado en la matriz del PUU mediante el uso de la técnica de intercalación por solución y posteriormente caracterizados por Difracción de Rayos X (XRD y por espectroscopia µ-Raman. A través de la espectroscopía micro-Raman se logró identificar modos característicos tanto de la arcilla modificada como del PUU, siendo los más importantes para la arcilla modificada dos picos más intensos localizados en 2.850 y 2.884 cm-1 correspondientes al modo vibracional de grupo -CH2-. En la mayoría de las arcillas, la banda 800-600 cm-1 corresponde a modos vibracionales Si-O-Si conectados al SiO4 del tetraedro, siendo el modo vibracional de control de la arcilla ubicado alrededor de 707cm-1 y para PUU los modos asociados a las bandas 1.640 y 1.716 cm-1 del grupo carbonilo de la urea y el uretano respectivamente. Para el nanocompuesto se observaron cambios acentuados en la intensidad de los modos vibracionales del grupo éter simétrico y asimétrico (912 cm-1 y 1.200 cm-1, por la incorporación de arcilla en estas fases. Por XRD se determinó que la arcilla modificada presentaba una morfología de exfoliación dentro de una matriz amorfa.


    Directory of Open Access Journals (Sweden)

    V. N. Kovalevskij


    Full Text Available Production of porous powder materials from spherical powders of corrosion-resistant steel 12Х18н10Т with formation at low pressures 120–140 mpa in the mold with the subsequent activated sintering became possible due to increase of duration of process of spattering and formation of condensate particles (Si–C or (Mo–Si on surface.

  3. Development of Rare-Earth Free Mn-Al Permanent Magnet Employing Powder Metallurgy Route (United States)

    Singh, N.; Shyam, R.; Upadhyay, N. K.; Dhar, A.


    Most widely used high-performance permanent magnets are currently based on intermetallics of rare-earths in combination with Fe and Co. Rare-earth elements required for these magnets are getting expensive by the day. Consequently, there is a thrust worldwide to develop economical rare-earth free permanent magnets. It is acknowledged that the phase in Mn-Al alloys possesses magnetic properties without the presence of ferromagnetic elements such as Fe, Co, and Ni. In the present study, we report the synthesis of magnetic phase of Mn54Al46 alloy synthesized using mechanical alloying followed by solutionizing and annealing to obtain the desired magnetic phase. It is well known that Al dissolves partially in Mn matrix hence supersaturated solid solution of Mn54Al46 alloy powder was obtained by mechanical alloying using a planetary high-energy ball mill. For this purpose elemental Mn and Al powders were ball-milled in Argon atmosphere at 400 rpm using stainless steel bowl with ball to powder ratio of 15:1. These mechanically alloyed Mn54Al46 powders were then consolidated using spark plasma sintering at 550°C for 20 min. followed by solution treatment at 1050°C for 5 hrs and then water quenched to retain high temperature phase. Subsequently, the Mn54Al46 samples were annealed in the temperature range 450°C-650°C to obtain the magnetic phase. These samples were characterized by XRD and SEM and the magnetic properties were measured using a vibrating sample magnetometer (VSM). It was observed that the magnetization and coercivity of MnAl magnets exhibited strong dependence on annealing temperature and annealing time.

  4. A preliminary evaluation of volcanic rock powder for application in agriculture as soil a remineralizer

    Energy Technology Data Exchange (ETDEWEB)

    Ramos, Claudete G., E-mail: [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Mestrado em Avaliação de Impactos Ambientais, Victor Barreto, 2288 Centro, 92010-000 Canoas, RS (Brazil); Querol, Xavier [Institute of Environmental Assessment and Water Research (IDÆA-CSIC), C/Luis Solé y Sabarís s/n, 08028 Barcelona (Spain); Oliveira, Marcos L.S. [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Mestrado em Avaliação de Impactos Ambientais, Victor Barreto, 2288 Centro, 92010-000 Canoas, RS (Brazil); Pires, Karen [Departamento Nacional de Produção Mineral (DNPM), Washington Luiz, 815, Centro, 90010-460 Porto Alegre, RS (Brazil); Kautzmann, Rubens M. [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Mestrado em Avaliação de Impactos Ambientais, Victor Barreto, 2288 Centro, 92010-000 Canoas, RS (Brazil); Oliveira, Luis F.S., E-mail: [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Mestrado em Avaliação de Impactos Ambientais, Victor Barreto, 2288 Centro, 92010-000 Canoas, RS (Brazil)


    Mineralogical and geochemical characteristics of volcanic rock residue, from a crushing plant in the Nova Prata Mining District, State of Rio Grande do Sul (RS), Brazil, in this work named rock powder, were investigated in view of its potential application as soil ammendment in agriculture. Abaut 52,400 m{sup 3} of mining waste is generated annually in the city of Nova Prata without a proper disposal. The nutrients potentially available to plants were evaluated through leaching laboratory tests. Nutrient leaching tests were performed in Milli-Q water; citric acid solution 1% and 2% (AC); and oxalic acid solution 1% and 5% (AO). The bulk and leachable contents of 57 elements were determined by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES). Mining waste were made up by CaO, K{sub 2}O, SiO{sub 2}, Al{sub 2}O{sub 3}, Fe{sub 2}O{sub 3}, and P{sub 2}O{sub 5}. The analysis by X-ray diffraction (XRD) showed the major occurence of quartz, anorthite, cristobalite, sanidine, and augite. The water leachable concentrations of all elements studied were lower than 1.0 mg/kg, indicating their low solubility. Leaching tests in acidic media yield larger leachable fractions for all elements being studied are in the leachate of the AO 1%. These date usefulness of volcanic rock powder as potential natural fertilizer in agriculture in the mining district in Nova Prata, Rio Grande do Sul, Brazil to reduce the use of chemical fertilizers. - Highlights: • Volcanic rock powder as fertilizer in agriculture • Volcanic rock powder as a source of nutrients to plants • This technology may favor the use of volcanic rock in agriculture.

  5. Shape memory characteristics and mechanical properties of powder metallurgy processed Ti50Ni40Cu10 alloy. (United States)

    Kim, Yeon-Wook


    Ti-Ni-Cu alloy powders were prepared by gas atomization and porous bulk specimens were fabricated by spark plasma sintering (SPS). The microstructure of as-solidified powders exhibited a cellular structure and they contained a high density of nano-sized porosities which were located in the intercellular regions. XRD analysis showed that one-step martensitic transformation of B2-B19 occurred in all alloy powders and SPS specimens. When the martensitic transformation start temperature (M(s)) and austenite transformation finish temperature (A(f)) were determined in order to analyze the dependence of powder size on transformation temperatures, the M(s) increased slightly from -17.5 degrees C to - 14.6 degrees C as increasing the powder size ranging from between 25 and 50 μm to ranging between 100 and 150 μm. However, the M(s) and A(f) of the as-atomized powders is much smaller than those of SPS specimens and the M(s) of porous specimen was about 10.9 degrees C. Loading-unloading compressive tests were carried out to investigate the mechanical properties of porous Ti-Ni-Cu specimen. The specimen was compressed to the strain of 6% at a temperature higher than A,. After unloading, the residual strain was 2.1%. After the compressed specimen was heated to 60 degrees C and held for 30 minutes and then cooled to room temperature, the changes in the length of the specimens were measured. Then it was found that the recovered strain ascribed to shape memory effect was 1.5%.

  6. Magnetic properties of co-precipitated hexaferrite powders with Sm-Co substitutions optimized with the molten flux method (United States)

    Serletis, C.; Litsardakis, G.; Pavlidou, E.; Efthimiadis, K. G.


    In this work, using the chemical coprecipitation method, Sr1-xSmxFe12-xCoxO19 (x = 0, 0.1, 0.2) hexaferrite powders were prepared. Major magnetization loops were recorded at room temperature in order to determine the correct calcination temperature for optimum hard magnetic properties. It is found that a small degree of substitution increases substantially the coercive field. Also, the use of the molten flux calcination method increases the remanent magnetization. SEM/EDXS and XRD measurements were performed at the calcined powders: the results show that a single hexaferrite phase is formed and that the substituted powders consist of an assembly of grains with a mean diameter of 40 nm. Measurements of minor magnetization loops and of the temperature and time dependence of the magnetization confirm that the powders consist of a non-oriented single domain magnetic particles assembly. The results indicate that Sm could be a viable replacement for La in the manufacturing of hexaferrites with a high-energy product.


    Directory of Open Access Journals (Sweden)

    Seyed Mohsen Latifi


    Full Text Available Ca ion release from bioactive biomaterials could play an important role in their bioactivity and osteoconductivity properties. In order to improve hydroxyapatite (HA dissolution rate, in situ apatite-silica nanocomposite powders with various silica contents were synthesized via sol-gel method and mechanisms controlling the Ca ion release from them were investigated. Obtained powders were characterized by X-ray diffraction (XRD and transmission electron spectroscopy (TEM techniques, acid dissolution test, and spectroscopy by atomic absorption spectrometer (AAS. Results indicated the possible incorporation of (SiO44- into the HA structure and tendency of amorphous silica to cover the surface of HA particles. However, 20 wt. % silica was the lowest amount that fully covered HA particles. All of the nanocomposite powders showed more Ca ion release compared with pure HA, and HA - 10 wt. % silica had the highest Ca ion release. The crystallinity, the crystallite size, and the content of HA, along with the integrity, thickness, and ion diffusion possibility through the amorphous silica layer on the surface of HA, were factors that varied due to changes in the silica content and were affected the Ca ion release from nanocomposite powders.

  8. Effect of Ultrasonication Dispersion Technique on Sintering Properties of CNT Reinforced Al-Zn-Mg-Cu Powder

    Directory of Open Access Journals (Sweden)

    Rudianto H.


    Full Text Available CNT has been researched significantly due to its properties especially mechanical and conductivity properties. Due to strong affinity between particles, dispersion has been remained a problem for its applications. Ultrasonication technique was used to disperse CNT on aluminum powder. Ultrasonication has successfully dispersed CNT on aluminum powder in ethanol. Low energy ball milling for 1h under argon gas with 5:1 ball to powder ratio was used to optimize dispersion of CNT on aluminum. CNT concentration in this research is ranged from 0.1 up to 3wt%. Premix Al-5.5Zn-2.5Mg-0.5Cu powder was used as matrix for this research. Sintering at 580°C for 1h under argon gas was carried to produce high density materials. Pores are still remained on material and it is possibility that pores were caused by agglomeration of CNT. Dispersion high content of CNT is still remained obstacle on this research. Aluminum carbide, Al4C3 is recognized as a ‘bridge between aluminum and CNT for stress transfer was investigated in this research. Raman Spectroscopy, XRD and SEM-EDS were carried out to characterize materials.

  9. Influence of Milling Time on the Crystallite Size of AlSi5Cu2/SiC Composite Powder

    Directory of Open Access Journals (Sweden)

    Suśniak M.


    Full Text Available AlSi5Cu2/SiC nanocrystalline composite powder was successfully obtained by mechanical alloying of AlSi5Cu2 chips with reinforcement of 0, 10, 15, 20 wt. % of silicon carbide. X-ray powder diffraction was used to characterize obtained material. Detailed analyses using transmission and scanning electron microscopy have been conducted in order to collaborate the grain size measurement determined from the XRD analyses. Powders produced in a planetary ball mill with milling time: 1, 5, 10, 15, 20 and 40 hours, have shown shape and size evaluation during mechanical alloying process. It can be seen tendency to decrease the size of the grain as the milling time is increased. It is also noted that the grains of composites (AlSi5Cu2/SiC are smaller than samples prepares without SiC addition. 40 hours of milling lead to formed very small grains of Al phase (20 nm in average in composite powder.

  10. Inhaled dry powder formulations for treating tuberculosis. (United States)

    Das, Shyamal; Tucker, Ian; Stewart, Peter


    Tuberculosis is the second leading cause of death from infectious diseases. Although antitubercular drugs have been traditionally administered orally, there is a growing interest in delivering drugs via the pulmonary route using nebulisers or dry powder inhalers. Drugs in dry powder inhalers (DPI) are stable and DPI are user-friendly compared to nebulisation which is time consuming, inconvenient and inefficient and requires special equipment. For tuberculosis treatment, drugs should target alveolar macrophages that harbour microorganisms and/or maintain high drug concentration at the infection site in the lung. Drug particles include micro-particles or nanoparticles. Powders can be engineered by micronisation, crystallisation, spray drying, freeze drying and particle coating approaches. The formulation may contain single or combination drugs. This paper will provide an update on current status of TB, its pathogenesis, current treatment strategies, shortcomings of current oral or parenteral delivery strategies, pulmonary delivery devices, advantages of pulmonary delivery of powder formulations, formulation approaches and pharmacokinetic studies of pulmonary delivery of powders for inhalation.

  11. Laser powder microdeposition of CP2 Titanium

    Energy Technology Data Exchange (ETDEWEB)

    Meacock, C. [Departamento de Engenharia de Materiais, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal)], E-mail:; Vilar, R. [Departamento de Engenharia de Materiais, Instituto Superior Tecnico, Av. Rovisco Pais, 1049-001 Lisboa (Portugal)


    Laser powder microdeposition (LPMD) uses a finely focused laser beam to generate a minute meltpool on the surface of a metallic substrate into which metallic powder is blown. The laser/powder interaction zone is scanned over the substrate and molten material re-solidifies leaving microscale tracks of deposited material. The ability to deposit material on this scale opens up the possibilities of the alteration of the surface properties of small metallic components, the repair of fine damage such as fractures and wear and the fabrication of small components that require high dimensional accuracy such as dental and maxillofacial implants. In this paper, a novel Laser powder microdeposition system is described whereby the powder is fed via a fine capillary. The system was used to deposit single tracks, thin walls and a solid part of grade 2 commercially pure (CP2) Titanium, a material suitable for the fabrication of dental implants. The geometry of both single tracks and thin walls of CP2 Titanium deposited by LPMD can be controlled by variation of laser power and scanning speed. The process can be used to produce porosity free thin wall structures with widths lower than 450 {mu}m and with a surface roughness lower than 20 {mu}m (Ra)

  12. Cosmetic powder suspensions in compliant, fingerprintlike contacts. (United States)

    Timm, K; Myant, C; Spikes, H A; Schneider, M; Ladnorg, T; Grunze, M


    Cosmetic powders are regularly employed in skin creams and cosmetic formulations to improve performance and enhance skin feel. A previous study investigated the effect of particle concentration and size on the lubricating properties of powder suspensions in smooth, compliant contacts [Timm et al., Tribol. Int. (2011)]. In this paper the tribological properties of cosmetic powder suspensions are investigated in compliant contacts having model fingerprintlike surface topography. Friction coefficients were measured for a series of powder suspensions with varying particle size and concentration in a polydimethylsiloxane (PDMS)/PDMS contact. A commercial tribometer (MTM, PCS Instruments) was employed to measure friction as a function of rubbing time (20 min), under pure sliding (50 mm/s) and low load (0.5 N) conditions. Compared to results using smooth surfaces, it was clear that surface topography has a pronounced affect on the time-dependent tribological behavior of the cosmetic powder suspensions studied. A two-stage friction coefficient versus time curve was observed. By varying the particle size and concentration it was shown that the duration and magnitude of each stage can be controlled.

  13. Polymer powders for selective laser sintering (SLS) (United States)

    Schmid, Manfred; Amado, Antonio; Wegener, Konrad


    Selective Laser Sintering (SLS) is close to be accepted as a production technique (Additive Manufacturing). However, one problem limiting employment of SLS for additive manufacturing in a wide-ranging industrial scope is the narrow variety of applicable polymers. The commonly applied SLS powder to date is polyamide 12 (PA 12). PA 12 or ccompounds of PA 12 (dry blends) are approximately 90 % of complete industrial consumption. The remaining small quantity is distributed on polyamide 11 (PA11) and some other `exotic' polymers (TPU, PEBA, P(E)EK). Industry is awaiting commodity polymers like polypropylene (PP) or polyethylene (PE) crucial to open new market segments. But several approaches launching those polymers failed. But what are the reasons for the difficulties in developing new SLS powders? The contribution is to answer this and highlights the combination of intrinsic and extrinsic polymer properties necessary to generate a polymer powder promising for SLS application. Particle shape, powder distribution, thermal, rheological and optical requirements must be considered and only a particularly controlled property combination leads to successful SLS implementation. Thermal behavior, particle shape and -distribution is discussed in detail, although the other properties can't be disregarded for providing new commercially successful SLS powder finally.

  14. Formulation Design of Dry Powders for Inhalation. (United States)

    Weers, Jeffry G; Miller, Danforth P


    Drugs for inhalation are no longer exclusively highly crystalline small molecules. They may also be amorphous small molecules, peptides, antibodies, and myriad types of engineered proteins. The evolution of respiratory therapeutics has created a need for flexible formulation technologies to engineer respirable particles. These technologies have enabled medicinal chemists to focus on molecular design without concern regarding compatibility of physicochemical properties with traditional, blend-based technologies. Therapeutics with diverse physicochemical properties can now be formulated as stable and respirable dry powders. Particle engineering technologies have also driven the deployment of new excipients, giving formulators greater control over particle and powder properties. This plays a key role in enabling efficient delivery of drugs to the lungs. Engineered powder and device combinations enable aerosols that largely bypass the mouth and throat, minimizing the inherent variability among patients that arises from differences in oropharyngeal and airway anatomies and in breathing profiles. This review explores how advances among molecules, particles, and powders have transformed inhaled drug product development. Ultimately, this scientific progress will benefit patients, enabling new classes of therapeutics to be formulated as dry powder aerosols with improved efficacy, reduced variability and side effects, and improved patient adherence. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

  15. The Characterization of the Desulfurization Powder in the Semi-Dry DE-SO2 Process of the Sintering Plant Exhaust Gas and its Interaction with the Soil Particles (United States)

    Kang, Ling-Chen; Lu, Li-jun; Xue, Gai-feng; Hwang, Jiann-Yang

    The desulfurization (de-SO2) powders are a solid waste obtained from the sintering plants of the iron and steel industries. It is mostly landfilled due to its massive quanti ties and complicate compositions. A new utilization was developed in this study as a de-soil reagent for the treatment of tailings in the open-pit mines. In this paper, the de-SO2 powders were collected from a sintering plant using the semi-dry de-SO2 process. The chemical compositions of the de-SO2 powders were analyzed by titrations and the chemical phases were determined with a X-ray diffractometer (XRD). The size distribution was measured by a laser particle size analyzer. The micro-morphology was observed by a scanning electron microscopy (SEM). Furthermore, the interaction between the de-SO2 powder and the soil particle was studied.

  16. Low temperature synthesis of nanocrystalline lanthanum monoaluminate powders by chemical coprecipitation

    Energy Technology Data Exchange (ETDEWEB)

    Kuo, C.-L. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, C.-L. [Department of Materials Science and Engineering, I-Shou University, 1 Section 1, Hsueh-Cheng Road, Ta-Hsu Hsiang, Kaohsiung 840, Taiwan (China); Chen, T.-Y. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Chen, G.-J. [Department of Materials Science and Engineering, I-Shou University, 1 Section 1, Hsueh-Cheng Road, Ta-Hsu Hsiang, Kaohsiung 840, Taiwan (China); Hung, I-M. [Department of Chemical Engineering and Materials Science, Yuan Ze University, 135 Yuan-Tung Road, Chungli, Taoyuan 320, Taiwan (China); Shih, C.-J. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China)]. E-mail:; Fung, K.-Z. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China)


    Nanocrystalline lanthanum monoaluminate (LaAlO{sub 3}) powders were prepared by chemical coprecipitation using 25 vol.% of NH{sub 4}OH, 0.05 M La(NO{sub 3}){sub 3}.6H{sub 2}O and 0.05 M Al(NO{sub 3}){sub 3}.9H{sub 2}O aqueous solutions as the starting materials. Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analyses (TGA/DTA), X-ray diffraction (XRD), Raman spectrometry, specific surface area (BET) analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED) were utilized to characterize the LaAlO{sub 3} powders prepared by chemical coprecipitation. The crystallization temperature of the LaAlO{sub 3} precursor gels precipitated at pH 9 is estimated as 810 deg. C by TG/DTA. The XRD pattern of the LaAlO{sub 3} precursor gels precipitated at pH 8-12 and calcined at 700 deg. C for 6 h shows a broad arciform continuum exist between 24{sup o} and 32{sup o} and sharp peaks of LaAlO{sub 3} except the precursor gels precipitated at pH 9. For the LaAlO{sub 3} precursor gels precipitated at pH 9 and calcined at 700 deg. C for 6 h, the formation of the perovskite LaAlO{sub 3} phase occurs and the presence of crystalline impurities is not found. The crystallite size of LaAlO{sub 3} slightly increases from 37.8 to 41.5 nm with calcination temperature increasing from 700 to 900 deg. C for 6 h. The LaAlO{sub 3} powders prepared by chemical coprecipitation have a considerably large specific surface of 30 m{sup 2}/g. The relative density greater than 97% is obtained when these nanocrystalline LaAlO{sub 3} powders are sintered at 1550 deg. C for 2 h.

  17. Synthesis of yttria powders by electrospray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Rulison, A.J.; Flagan, R.C. (California Inst. of Technology, Pasadena, CA (United States))


    Electrospray atomization of high-concentration ([approximately]400 g/L) chemical precursor solutions was applied to the synthesis of yttria powders. Conditions were found which led to high-quality powders, composed of dense, spheroidal, submicrometer, and nanocrystalline oxide particles. The precursor solutions were hydrated yttrium nitrates dissolved in n-propyl alcohol at concentrations ranging from 44.1 to 455 g/L. Electrospray atomization produced submicrometer precursor droplets which were dispersed in air and carried through an electric furnace for thermal decomposition at 500 C for several seconds residence time. X-ray powder diffraction patterns indicated the expected cubic phase. Transmission electron micrographs showed that the particle structure varied with solution composition, ranging from hollow, inflated spheres for 6-hydrated nitrates to dense spheroids for 5-hydrated nitrates. The use of 6-hydrated nitrates in the solutions appeared to form particle surfaces which were impermeable to alcohol vapor evolved during thermal decomposition, leading to hollow, inflated spheres.

  18. Red man syndrome caused by vancomycin powder. (United States)

    Nagahama, Yasunori; VanBeek, Marta J; Greenlee, Jeremy D W


    Red man syndrome (RMS) is a well-known hypersensitivity reaction caused by intravenous administration of vancomycin, with symptoms ranging from flushing, erythematous rash, pruritus, mild to profound hypotension, and even cardiac arrest. RMS has not previously been described from local application of vancomycin powder in a surgical wound, a technique increasingly utilized for infection prophylaxis in many surgical disciplines including neurosurgery. We describe the first reported case of RMS as a result of local intra-wound application of vancomycin powder for infection prophylaxis. A 73-year-old male with a history of Parkinson's disease underwent 2-stage deep brain stimulation implantation surgeries. Vancomycin powder was applied locally in the surgical wounds for infection prophylaxis during both of the surgeries. The patient developed a well-demarcated, geometric erythematous pruritic rash following the second surgery that was clinically diagnosed as RMS and resolved without sequelae. Copyright © 2018 Elsevier Ltd. All rights reserved.

  19. Recent analytical developments for powder characterization (United States)

    Brackx, E.; Pages, S.; Dugne, O.; Podor, R.


    Powders and divided solid materials are widely represented as finished or intermediary products in industries as widely varied as foodstuffs, cosmetics, construction, pharmaceuticals, electronic transmission, and energy. Their optimal use requires a mastery of the transformation process based on knowledge of the different phenomena concerned (sintering, chemical reactivity, purity, etc.). Their modelling and understanding need a prior acquisition of sets of data and characteristics which are more or less challenging to obtain. The goal of this study is to present the use of different physico-chemical characterization techniques adapted to uranium-containing powders analyzed either in a raw state or after a specific preparation (ionic polishing). The new developments touched on concern dimensional characterization techniques for grains and pores by image analysis, chemical surface characterization and powder chemical reactivity characterization. The examples discussed are from fabrication process materials used in the nuclear fuel cycle.

  20. Hydration of Blended Portland Cements Containing Calcium-Aluminosilicate Glass Powder and Limestone

    DEFF Research Database (Denmark)

    Moesgaard, Mette; Poulsen, S.L.; Herfort, D.


    This work investigates the hydration of blended Portland cement containing 30 wt.% Na2O-CaO-Al2O3-SiO2 (NCAS) glass particles either as the only supplementary cementitious material (SCM) or in combination with limestone, using 29Si MAS NMR, powder XRD, and thermal analyses. The NCAS glass...... represents a potential alternative to traditional SCMs, used for reduction of the CO2 emission associated with cement production. It is found that the NCAS glass takes part in the hydration reactions after about two weeks of hydration and a degree of reaction of approx. 50 % is observed after 90 days...... of hydration. The hydrated glass contributes to the formation of the calcium-silicate-hydrate (C-S-H) phase, consuming a part of the Portlandite (Ca(OH)2) formed during hydration of the Portland cement. Furthermore, the presence of the glass and limestone particles, alone or in combination, results...

  1. In-house characterization of protein powder

    DEFF Research Database (Denmark)

    Hartmann, Christian Grundahl; Harris, Pernille; Ståhl, Kenny


    Collecting protein powder diffraction data on standard in-house powder diffractometers requires careful handling of the samples. Specially designed sample holders combined with optimized collimation were found to be the key factors in improving the data quality and reducing the data collection time....... For safe identification of the crystal form the experimental patterns have to be compared with patterns calculated from known crystal structures. Very good agreement with Protein Data Bank data was obtained after including corrections for background, unit cell parameters, disordered bulk...

  2. Hypolipidemic effects of fenugreek seed powder

    Directory of Open Access Journals (Sweden)

    Abu Saleh M. Moosa, Mamun Ur Rashid, A.Z.S. Asadi, Nazma Ara, M. Mojib Uddin and A. Ferdaus


    Full Text Available Effects of fenugreek (Trigonella foenugraecum Linn on serum lipid profile in hypercholesteremic type 2 diabetic patients were studied. Administration of fenugreek seed powder of 25 gm orally twice daily for 3 weeks and 6 weeks produces significant (P<0.001 reduction of serum total cholesterol, triacylglyceride and LDL-cholesterol in hypercholesteremic group but the change of serum HDL-cholesterol was not significant. On other hand, changes of lipid profile in hypercholesteremic type 2 diabetic patients without fenugreek were not significant (P<0.001. The present study suggests that fenugreek seed powder would be considered as effective agent for lipid lowering purposes.

  3. Desensitizing nano powders to electrostatic discharge ignition

    Energy Technology Data Exchange (ETDEWEB)

    Steelman, Ryan [Texas Tech Univ., Lubbock, TX (United States). Dept. of Mechanical Engineering; Clark, Billy [Texas Tech Univ., Lubbock, TX (United States). Dept. of Mechanical Engineering; Pantoya, Michelle L. [Texas Tech Univ., Lubbock, TX (United States). Dept. of Mechanical Engineering; Heaps, Ronald J. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Daniels, Michael A. [Idaho National Lab. (INL), Idaho Falls, ID (United States)


    Electrostatic discharge (ESD) is a main cause for ignition in powder media ranging from grain silos to fireworks. Nanoscale particles are orders of magnitude more ESD ignition sensitive than their micron scale counterparts. This study shows that at least 13 vol. % carbon nanotubes (CNT) added to nano-aluminum and nano-copper oxide particles (nAl + CuO) eliminates ESD ignition sensitivity. The CNT act as a conduit for electric energy and directs electric charge through the powder to desensitize the reactive mixture to ignition. For nanoparticles, the required CNT concentration for desensitizing ESD ignition acts as a diluent to quench energy propagation.

  4. A mechanistic analysis of bulk powder caking (United States)

    Calvert, G.; Curcic, N.; Ghadiri, M.


    Bulk powder transformations, such as caking, can lead to numerous problems within industry when storing or processing materials. In this paper a new Environmental Caking Rig (ECR) is introduced and has been used to evaluate the caking propensity of a hygroscopic powder as a function of temperature, Relative Humidity (RH), mechanical stress and also when RH is cycled. A linear relationship exists between cake strength and the extent of bulk deformation, here defined by the engineering strain. An empirical model has been used to predict the caking behaviour based on consolidation stress and environmental conditions.

  5. Safety consideration when handling metal powders

    CSIR Research Space (South Africa)

    Benson, JM


    Full Text Available . No compressed air hoses should be used � The dust extraction or venting system must be designed to convey powders at concentrations below their MEC. Eliminate all sources of ignition in powder-handling areas � No smoking or smoking materials, including..., and this gives some perspective on the immensity of the hazard. Aluminium dust particles produced during the diecasting process were collected by a dust extraction system for recycling and were stored in a trap outside the factory. A spark ignited an initial...

  6. In Situ XRD Investigations on Structural Change of P2-Layered Materials during Electrochemical Sodiation/Desodiation

    DEFF Research Database (Denmark)

    Jung, Young Hwa; Johnsen, Rune E.; Christiansen, Ane Sælland


    , the initial layered structure is maintained from 2.0 to 4.0 V vs. Na+/Na during first desodiation. The phase transformation is observed over the 4.0 V, but the original P2 structure is completely restored at the following sodiation process. The relationship between structural and electrochemical properties......; as a result, rich experiences for structural studies of O3-layered compounds have been accumulated over the past decades. For sodium layered oxides, however, P2-layered compounds have been reported for better cyclability and structural stability during electrochemical reactions than O3-structure. Therefore......, systematic studies on P2-layered materials for SIBs are highly required. In this study, we report the structural and electrochemical property of P2-NaxFeyMnyCo1-2yO2 synthesized by simple solid state reaction. The X-ray diffraction pattern of as-synthesized powder is indexed as a hexagonal lattice (P63/mmc...

  7. Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science. (United States)

    Svarcová, Silvie; Kocí, Eva; Bezdicka, Petr; Hradil, David; Hradilová, Janka


    The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions.

  8. Air permeability of powder: a potential tool for Dry Powder Inhaler formulation development. (United States)

    Le, V N P; Robins, E; Flament, M P


    Dry Powder Inhalers have drawn great attention from pharmaceutical scientists in recent years in particular those consisting of low-dose micronized drug particles associated with larger carrier particles and called interactive mixtures. However, there is little understanding of the relation between bulk powder properties such as powder structure and its aerodynamic dispersion performance. The aim of this work was to develop a simple method to measure the air permeability of interactive mixtures used in Dry Powder Inhalers by using Blaine's apparatus--a compendial permeameter and to relate it to the aerodynamic behaviour. The study was done with fluticasone propionate and terbutaline sulphate as drug models that were blended with several lactoses having different particle size distribution thus containing different percentages of fine particle lactose. The quality of the blends was examined by analysing the drug content uniformity. Aerodynamic evaluation of fine particle fraction was obtained using a Twin Stage Impinger. A linear correlation between a bulk property--air permeability of packed powder bed--and the fine particle fraction of drug was observed for the tested drugs. The air permeability reflects the quantity of the free particle fraction in the interparticulate spaces of powder bed that leads to fine particle fraction during fluidization in air flow. A theoretical approach was developed in order to link the air permeability of powder bed and drag force acting on powders during aerosolization process. The permeability technique developed in this study provides a potential tool for screening Dry Powder Inhaler formulations at the development stage. Copyright © 2010 Elsevier B.V. All rights reserved.

  9. Cheese powder as an ingredient in emulsion sausages

    DEFF Research Database (Denmark)

    Chen, Xiang; Ruiz Carrascal, Jorge; Petersen, Mikael Agerlin


    modified their profile of volatile compounds. Blue cheese increased some ketones, alcohols, and esters, while brown cheese brought typical Maillard reaction compounds. Overall, addition of cheese powders to sausages enhanced the intensity of flavour traits. A mixture of hard and blue cheese powder showed...... the highest effect on boosting saltiness, while brown cheese powder showed the strongest umami and meat flavour boosting effect, and sausages with added blue cheese powder showed a more intense aftertaste. Hardness significantly increased due to the addition of blue cheese powder. Addition of cheese powder...

  10. Sintering activation of 316L powder using a liquid phase forming powder

    Directory of Open Access Journals (Sweden)

    Nattaya Tosangthum


    Full Text Available It was found that the addition of a liquid forming powder (up to 6 wt.% of a gas-atomized tin powder to 316L powdercould activate the sintering process. Sintering activation could be observed by an increase of the sintered density and selected mechanical properties. When optimized tin powder content was used, shorter sintering time and lower sintering temperaturecould produce sintered 316L+tin materials with excellent mechanical properties. Electron dispersive spectroscopy analyses across 316L-tin-316L grains indicated that Ni transportation during the sintering process was enhanced by the presence of liquid tin.

  11. In Vitro Bioactivity and Antimicrobial Tuning of Bioactive Glass Nanoparticles Added with Neem (Azadirachta indica) Leaf Powder (United States)

    Prabhu, M.; Ruby Priscilla, S.; Kavitha, K.; Manivasakan, P.; Rajendran, V.; Kulandaivelu, P.


    Silica and phosphate based bioactive glass nanoparticles (58SiO2-33CaO-9P2O5) with doping of neem (Azadirachta indica) leaf powder and silver nanoparticles were prepared and characterised. Bioactive glass nanoparticles were produced using sol-gel technique. In vitro bioactivity of the prepared samples was investigated using simulated body fluid. X-ray diffraction (XRD) pattern of prepared glass particles reveals amorphous phase and spherical morphology with a particle size of less than 50 nm. When compared to neem doped glass, better bioactivity was attained in silver doped glass through formation of hydroxyapatite layer on the surface, which was confirmed through XRD, Fourier transform infrared (FTIR), and scanning electron microscopy (SEM) analysis. However, neem leaf powder doped bioactive glass nanoparticles show good antimicrobial activity against Staphylococcus aureus and Escherichia coli and less bioactivity compared with silver doped glass particles. In addition, the biocompatibility of the prepared nanocomposites reveals better results for neem doped and silver doped glasses at lower concentration. Therefore, neem doped bioactive glass may act as a potent antimicrobial agent for preventing microbial infection in tissue engineering applications. PMID:25276834

  12. Preparation of Cu2ZnSnS4 nano-crystalline powder by mechano-chemical method (United States)

    Alirezazadeh, Farzaneh; Sheibani, Saeed; Rashchi, Fereshteh


    Copper zinc tin sulfide (Cu2ZnSnS4, CZTS) is one of the most promising ceramic materials as an absorber layer in solar cells due to its suitable band gap, high absorption coefficient and non-toxic and environmental friendly constituent elements. In this work, nano-crystalline CZTS powder was synthesized by mechanical milling. Elemental powders of Cu, Zn, Sn and were mixed in atomic ratio of 2:1:1:4 according to the stoichiometry of Cu2ZnSnS4 and then milled in a planetary high energy ball mill under argon atmosphere. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and diffusion reflectance spectroscopy (DRS). XRD results confirm the formation of single-phase CZTS with kesterite structure after 20 h of milling. Also, the mean crystallite size was about 35 nm. SEM results show that after 20 h of milling, the product has a relatively uniform particle size distribution. Optical properties of the product indicate that the band gap of prepared CZTS is 1.6 eV which is near to the optimum value for photovoltaic solar cells showing as a light absorber material in solar energy applications.

  13. Synthesis and characterization of ceramic powders of pure and doped with trivalent erbium barium tungstate; Sintese e caracterizacao de pos ceramicos de tungstato de bario puro e dopado com erbio trivalente

    Energy Technology Data Exchange (ETDEWEB)

    Sousa, R.B. de; Nascimento, V.A. do; Matos, J. M.E. de; Santos, M.R.M.C., E-mail: [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil). Centro de Ciencias da Natureza. Laboratorio Interdisciplinar de Materiais Avancados


    This research proposes the synthesis and characterization of pure and doped with Er{sup 3+} (1 and 2 %) barium tungstate powders prepared by the coprecipitation method. In order to characterize the obtained powders were used X-Ray Diffractometry, Raman Spectroscopy and Fourier Transform Infrared Spectroscopy. According to the standard XRD spectra, the crystals exhibited the presence of tetragonal scheelite structure without the presence of secondary phases. Raman spectra showed the presence of eleven vibrational modes and two modes were observed in the infrared spectra. The synthesized oxides showed good crystallinity and structurally ordered at short and long-range. (author)

  14. SR-XRD and SR-FTIR study of the alteration of silver foils in medieval paintings. (United States)

    Salvadó, Nati; Butí, Salvador; Labrador, Ana; Cinque, Gianfelice; Emerich, Hermann; Pradell, Trinitat


    Altarpieces and polychrome carved wood from the fifteenth century AD usually exhibit golden and silvery areas by the application of a very thin foil of metal. The metal foils were normally protected from the atmosphere by a varnish or resin which maybe either preserved or absent. Moreover, they were glued to the background surface by adhesive substances (egg yolk, drying oil or animal glue). The high proportion of the glueing substances often renders the development of reaction compounds. With time, silver alters blacken or simply disappear completely. In this paper, we study the alterations to metal foils from a selection of fifteenth century artworks showing different glueing agents, organic coatings and several degrees of conservation of the organic coatings and metal leafs. The submillimetric layered structure and the high variability and low amount of most of the compounds present in the different layers, as well as their differing nature (organic and inorganic) make the use of micron-sensitive high-resolution techniques essential for their study. In particular, the high resolution, high brilliance and small footprint renders synchrotron radiation most adequate for their study. SR-XRD was performed to identify the reaction compounds formed in the different layers; μFTIR was used at to identify the silver protecting organic coatings, the metal foil glueing layers and the corresponding reaction compounds. The results obtained suggest that atmospheric corrosion is the dominant mechanism, and therefore that the degree of corrosion of the metal foils is mainly related to the conservation state of the protecting coatings.

  15. Study on the Reactivity of Amino Acid Chemosensor, NPFNP, with Ethanol: Structural Elucidation through Single Crystal XRD and DFT Calculations

    Directory of Open Access Journals (Sweden)

    Beena Varghese


    Full Text Available A novel ethoxy derivative of an amino acid chemosensor, 3-naphthyl-1-phenyl-5-(2ʹ-fluoro-5ʹ-nitrophenyl-2-pyrazoline (NPFNP, has been synthesized and characterized by different spectroscopic methods.  A single crystal of the ethoxy derivative, 3-naphthyl-1-phenyl-5-(2ʹ-ethoxy-5ʹ-nitrophenyl-2-pyrazoline NPENP, has been obtained and characterized.  The structure holds interest as it carries biologically active pyrazoline as a central ring attaching to electron donating and withdrawing substituents. The major motivation for this work was to gain detailed insight into the structural parameters of this compound for investigating the influence of crystal packing and geometrical dimensions on optical properties. Time-dependent DFT calculations have been employed for comparing the XRD data with theoretical parameters. The results show that the DFT method at B3LYP/6-31G level can well reproduce the structure of the title compound.

  16. Surface preparation for XRD residual stress measurements; Preparacao de superficie para medicao de tensoes residuais em soldagem por DRX

    Energy Technology Data Exchange (ETDEWEB)

    Mishchenko, Andrii; Oliveira, Bruno Jose de; Scotti, Americo, E-mail:, E-mail:, E-mail: [Universidade Federal de Uberlandia (UFU), MG (Brazil)


    A characteristic feature of the X Ray Diffraction (XRD) method for stress determination is that measurements occur at a thin surface layer. Steel sheets come with surfaces modified by lamination, cleaning (sandblasting, grinding) and even corrosion, which induce residual stresses or roughness inherent to the material. Therefore, surface preparation prior to the residual stress measurement is essential, although no standard procedure seems to be available. A general recommendation is to remove a thin layer so that only residual stresses related to the welding process will be measured. In this study, the use of portable electrolytic equipment was evaluated for mechanized surface material removal. Chemical compositions of electrolytic solutions and the influence of current on the removed material, removal time and temperature during the process were studied. As a result, a suitable chemical solution for electro etching of low carbon steel was developed and a set of “soft” parameters that allowed the removal of about 300 um in a reasonable time was found. Higher currents reduce the removal time, yet increasing the consumption of the solution and plate temperature (which could adversely alter the microstructure or generate thermal stresses). Furthermore, the influence of these parameters on the operability of the process was demonstrated. (author)

  17. Synthesis and characterization of low-OH-fluor-chlorapatite: A single-crystal XRD and NMR spectroscopic study

    Energy Technology Data Exchange (ETDEWEB)

    McCubbin, Francis M; Mason, Harris E; Park, Hyunsoo; Phillips, Brian L; Parise, John B; Nekvasil, Hanna; Lindsley, Donald H [SBU


    Los-OH apatite of the compositional range Ca{sub 4.99-5.06}(PO{sub 4}){sub 2.98-3.00}F{sub 0.51-0.48}Cl{sub 0.38-0.36}OH{sub 0.14-0.12} was synthesized and characterized structurally by synchrotron-based single-crystal X-ray diffraction (XRD), and multiple nuclear magnetic resonance (NMR) spectroscopic techniques. the average structure is hexagonal with space group P6{sub 3}/m. The presence of scattering in the single-crystal diffraction data set, which is incommensurate within the average hexagonal structure, suggests the presence of localized short-range monoclinic domains. Complex lineshapes in the {sup 31}P and {sup 19}F MAS NMR spectra are also consistent with the presence of an incommensurate phase. No evidence was detected for splitting of the Ca2 site into two distinct sites (as had been previously reported for hexagonal ternary apatities). Structure refinement and {sup 19}F{l_brace}{sup 35}Cl{r_brace} TRAPDOR NMR experiments verified intercolumnal neighboring of F and Cl atoms (inter-column distance of 2.62 {angstrom}) within this low-OH{sup -} apatite suggesting that long-range neighboring of F and Cl within the apatite anion channels is feasible.

  18. Composite uranium carbide targets at TRIUMF: Development and characterization with SEM, XRD, XRF and L-edge densitometry (United States)

    Kunz, Peter; Bricault, Pierre; Dombsky, Marik; Erdmann, Nicole; Hanemaayer, Vicky; Wong, John; Lützenkirchen, Klaus


    The production of radioactive ion beams (RIB) from spallation targets by irradiation with a continuous 500 MeV proton beam, has been routine at TRIUMF for several years. Based on the experience with composite refractory carbide targets a procedure for the fabrication of UC2/C targets was developed. It includes the preparation of UC2 by carbothermal reduction of UO2, the slip-casting of fine-grained UC2/C slurry on graphite foil under inert gas atmosphere and the cutting of composite target discs which are stacked up to a lamellar structure. The thermal properties of such an arrangement are adequate to withstand the high power deposition of an intense, continuous proton beam and also beneficial for the fast release of short-lived radioactive isotopes. Molecular structure, particle size and the impact of sintering of the target discs were investigated via XRD and SEM. Thickness and mass distribution were measured with position-sensitive LIII-edge densitometry. The results confirm that the properties of the UC2/C target material are well suited for RIB production at TRIUMF while there is still room for improvement with regard to uniformity of mass distribution in target disc thickness.

  19. UV exposure and photon degradation of Alq{sub 3} powders

    Energy Technology Data Exchange (ETDEWEB)

    Duvenhage, M.M.; Ntwaeaborwa, O.M. [Department of Physics, University of the Free State, P.O. Box 339, Bloemfontein ZA9300 (South Africa); Swart, H.C., E-mail: [Department of Physics, University of the Free State, P.O. Box 339, Bloemfontein ZA9300 (South Africa)


    Tris-(8-hydroxyquinoline)aluminum (Alq{sub 3}) is a widely used light emitting material. It is also used as an electron transporting layer in organic light emitting devices (OLEDs). Degradation is, however, a major problem in these devices. The device performance is affected by parameters such as air, moisture and light exposure. In this work the effect of photon degradation of Alq{sub 3} in air is investigated. Alq{sub 3} phosphor powder was synthesized using a co-precipitation method and recrystalized in acetone. The structure of the sample was determined by using x-ray diffraction (XRD). The averaging particle size estimated from the broadened XRD peaks using Scherrer's equation was 40{+-}4 nm in diameter. The excitation photoluminescence data that was collected correspond well to the absorption data. To study the photon degradation, the sample was irradiated with an UV lamp for {approx}330h. The emission data was collected and the change in photoluminescence intensity with time was monitored.

  20. Crystal structure of radium sulfate: An X-ray powder diffraction and density functional theory study (United States)

    Matyskin, Artem V.; Ylmen, Rikard; Lagerkvist, Petra; Ramebäck, Henrik; Ekberg, Christian


    Radium-barium sulfate (Ra0.76Ba0.24SO4) powder was examined using X-ray Diffraction (XRD) technique and its crystal structure was optimized using Density Functional Theory (DFT). XRD data show that radium and barium sulfate form a solid solution and that Ra0.76Ba0.24SO4 is orthorhombic and isostructural with pure RaSO4, barite (BaSO4), celestite (SrSO4) and anglesite (PbSO4), crystallizing in the space group Pmna (No. 62). The unit cell parameters of the Ra0.76Ba0.24SO4 crystal have been determined using Rietveld refinement and were extrapolated to unit cell parameters of the pure RaSO4 phase using Vegard's law: a=9.129(8), b=5.538(3), c=7.313(5) Å. DFT geometry optimization was used to derive atomic coordinates and interatomic distances in both Ra0.76Ba0.24SO4 and pure RaSO4. The experimental and DFT geometry optimization results obtained in this work are in good agreement with each other, and furthermore with literature data.

  1. Annealing effect on nano-ZnO powder studied from positron lifetime and optical absorption spectroscopy (United States)

    Dutta, Sreetama; Chattopadhyay, S.; Jana, D.; Banerjee, A.; Manik, S.; Pradhan, S. K.; Sutradhar, Manas; Sarkar, A.


    Mechanical milling and subsequent annealing in air at temperatures between 210 and 1200°C have been carried out on high purity ZnO powder to study the defect generation and recovery in the material. Lowering of average grain size (from 76±1to22±0.5nm) as a result of milling has been estimated from the broadening of x-ray lines. Substantial grain growth in the milled sample occurs above 425°C annealing temperature. Positron annihilation lifetime (PAL) analysis of the samples shows a distinct decrease of the average lifetime of positrons very near the same temperature zone. As indicated from both x-ray diffraction (XRD) and PAL results, high temperature (>700°C) annealed samples have a better crystallinity (or lower defect concentration) than even the nonmilled ZnO. In contrast, the measured optical band gap of the samples (from absorption spectroscopy) does not confirm lowering of defects with high temperature annealing. Thermally generated defects at oxygen sites cause significant modification of the optical absorption; however, they are not efficient traps for positrons. Different thermal stages of generation and recovery of cationic as well as anionic defects in granular ZnO are discussed in the light of XRD, PAL, and optical absorption studies.

  2. About some practical aspects of X-ray diffraction : From powder to thin film

    Energy Technology Data Exchange (ETDEWEB)

    Valvoda, V. [Charles Univ. Prague (Czech Republic). Faculty of Mathematics and Physics


    Structure of thin films can be amorphous, polycrystalline or epitaxial, and the films can be prepared as a single layer films, multilayers or as graded films. A complete structure analysis of thin films by means of X-ray diffraction (XRD) usually needs more than one diffraction geometry to be used. Their principles, advantages and disadvantages will be shortly described, especially with respect to their different sampling depth and different response to orientation of diffracting crystallographic planes. Main differences in structure of thin films with respect to powder samples are given by a singular direction of their growth, by their adhesion to a substrate and often also by a simultaneous bombardment by atomic species during the growth. It means that a thermodynamically unstable atomic structures can be found too. These special features of growth of thin polycrystalline films are reflected in often found strong preferred orientation of grains and in residual stresses conserved in the films. The methods of structure analysis of thin films by XRD will be compared with other techniques which can supply structure images on different scales.

  3. Powder-Metallurgy Process And Product (United States)

    Paris, Henry G.


    Rapid-solidification processing yields alloys with improved properties. Study undertaken to extend favorable property combinations of I/M 2XXX alloys through recently developed technique of rapid-solidification processing using powder metallurgy(P/M). Rapid-solidification processing involves impingement of molten metal stream onto rapidly-spinning chill block or through gas medium using gas atomization technique.

  4. Laboratory Powder Metallurgy Makes Tough Aluminum Sheet (United States)

    Royster, D. M.; Thomas, J. R.; Singleton, O. R.


    Aluminum alloy sheet exhibits high tensile and Kahn tear strengths. Rapid solidification of aluminum alloys in powder form and subsequent consolidation and fabrication processes used to tailor parts made of these alloys to satisfy such specific aerospace design requirements as high strength and toughness.

  5. Progress in Titanium Metal Powder Injection Molding

    Directory of Open Access Journals (Sweden)

    Randall M. German


    Full Text Available Metal powder injection molding is a shaping technology that has achieved solid scientific underpinnings. It is from this science base that recent progress has occurred in titanium powder injection molding. Much of the progress awaited development of the required particles with specific characteristics of particle size, particle shape, and purity. The production of titanium components by injection molding is stabilized by a good understanding of how each process variable impacts density and impurity level. As summarized here, recent research has isolated the four critical success factors in titanium metal powder injection molding (Ti-MIM that must be simultaneously satisfied—density, purity, alloying, and microstructure. The critical role of density and impurities, and the inability to remove impurities with sintering, compels attention to starting Ti-MIM with high quality alloy powders. This article addresses the four critical success factors to rationalize Ti-MIM processing conditions to the requirements for demanding applications in aerospace and medical fields. Based on extensive research, a baseline process is identified and reported here with attention to linking mechanical properties to the four critical success factors.

  6. Progress in Titanium Metal Powder Injection Molding. (United States)

    German, Randall M


    Metal powder injection molding is a shaping technology that has achieved solid scientific underpinnings. It is from this science base that recent progress has occurred in titanium powder injection molding. Much of the progress awaited development of the required particles with specific characteristics of particle size, particle shape, and purity. The production of titanium components by injection molding is stabilized by a good understanding of how each process variable impacts density and impurity level. As summarized here, recent research has isolated the four critical success factors in titanium metal powder injection molding (Ti-MIM) that must be simultaneously satisfied-density, purity, alloying, and microstructure. The critical role of density and impurities, and the inability to remove impurities with sintering, compels attention to starting Ti-MIM with high quality alloy powders. This article addresses the four critical success factors to rationalize Ti-MIM processing conditions to the requirements for demanding applications in aerospace and medical fields. Based on extensive research, a baseline process is identified and reported here with attention to linking mechanical properties to the four critical success factors.

  7. Neutron Powder Diffraction and Constrained Refinement

    DEFF Research Database (Denmark)

    Pawley, G. S.; Mackenzie, Gordon A.; Dietrich, O. W.


    The first use of a new program, EDINP, is reported. This program allows the constrained refinement of molecules in a crystal structure with neutron diffraction powder data. The structures of p-C6F4Br2 and p-C6F4I2 are determined by packing considerations and then refined with EDINP. Refinement...

  8. High-Performance Polyimide Powder Coatings (United States)

    Leahy, Jonathan J.


    Researchers at NASA's Kennedy Space Center have developed advanced powder coatings for longer-lasting, improved corrosion control. The results of preliminary tests of the coatings and their resistance to salt spray corrosion are very encouraging, and commercial partners are sought for further development.

  9. Tomato pomace powder ameliorated cisplatin-induced ...

    African Journals Online (AJOL)

    Tomato (Lycopersicon esculentum) pomace powder (TPP) may be a preventive agent by virtue of its known antioxidant property. The possible protective role of TPP against cisplatin-induced alteration of the microanatomy of rat brain was investigated. Thirty rats were divided equally into five groups: control, propylene glycol ...

  10. Balanced mechanical resonator for powder handling device (United States)

    Sarrazin, Philippe C. (Inventor); Brunner, Will M. (Inventor)


    A system incorporating a balanced mechanical resonator and a method for vibration of a sample composed of granular material to generate motion of a powder sample inside the sample holder for obtaining improved analysis statistics, without imparting vibration to the sample holder support.

  11. Quantification of the compactibility of pharmaceutical powders

    DEFF Research Database (Denmark)

    Sonnergaard, Jørn


    The purpose of this study is to investigate and to quantify the compactibility of pharmaceutical powders by a simple linear relationship between the diametral compressive strength of tablets and the applied compaction pressure. The mechanical strength of the tablets is characterized as the crushing...

  12. Sinterable Powders from Laser Driven Reactions (United States)


    Agency or the U. S. Government. unclassified - S7 CURITY CLASIFPICATION of THI PAGE ,(1in Dato at" ’he laser heated process has been modeled in terms...for Si, Si 3N4 , and SiC are presented below. A comprehensive tabular listing of the individual run conditions and the resultant powder characteristics

  13. 21 CFR 73.1647 - Copper powder. (United States)


    ... 21 Food and Drugs 1 2010-04-01 2010-04-01 false Copper powder. 73.1647 Section 73.1647 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES GENERAL LISTING OF COLOR... use in color additive mixtures for coloring externally applied drugs. (b) Specifications. Copper...

  14. Powder Characterization and Optimization for Additive Manufacturing

    NARCIS (Netherlands)

    Cordova, Laura; Campos, Mónica; Tinga, Tiedo


    Achieving the optimal quality for Additive Manufactured (AM) parts does not only depend on setting the right process parameters. Material feedstock also plays an important role when aiming for high performance products. The metal AM processes that are most applicable to industry, Powder Bed Fusion

  15. Effectiveness of botanical powders against Callosobruchus maculatus

    African Journals Online (AJOL)



    Mar 20, 2013 ... The phytochemical analysis revealed that alkaloids, steroids, glycosides and terpenoids were present in .... Phytochemistry of plant materials. The 5 g of each powdered plant material was weighed using ..... Bruchidae) on stored cowpea. Unpublished M.Sc. Thesis, Ahmadu. Bello University, Zaria, Nigeria ...

  16. Synergy Between Moringa oleifera Seed Powder

    African Journals Online (AJOL)


    with alum for water purification in rural communities. Keywords: Phytochemicals, coagulant ... derivatives are widely used in water treatment (Najm et al.,1998). However, there is a fear that aluminum may induce ..... well as the cost of water treatment (Muyibi & Okuofu, 1995). Blending alum and M. oleifera seed powder in ...


    African Journals Online (AJOL)

    Adeyinka Odunsi

    Ladoke Akintola University of Technology Ogbomoso, to determine the effects of powdered castor oil seed. (Ricinus communis L.Euphorbiaceae) on kidney, liver, spleen of albino rats. The rats were in five groups, which were replicated three (3) times. The castor oil seed was turned to powdery form using pestle and mortal.

  18. Evaluation of powder metallurgy superalloy disk materials (United States)

    Evans, D. J.


    A program was conducted to develop nickel-base superalloy disk material using prealloyed powder metallurgy techniques. The program included fabrication of test specimens and subscale turbine disks from four different prealloyed powders (NASA-TRW-VIA, AF2-1DA, Mar-M-432 and MERL 80). Based on evaluation of these specimens and disks, two alloys (AF2-1DA and Mar-M-432) were selected for scale-up evaluation. Using fabricating experience gained in the subscale turbine disk effort, test specimens and full scale turbine disks were formed from the selected alloys. These specimens and disks were then subjected to a rigorous test program to evaluate their physical properties and determine their suitability for use in advanced performance turbine engines. A major objective of the program was to develop processes which would yield alloy properties that would be repeatable in producing jet engine disks from the same powder metallurgy alloys. The feasibility of manufacturing full scale gas turbine engine disks by thermomechanical processing of pre-alloyed metal powders was demonstrated. AF2-1DA was shown to possess tensile and creep-rupture properties in excess of those of Astroloy, one of the highest temperature capability disk alloys now in production. It was determined that metallographic evaluation after post-HIP elevated temperature exposure should be used to verify the effectiveness of consolidation of hot isostatically pressed billets.


    African Journals Online (AJOL)

    Preferred Customer

    This paper reports the use of powdered activated carbon (PAC) and raw coal fly ash (RFA) in the removal of eosin dye from aqueous ... calculation is hereby reported to know the amount of adsorbent required for efficient removal of eosin dye. EXPERIMENTAL. Dye properties and preparation. Analytical grade eosin dye ...

  20. Evaluating the Johanson theory for titanium powder

    CSIR Research Space (South Africa)

    Chikosha, S


    Full Text Available Direct powder rolling (DPR)/roll compaction has been labelled a complex and sample sensitive process. As such the design of the instrument and the determination of the optimal processing conditions for a given feed are very challenging...


    African Journals Online (AJOL)

    The efficacy of the powder of a natural plant product (Acorus calamus L.) and two synthetic insecticides (i.e. Pirimiphos methyl and Rotenone) was compared in the laboratory for the control Sitophilus oryzea (L), Rhizopertha dominica (F) and Tribolium castaneum (Herbst) in stored wheat grains. Seven concentrations of the ...

  2. [Analysis on the chemical compositions of the volatile oil from ultramicro-powder and common grinding powder of Cinnamomum cassia]. (United States)

    Liu, Li; Liu, Nu-Yun; Liu, Qiang


    To analyse and compare the chemical compositions in the volatile oil from Utramicro-powder and Common Grinding Powder of Cinnamomum. The volatile oil was extracted by steam-stilling and analyzed by GC-MS. The relative content of each component was calculated by area normalization method. 34 and 19 peaks were isolated from Ultramicro-powder and Common Grinding Powder of Cinnamomum respectively. All of them were identified. The chemical components of the volatile oil from Ultramicro-powder and Common Grinding Powder of Cinnamomum are reported, the results here provides scientific proof for the application in external preparation of Cinnamomum.

  3. Particle-based simulations of powder coating in additive manufacturing suggest increase in powder bed roughness with coating speed

    Directory of Open Access Journals (Sweden)

    Parteli Eric J. R.


    Full Text Available We have developed the first particle-based numerical tool to simulate the coating of powder particles in additive manufacturing devices. Our Discrete Element Method considers realistic particle shapes and incorporates attractive interaction (van-der-Waals forces between the particles. From simulations of powder coating using a roller as coating device, we find that the surface roughness of the powder bed scales with the square of coating speed. Moreover, we find that using fine, highly polydisperse powders may lead to larger powder bed roughness, compared to process simulations using coarser powders, due to the formation of agglomerates resulting from cohesive forces.

  4. Coating powdered copper catalyst with yttria sol

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Kuan-Ying [Department of Chemical and Engineering and Materials Science, Yuan Ze University, Chung-Li, Taiwan (China); Fuel Cell Center, Yuan Ze University, Chung-Li, Taiwan (China); Shen, Chia-Chieh, E-mail: [Fuel Cell Center, Yuan Ze University, Chung-Li, Taiwan (China); Department of Mechanical Engineering, Yuan Ze University, Chung-Li, Taiwan (China); Graduate School of Renewable Energy Engineering, Yuan Ze University, Chung-Li, Taiwan (China); Lee, Chi-Yuan; Lee, Shuo-Jen [Fuel Cell Center, Yuan Ze University, Chung-Li, Taiwan (China); Department of Mechanical Engineering, Yuan Ze University, Chung-Li, Taiwan (China); Graduate School of Renewable Energy Engineering, Yuan Ze University, Chung-Li, Taiwan (China); Leu, Chih-Hsing [Energy and Environment Research Laboratories, Industrial Technology Research Institute, Hsinchu, Taiwan (China); Wang, Jung-Hui [Fuel Cell Center, Yuan Ze University, Chung-Li, Taiwan (China); Yeh, Chuin-Tih [Department of Chemical and Engineering and Materials Science, Yuan Ze University, Chung-Li, Taiwan (China); Fuel Cell Center, Yuan Ze University, Chung-Li, Taiwan (China)


    Research highlights: {yields} The neutral Y{sub 2}O{sub 3} sol is an effective binder for coating powders of CuZnAl catalyst. {yields} A particle size ratio of 15 for catalyst to binder is suggested for stable coating. {yields} Sufficient stirring is an important step in the catalyst slurry preparation. - Abstract: A commercial Y{sub 2}O{sub 3} sol was tested as a binder for coating CuZnAl catalyst powder onto microchannels of a stainless steel plate (SSP). Coated plates were used to fabricate microchannel reactors that generate hydrogen via the steam reforming of methanol (SRM). Washcoating slurries were prepared by suspending catalyst powders into the sol. Slurry parameters, such as solid content, binder content, pH value, and stir time, were optimized to achieve a stable catalyst coating and good SRM performance. The expected stable coating could be obtained from neutral (pH 7) Y{sub 2}O{sub 3} slurry that is required for a negligible dissolution of the copper component of the catalyst. The experimental coating stability generally improved with the slurry stir time. Observed improvements were attributed to a dispersion of catalyst powders in the slurry through a two-step mechanism: the mechanical disassembly of agglomerated CuZnAl powders into primary particles, and the repelling of dissembled particles through adsorption of positively charged Y{sub 2}O{sub 3} binders. A reasonable reaction temperature of 280 deg. C was found for 95% conversion of methanol in SRM from the resulted microchannel reactors. A low CO fraction of 0.3% was also found in the hydrogen-rich gas reformed.

  5. Moisture-induced caking of beverage powders. (United States)

    Chávez Montes, Edgar; Santamaría, Nadia Ardila; Gumy, Jean-Claude; Marchal, Philippe


    Beverage powders can exhibit caking during storage due to high temperature and moisture conditions, leading to consumer dissatisfaction. Caking problems can be aggravated by the presence of sensitive ingredients. The caking behaviour of cocoa beverage powders, with varying amounts of a carbohydrate sensitive ingredient, as affected by climate conditions was studied in this work. Sorption isotherms of beverage powders were determined at water activities (a(w) ) ranging from 0.1 to 0.6 in a moisture sorption analyser by gravimetry and fitted to the Brunauer-Emmett-Teller (BET) or the Guggenheim-Anderson-de Boer (GAB) equation. Glass transition temperatures (T(g) ) at several a(w) were analysed by differential scanning calorimetry and fitted to the Gordon-Taylor equation. Deduced T(g) = f(a(w) ) functions helped to identify stability or caking zones. Specific experimental methods, based on the analysis of mechanical properties of powder cakes formed under compression, were used to quantify the degree of caking. Pantry tests complemented this study to put in evidence the visual perception of powder caking with increasing a(w) . The glass transition approach was useful to predict the risks of caking but was limited to products where T(g) can be measured. On the other hand, quantification of the caking degree by analysis of mechanical properties allowed estimation of the extent of degradation for each product. This work demonstrated that increasing amounts of a carbohydrate sensitive ingredient in cocoa beverages negatively affected their storage stability. Copyright © 2011 Society of Chemical Industry.

  6. Oxidation behaviour of boron carbide powder

    Energy Technology Data Exchange (ETDEWEB)

    Li, Y.Q. [College of Materials Science and Engineering, Nanjing University of Technology, New Model Road 5, Nanjing, Jiangsu 210009 (China)]. E-mail:; Qiu, T. [College of Materials Science and Engineering, Nanjing University of Technology, New Model Road 5, Nanjing, Jiangsu 210009 (China)


    Isothermal oxidation behaviour of powdered boron carbide (B{sub 4}C) with the fine (1.52 {mu}m), medium (22.5 {mu}m) and coarse (59.6 {mu}m) particle size has been studied in air ranging from 500 to 800 deg. C. The oxidation rate strongly depends on the particle size of boron carbide and temperature. The smaller particle size the higher oxidation rate of B{sub 4}C powder due to its larger surface area. When B{sub 4}C powder is oxidized in air, a B{sub 2}O{sub 3} glass film is formed on the surface of B{sub 4}C grain which retards the further oxidation reaction. The oxidation kinetics is approximately fitted to the diffusion-controlled rate law which can be described by the Jander's equation. The apparent activation energy for the fine-, medium- and coarse-B{sub 4}C powders is 209.4 {+-} 11.4, 212.7 {+-} 35.8 and 219.2 {+-} 45.3 kJ mol{sup -1}, respectively, slightly varying with the impurity content of B{sub 4}C powders. The type of rate law suggests that the diffusion of oxygen through the oxide layer is the rate-limiting step in the oxidation reactions. In addition, the change in the oxidation process at higher oxidation fraction might associate with the B{sub 2}O{sub 3} volatilization at higher temperatures.

  7. Powder metallurgy of turbine disc alloys

    Energy Technology Data Exchange (ETDEWEB)

    Ingesten, N.G. (Dep. of Engineering Metals)


    The first part embraced a study of carbide precipitated in IN 100 and astrology powders. The powder was heat treated at temperatures between 950/sup 0/C and 1150/sup 0/C. After aging at 950-1100/sup 0/C the MC-carbides formed during atomization were replaced by M/sub 23/C/sub 6/-carbides. After 1150/sup 0/C treatments the MC carbides were present again. Precipitation comparable with that obtained in HIP:ed specimens was not observed at free particle surfaces. However, powder particles which had agglomerated during atomization often exhibited considerable precipitation at contiguous surfaces. Obviously, contact between the particles must occur if coarse precipitation at particle surfaces is to develop. Reduced PPB-precipitation was obtained by pre-heat- treatment of powder before compaction. It is suggested that the carbon otherwise available for PPB-precipitation forms carbides in the interior of the powder particles. The aim of the second part was to ..gamma..-strengthen a Co-based super-alloy (Co-15Cr-3Mo-5Ti). Here the Ti-addition gives a coherent and ordered ..gamma..-phase Co/sub 3/Ti. However, upon ageing the alloy is unstable in order to increase the stability modifications of the alloy were prepared by: leaving out the Mo-content, adding 10 % Ni and by decreasing the Ti-content to 4.2 %. In addition, the effect of enhanced grain size and of deformation was investigated. Significant reduction of the transformation rate was only obtained by decresing the Ti-content while deformation of the alloy greatly increased the transformation rate.(author).

  8. Effect of Powder Morphologies on the Property of Conductive Silicone Rubber Filled with Carbonyl Nickel Powder (United States)

    Xiao, Weimin; Lei, Yongping; Xia, Zhidong; Chen, Xin; Han, Yu; Nie, Jingkai; Huang, Pei


    Conductive silicone rubbers filled with the spherical, flaky, and chain-spherical carbonyl nickel powder were prepared. The effects of powder morphologies on their electromagnetic and mechanical properties were analyzed. The electromagnetic shielding effectiveness (SE) and tensile strength of the rubbers varies with their powder morphologies: the SE values increase from the spherical and the chain-spherical to the flaky morphology in the frequency range of 100-400 MHz. In the range of 500-1500 MHz, the SE rises from the spherical and the flaky to the chain-spherical morphologies. In addition, the tensile strength increases from the spherical and the flaky to the chain-spherical morphologies. These variations are related to the differences in the conductive network structure and the powder distribution in the rubber.

  9. Effects of dietary supplement of turmeric powder (Curcuma longa ...

    African Journals Online (AJOL)

    Ross 308) to investigate the effects of dietary supplementation with various levels of turmeric powder on blood constituents and antioxidant activity. The chicks were randomly assigned to eight dietary groups, which were given turmeric powder ...

  10. Research on Durability of Recycled Ceramic Powder Concrete (United States)

    Chen, M. C.; Fang, W.; Xu, K. C.; Xie, L.


    Ceramic was ground into powder with 325 mesh and used to prepare for concrete. Basic mechanical properties, carbonation and chloride ion penetration of the concrete tests were conducted. In addition, 6-hour electric fluxes of recycled ceramic powder concrete were measured under loading. The results showed that the age strength of ceramics powder concrete is higher than that of the ordinary concrete and the fly ash concrete. The ceramic powder used as admixture would reduce the strength of concrete under no consideration of its impact factor; under consideration of the impact factor for ceramic powder as admixture, the carbonation resistance of ceramic powder concrete was significantly improved, and the 28 day carbonation depth of the ceramic powder concrete was only 31.5% of ordinary concrete. The anti-chloride-permeability of recycled ceramic powder concrete was excellent.

  11. Physical properties of yoghurt powder produced by spray drying

    National Research Council Canada - National Science Library

    Koç, Banu; Sakin-Yılmazer, Melike; Kaymak-Ertekin, Figen; Balkır, Pınar


    ... (the feed, outlet and inlet air temperatures) for producing yoghurt powder. The resulting yoghurt powder at each condition was subjected to the measurement of physical properties, moisture content, and reconstitution properties...

  12. Phase and morphology evolution of (Na1-xKxNbO3 powders related to calcinations and K2CO3 content

    Directory of Open Access Journals (Sweden)

    Steven J. Milne


    Full Text Available Sodium-potassium niobate ((Na1-xKxNbO3 powders with x = 0.2, 0.4, 0.6 and 0.8 were prepared following the conventional mixed oxide method and characterized by TG-DTA, XRD and SEM techniques.The effects of calcination temperature, dwell time and K2CO3 content on phase formation behavior and morphology of the powders were investigated. The calcination temperature and dwell time were found tohave a pronounced effect on the phase formation of the calcined sodium-potassium niobate powders. It was found that the crystallized phase depended on calcination conditions. The high calcination temperature andlong dwell time clearly favored particle growth and the formation of large and hard agglomerates. All the (Na1-xKxNbO3 powders showed a similar orthorhombic phase structure. The K2CO3 content significantlyaffected the calcination temperature and particle size and shape. Large particle size, cubic shape and a lower calcined condition were observed in (Na1-xKxNbO3 powder with low K2CO3 content (x = 0.2.

  13. Kinetics of phase transformation and optical property of pink coral zirconia powders

    Energy Technology Data Exchange (ETDEWEB)

    Chu, Hsueh-Liang; Wang, Cheng-Li [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hwang, Weng-Sing [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Institute of Nanotechnology and Microsystems Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Lee, Kuen-Chan, E-mail: [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Zhou, Xuedong [State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070 (China); Wang, Moo-Chin, E-mail: [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China)


    Highlights: • The single phase of tetragonal ZrO{sub 2} formed when calcined at 1223 K for 1 h. • The tetragonal ZrO{sub 2} fully converted to ZrSiO{sub 4} when calcined at 1323–1473 K for 1 h. • The activation energy of t-ZrO{sub 2} formed is 399.9 kJ/mol when 5 mol% Fe{sub 2}O{sub 3} added. • The activation energy of the Fe/ZrSiO{sub 4} formed is 257.7 kJ/mol when 5 mol% Fe{sub 2}O{sub 3} added. • The growth morphology parameter and crystallization index are about 2.0 and 1.0. - Abstract: The kinetics of phase transformation and optical property of pink coral zircon powders have been studied. The ZrO{sub 2}–SiO{sub 2}–Fe{sub 2}O{sub 3} precursor powders were synthesized using Zr(NO{sub 3}){sub 4}⋅4H{sub 2}O, Si(C{sub 2}H{sub 5}O){sub 4} and Fe(NO{sub 3}){sub 3}⋅9H{sub 2}O as initial materials via the hot–wet routes. The kinetics of phase transformation of the ZrO{sub 2}–SiO{sub 2}–Fe{sub 2}O{sub 3} precursor powders was characterized by thermo-gravimetric (TG)/differential scanning calorimeter (DSC), X-ray diffraction (XRD), transmission electron microscopy (TEM), nano-beam electron diffraction (NBED), and spectrophotometry. The crystallization temperatures of tetragonal zirconia (t-ZrO{sub 2}) and zircon (ZrSiO{sub 4}) of ZrO{sub 2}–SiO{sub 2} precursor powders with 1 mol% Fe{sub 2}O{sub 3} were estimated to be approximately 1204 K and 1496 K, respectively, based on a DSC analysis conducted at a heating rate of 20 K/min. The activation energies of t-ZrO{sub 2} formulation are 428.2, 403.2, and 399.9 kJ/mol, respectively, for ZrO{sub 2}–SiO{sub 2} precursor powders containing 1, 3, and 5 mol% Fe{sub 2}O{sub 3}, respectively, whereas the activation energies of the Fe/ZrSiO{sub 4} formulation are 271.9, 261.9, and 257.7 kJ/mol, respectively. The parameter of growth morphology (n) and index of crystallization (m) were approximated as 2.0 and 1.0, respectively, meaning that two-dimensional growth with plate-like morphology was the

  14. Influence of Ultrafine 2CaO·SiO2 Powder on Hydration Properties of Reactive Powder Concrete

    Directory of Open Access Journals (Sweden)

    Hongfang Sun


    Full Text Available In this research, we assessed the influence of an ultrafine 2CaO·SiO2 powder on the hydration properties of a reactive powder concrete system. The ultrafine powder was manufactured through chemical combustion method. The morphology of ultrafine powder and the development of hydration products in the cement paste prepared with ultrafine powder were investigated by scanning electron microscopy (SEM, mineralogical composition were determined by X-ray diffraction, while the heat release characteristics up to the age of 3 days were investigated by calorimetry. Moreover, the properties of cementitious system in fresh and hardened state (setting time, drying shrinkage, and compressive strength with 5% ordinary Portland cement replaced by ultrafine powder were evaluated. From SEM micrographs, the particle size of ultrafine powder was found to be up to several hundred nanometers. The hydration product started formulating at the age of 3 days due to slow reacting nature of belitic 2CaO·SiO2. The initial and final setting times were prolonged and no significant difference in drying shrinkage was observed when 5% ordinary Portland cement was replaced by ultrafine powder. Moreover, in comparison to control reactive powder concrete, the reactive powder concrete containing ultrafine powder showed improvement in compressive strength at and above 7 days of testing. Based on above, it can be concluded that the manufactured ultrafine 2CaO·SiO2 powder has the potential to improve the performance of a reactive powder cementitious system.

  15. Study of Velocity and Materials on Tribocharging of Polymer Powders for Powder Coating Applications (United States)

    Biris, Alex S.; Trigwell, Steve; Sims, Robert A.; Mazumder, Malay K.


    Electrostatic powder deposition is widely used in a plethora of industrial-applications ranging from the pharmaceutical and, to farm equipment and automotive applications. The disadvantages of this technique are possible back corona (pin-like formations) onset and the Faraday penetration limitation (when the powder does not penetrate in some recessed areas). A possible solution to overcome these problems is to use tribochargers to electrostatically charge the powder. Tribocharging, or contact charging while two materials are in contact, is related to the work function difference between the contacting materials and generates bipolarly charged particles. The generation of an ion-free powder cloud by tribocharging with high bipolar charge and an overall charge density of almost zero, provides a better coverage of the recessed areas. In this study, acrylic and epoxy powders were fluidized and charged by passing through stainless steel, copper, aluminum, and polycarbonate static mixers, respectively. The particle velocity was varied to determine its effect on the net charge-to-mass ratio (QIM) acquired by the powders. In general, the Q/M increases rapidly when the velocity was increased from 1.5 to 2.5 m/s, remaining almost constant for higher velocities. Charge separation experiments showed bipolar charging for all chargers.

  16. Dust generation in powders: Effect of particle size distribution


    Chakravarty Somik; Le Bihan Olivier; Fischer Marc; Morgeneyer Martin


    This study explores the relationship between the bulk and grain-scale properties of powders and dust generation. A vortex shaker dustiness tester was used to evaluate 8 calcium carbonate test powders with median particle sizes ranging from 2μm to 136μm. Respirable aerosols released from the powder samples were characterised by their particle number and mass concentrations. All the powder samples were found to release respirable fractions of dust particles which end up decreasing with time. Th...

  17. 49 CFR 173.170 - Black powder for small arms. (United States)


    ... 49 Transportation 2 2010-10-01 2010-10-01 false Black powder for small arms. 173.170 Section 173... Class 7 § 173.170 Black powder for small arms. Black powder for small arms that has been classed in... § 173.56; (d) Each completed package must be marked “BLACK POWDER FOR SMALL ARMS” and “NA 0027”; and (e...

  18. Microstructural and mechanical characteristics of porous iron prepared by powder metallurgy. (United States)

    Capek, Jaroslav; Vojtěch, Dalibor


    The demand for porous biodegradable load-bearing implants has been increasing recently. Based on investigations of biodegradable stents, porous iron may be a suitable material for such applications. In this study, we prepared porous iron samples with porosities of 34-51 vol.% by powder metallurgy using ammonium bicarbonate as a space-holder material. We studied sample microstructure (SEM-EDX and XRD), flexural and compressive behaviors (universal loading machine) and hardness HV5 (hardness tester) of the prepared samples. Sample porosity increased with the amount of spacer in the initial mixtures. Only the pore surfaces had insignificant oxidation and no other contamination was observed. Increasing porosity decreased the mechanical properties of the samples; although, the properties were still comparable with human bone and higher than those of porous non-metallic biomaterials and porous magnesium prepared in a similar way. Based on these results, powder metallurgy appears to be a suitable method for the preparation of porous iron for orthopedic applications. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Development of cobalt ferrite powder preparation employing the sol-gel technique and its structural characterisation

    Directory of Open Access Journals (Sweden)

    Olabi A.G.


    Full Text Available This work focuses on the development of a method to make nano cobalt ferrite powder using a solgel process. A particular emphasis is devoted to the understanding of the role of the chemical parameters involved in the solgel technique, and of the heat treatment on the structures and morphologies of the materials obtained. Several samples of cobalt ferrite powder were obtained by varying the initial parameters of the process in addition to the heat treatment temperature. Xray diffraction and scanning electron microscopy were used to identify the structure and morphology of samples demonstrating the influence of the initial parameters. DTA/TGA was carried out on one sample to identify important reaction temperatures during the heat treatment. The average particle size, as estimated for one sample by the full width at half maximum (FWHM of the strongest Xray diffraction (XRD peak, was found to be about 45 nm. It has been found that the chelating agent and the crosslinker have a critical influence on the resultant structure, the particle size and the particle size distribution.


    Directory of Open Access Journals (Sweden)

    A. Izadpanahi


    Full Text Available In the following research, Lead magnesium niobate relaxor ferroelectric (PMN-PZT ceramic powders were synthesized using the combustion method grand urea as the fuel for the first time. The starting materials used were lead nitrate, magnesium acetate, niobium oxide, zirconium nitrate, titanium oxide.     The raw materials were first mixed using the general formula of (1-xPb(Mg1/3Nb2/3O3-xPb(Zr0.52Ti0.48O3, with  x=0.3. The synthesized powders were characterized using XRD, SEM and FTIR spectroscopy techniques. The X-ray diffraction patterns revealed that the structure of the prepared samples were tetragonal at 500,600,700 and 800 oC. However, the monoclinic phase was detected in the samples calcined at 800 oC and the amount of pyrocholore phase also drastically decreased at this temperature. The band gap widths of the samples were measured via UV spectroscopy in the wave number range of 400-4000cm-1. The results show that by increasing the calcination temperature, the band gap width of the prepared samples decreases. SEM micrographs verify that by rising the calcination temperature, the structure of the prepared samples becomes more homogenous.

  1. Carbothermal synthesis of Si3N4 powders using a combustion synthesis precursor (United States)

    Chu, Ai-min; Qin, Ming-li; Jia, Bao-rui; Lu, Hui-feng; Qu, Xuan-hui


    Si3N4 powders were synthesized by a carbothermal reduction method using a SiO2 + C combustion synthesis precursor derived from a mixed solution consisting of silicic acid (Si source), polyacrylamide (additive), nitric acid (oxidizer), urea (fuel), and glucose (C source). Scanning electron microscopy (SEM) micrographs showed that the obtained precursor exhibited a uniform mixture of SiO2 + C composed of porous blocky particles up to ˜20 μm. The precursor was subsequently calcined under nitrogen at 1200-1550°C for 2 h. X-ray diffraction (XRD) analysis revealed that the initial reduction reaction started at about 1300°C, and the complete transition of SiO2 into Si3N4 was found at 1550°C. The Si3N4 powders, synthesized at 1550°C, exhibit a mixture phase of α- and β-Si3N4 and consist of mainly agglomerates of fine particles of 100-300 nm, needle-like crystals and whiskers with a diameter of about 100 nm and a length up to several micrometers, and a minor amount of irregular-shaped growths.

  2. [Preparation of sub-standard samples and XRF analytical method of powder non-metallic minerals]. (United States)

    Kong, Qin; Chen, Lei; Wang, Ling


    In order to solve the problem that standard samples of non-metallic minerals are not satisfactory in practical work by X-ray fluorescence spectrometer (XRF) analysis with pressed powder pellet, a method was studied how to make sub-standard samples according to standard samples of non-metallic minerals and to determine how they can adapt to analysis of mineral powder samples, taking the K-feldspar ore in Ebian-Wudu, Sichuan as an example. Based on the characteristic analysis of K-feldspar ore and the standard samples by X-ray diffraction (XRD) and chemical methods, combined with the principle of the same or similar between the sub-standard samples and unknown samples, the experiment developed the method of preparation of sub-standard samples: both of the two samples above mentioned should have the same kind of minerals and the similar chemical components, adapt mineral processing, and benefit making working curve. Under the optimum experimental conditions, a method for determination of SiO2, Al2O3, Fe2O3, TiO2, CaO, MgO, K2O and Na2O of K-feldspar ore by XRF was established. Thedetermination results are in good agreement with classical chemical methods, which indicates that this method was accurate.

  3. An investigation of wear behaviors of different Monel alloys produced by powder metallurgy

    Energy Technology Data Exchange (ETDEWEB)

    Esgin, U.; Özyürek, D. [Karabük University, Technology Faculty, Department of Manufacturing Engineering / Karabuk (Turkey); Kaya, H., E-mail: [Kocaeli University, Asim Kocabiyik Vocational School of Higher Education, Department of Machine / Kocaeli (Turkey)


    In the present study, wear behaviors of Monel 400, Monel 404, Monel R-405 and Monel K-500 alloys produced by Powder Metallurgy (P/M) method were investigated. These compounds prepared from elemental powders were cold-pressed (600 MPa) and then, sintered at 1150°C for 2 hours and cooled down to the room temperature in furnace environment. Monel alloys produced by the P/M method were characterized through scanning electron microscope (SEM+EDS), X-ray diffraction (XRD), hardness and density measurements. In wear tests, standard pin-on-disk type device was used. Specimens produced within four different Monel Alloys were tested under 1ms{sup −1} sliding speed, under three different loads (20N, 30N and 40N) and five different sliding distances (400-2000 m). The results show that Monel Alloys have γ matrix and that Al{sub 0,9}Ni{sub 4,22} intermetallic phase was formed in the structure. Also, the highest hardness value was measured with the Monel K-500 alloy. In wear tests, the maximum weight loss according to the sliding distance, was observed in Monel 400 and Monel 404 alloys while the minimum weight loss was achieved by the Monel K-500 alloy.

  4. Characterisation of the Fe-10 wt% Si nanocrystalline powder obtained by mechanical alloying and annealing (United States)

    Stanciu, C. D.; Marinca, T. F.; Chicinaş, I.; Isnard, O.


    Nanocrystalline Fe-10 wt% Si powders has been obtained by mechanical alloying. The synthesis conditions as well as their influence on the structural and magnetic properties of this soft magnetic alloy have been investigated in the light of several experimental techniques (X-ray diffraction, neutron diffraction, DSC, magnetic measurement, SEM). By X-ray diffraction (XRD) investigations have been highlighted that Fe-Si alloy is formed after 4 h of mechanical milling and the mean crystallite size is down to 14 nm (8 h milled sample). The heat treatment leads to the formation of the Fe3Si compound with DO3-type superstructure for low milling times. The saturation magnetisation of the as-milled powders decreases in the first 4 h of milling due to the formation of the Fe-Si alloy. The behaviour of the saturation magnetisation versus milling time and annealing was explained by the different magnetic moment of iron atoms in Fe3Si structure. The Curie temperature decreases from 770 °C (the Curie temperature for pure iron) to about 650 °C after 8 h of milling.

  5. Surface modification of M-Ba-ferrite powders by polyaniline: Towards improving microwave electromagnetic response

    Energy Technology Data Exchange (ETDEWEB)

    Tang Xin, E-mail: [School of Petroleum Enginering, Southwest Petroleum University, 8, Xindu Road, Xindu District, Chengdu 610500 (China); Yang Yuanguang [School of Petroleum Enginering, Southwest Petroleum University, 8, Xindu Road, Xindu District, Chengdu 610500 (China)


    A composite of polyaniline (PANI)-coated M-type hexagonal barium ferrite (M-Ba-ferrite) powder was prepared by an in situ polymerization of an aniline monomer in the presence of M-Ba-ferrite particles. The obtained composite was characterized by Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The structure and microwave response properties were investigated. The continuous coverage of polyaniline has been produced on the platelet M-Ba-ferrite particle surface, and a core-shell structure has been formed. The results show that the coverage of polyaniline has a great influence on microwave response of M-Ba-ferrite particles. A polyaniline thin layer formed on the surface of a barium ferrite particle changes the character of frequency dispersion of microwave absorption. The results indicate the existence of an interaction at the interface of polyaniline macromolecule and barium ferrite particle, which influences the physical and chemical properties of the composite. The interaction and interfacial polarization are seen as important factors contributing to the influence on microwave response of the PANI-coated ferrite composite powders.

  6. Porous bioceramic bead prepared by calcium phosphate with sodium alginate gel and PE powder

    Energy Technology Data Exchange (ETDEWEB)

    Fu, Y.C. [Department of Orthopaedic Surgery, Kaohsiung Medical University Hospital, Kaohsiung 807, Taiwan (China); Ho, M.L.; Wu, S.C. [Department of Physiology, Kaohsiung Medical University, 100, Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China); Hsieh, H.S. [Faculty of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100, Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China); Wang, C.K. [Faculty of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100, Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China)], E-mail:


    The porous calcium phosphate beads were made by an alginate-interacting Ca ions mechanism on addition of a pore-forming polyethylene (PE) powder at 1250 deg. C sintering. The nature of the powders and porous beads were analyzed through X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR) and heavy metal analysis by inductively coupled plasma-optical emission spectroscopy (ICP-OES). The porous beads size and the pore microstructure characteristics were determined using scanning electron microscopy (SEM). Beside, the porosity analysis was evaluated out using an Archimedes' principle and mercury porosimetry. Then, the sodium ampicillin was penetrated/adsorbed onto calcium-deficient hydroxyapatite porous beads, and was subsequently released in PBS. No matter whether the raw material was HAp, TCP or biphase, the Ca{sub 9}(HPO{sub 4})(PO{sub 4}){sub 5}OH phase (CDHA) was formed only after sintering. Porous beads of various calcium phosphates with different sizes (0.9-1.1 mm) and pore size groups (60-120 {mu}m and lower than 10 {mu}m) were appeared. The release kinetics of sodium ampicillin from these porous beads have indicated the possibility of using these materials as possible carriers for drug delivery.

  7. Structural properties of delafossite multiferroic CuFeO2 powder (United States)

    Dhruv, Preksha N.; Solanki, Neha P.; Jotania, Rajshree B.


    CuFeO2 powder has been synthesized using modified sol-gel auto-combustion technique with and without the presence of Rosa indica and Vinca (Catharanthus roseus) flowers petal extract. In the first set of experiment, CuFeO2 ferrite precursors were heated in a muffle furnace at 1150°C for 4 hrs. and slowly cooled to room temperature. In the second set of experiment, CuFeO2 ferrite precursors were prepared in presence of Rosa indica flowers petal extract and then sintered at 1150°C for 4 hrs. The comparative studies have been carried out to observe the effect of Rosa indica flower petals extract on structural properties of the multiferroic CuFeO2 powder. XRD analysis of sample CuFeO2 prepared without using flower petals extract; heated at 1150 °C for 4 hrs. shows mixed phases while the sample synthesized in presence of Rosa indica flower petals extract shows formation of pure phase.

  8. Influence of a microcomposite and a nanocomposite on the properties of an epoxy-based powder coating

    Energy Technology Data Exchange (ETDEWEB)

    Piazza, Diego [Polymers Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil); Lorandi, Natalia P. [Corrosion and Surface Protection Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil); Pasqual, Charles I. [Polymers Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil); Scienza, Lisete C. [Corrosion and Surface Protection Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil); Zattera, Ademir J., E-mail: [Polymers Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil)


    Highlights: {yields} New materials for using as protective coatings for metal surfaces. {yields} Development of nanostructured powder paints. {yields} Characterization of the new material in the powder and coating form. {yields} Development of a new material for use in the automotive industry, industrial production of appliances, furniture industry. {yields} Development of new material using the process of mixing using a twin-screw extruder, followed by sintering process on a metal plate. - Abstract: The incorporation of nanoclays into coatings has been considered to be commercially favorable due to the improvements obtained in the barrier, thermal, and anticorrosion properties, among others, leading to the development of a new segment in the area of clean technologies: the application of nanocomposites to powder coatings. In this study, in order to compare the performance of a powder coating with the addition of a conventional load (barium sulfate) and a montmorillonite clay (MMT), two mixtures of commercial epoxy-based powder coating were prepared in the melt state, with the addition of 2 and 4% (w/w) of MMT, or 2 and 4% (w/w) of barium sulfate (BaSO{sub 4}). The thermal properties were investigated through thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to evaluate the load dispersion and the morphology of the systems formed. The physical and anticorrosion properties of the coatings were also investigated. The interaction of the MMT with the polymeric matrix, associated to the aspect ratio, resulted in better barrier properties, thermal stability, and adhesion to the metal substrate.

  9. Highly surface-roughened quasi-spherical silver powders in back electrode paste for silicon solar cells (United States)

    Yin, Peng; Liu, Shouchao; Li, Qiuying; Chen, Xiaolei; Guo, Weihong; Wu, Chifei


    In our work, highly surface-roughened quasi-spherical silver powders with controllable size and superior dispersibility, which have narrow size distribution and relatively high tap density, were successfully prepared by reducing silver nitrate with ascorbic acid in aqueous solutions. Gum arabic (AG) was selected as dispersant to prevent the agglomeration of silver particles. Furthermore, the effects of preparation conditions on the characteristics of the powders were systematically investigated. By varying the concentration of the reactants, dosage of dispersant, the feeding modes, synthesis temperature and the pH value of the mixture solution of silver nitrate and AG, the resulted silver particles displayed controllable size, different morphologies and surface roughness. The spherical silver powder with mean particle size of 1.20 µm, tap density of 4.1 g cm-3 and specific area value of 0.46 m2 g-1 was prepared by adjusting preparation conditions. The AG absorbed on the surface preventing the silver particles from diffusion and aggregation was proved by the ultraviolet spectra. Observations of SEM images showed that the as-prepared silver powders were relatively monodisperse silver spheres with highly roughened surface and the particle size was controllable from 1 µm to 5 µm, specific surface area value from approximately 0.2 m2 g-1 to 0.8 m2 g-1. X-ray diffraction (XRD) patterns, energy dispersive spectroscopy (EDS), x-ray photoelectron spectra (XPS) and thermal gravity analysis (TGA) demonstrated high crystallinity and purity of the obtained silver powders.

  10. Development of precipitation strengthened brass with Ti and Sn alloying elements additives by using water atomized powder via powder metallurgy route

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shufeng, E-mail: [Joining and Welding Research Institute, Osaka University, Osaka (Japan); Imai, Hisashi; Kondoh, Katsuyoshi [Joining and Welding Research Institute, Osaka University, Osaka (Japan); Kojima, Akimichi; Kosaka, Yoshiharu [San-Etsu Metals Co. LTD., 1892 OHTA, Tonami, Toyama (Japan); Yamamoto, Koji; Takahashi, Motoi [Nippon Atomized Metal Powders Corporation, 87-16, Nishi-Sangao, Noda, Chiba (Japan)


    Effect of Ti and Sn alloying elements on microstructure and mechanical properties of 60/40 brass has been studied via the powder metallurgy (P/M) route. The water-atomized BS40-0.6Sn1.0Ti (Cu40wt%Zn-0.6wt%Sn1.0wt%Ti) pre-alloyed powder was consolidated at various temperatures within range of 400-600 Degree-Sign C using spark plasma sintering (SPS) and hot extrusion was carried out at 500 Degree-Sign C. Effects of extrusion temperature on microstructure and tensile strength were investigated by employing SEM-EDS/EBSD, TEM, XRD and tensile test. Results indicated that super-saturated solid solution Ti and Sn elements created high chemical potential for a precipitate reaction in rapidly solidified brass powder, which showed significant strengthening effects on the extruded sample consolidated at lower temperature. Solid solubility of Ti in brass matrix decreased with increasing of sintering temperature, thus resulted in degradation of mechanical properties. Consequently, lower hot processing temperature is necessary to obtain excellent mechanical properties for BS40-0.6Sn1.0Ti during sintering and extrusion. An yield strength of 398 MPa and ultimate tensile strength of 615 MPa were achieved, they respectively showed 31.3% and 22.9% higher values than those of extruded Cu40Zn brass. -- Graphical abstract: The Ti and Sn alloying elements additions showed significant grain refinement on Cu40Zn-0.6Sn1.0Ti brass (b) as comparing with that of the conventional Cu40Zn brass (a), detected by electron backscatter diffraction (EBSD) technique. The grain boundaries maps of (a) BS40 (b) BS40-0.6Sn1.0Ti SPS compact sintered at 400 Degree-Sign C reveals by electron backscatter diffraction (EBSD) technique. Highlights: Black-Right-Pointing-Pointer Alloying elements Ti and Sn are proposed as additives in 60/40 brass. Black-Right-Pointing-Pointer Super-saturated Ti in powder creates high chemical potential for precipitation. Black-Right-Pointing-Pointer CuSn{sub 3}Ti{sub 5

  11. Transformation of meta-stable calcium silicate hydrates to tobermorite: reaction kinetics and molecular structure from XRD and NMR spectroscopy

    Directory of Open Access Journals (Sweden)

    Carroll Susan A


    Full Text Available Abstract Understanding the integrity of well-bore systems that are lined with Portland-based cements is critical to the successful storage of sequestered CO2 in gas and oil reservoirs. As a first step, we investigate reaction rates and mechanistic pathways for cement mineral growth in the absence of CO2 by coupling water chemistry with XRD and NMR spectroscopic data. We find that semi-crystalline calcium (alumino-silicate hydrate (Al-CSH forms as a precursor solid to the cement mineral tobermorite. Rate constants for tobermorite growth were found to be k = 0.6 (± 0.1 × 10-5 s-1 for a solution:solid of 10:1 and 1.6 (± 0.8 × 10-4 s-1 for a solution:solid of 5:1 (batch mode; T = 150°C. This data indicates that reaction rates for tobermorite growth are faster when the solution volume is reduced by half, suggesting that rates are dependent on solution saturation and that the Gibbs free energy is the reaction driver. However, calculated solution saturation indexes for Al-CSH and tobermorite differ by less than one log unit, which is within the measured uncertainty. Based on this data, we consider both heterogeneous nucleation as the thermodynamic driver and internal restructuring as possible mechanistic pathways for growth. We also use NMR spectroscopy to characterize the site symmetry and bonding environment of Al and Si in a reacted tobermorite sample. We find two [4]Al coordination structures at δiso = 59.9 ppm and 66.3 ppm with quadrupolar product parameters (PQ of 0.21 MHz and 0.10 MHz (± 0.08 from 27Al 3Q-MAS NMR and speculate on the Al occupancy of framework sites by probing the protonation environment of Al metal centers using 27Al{1H}CP-MAS NMR.

  12. Bone matrix calcification during embryonic and postembryonic rat calvarial development assessed by SEM-EDX spectroscopy, XRD, and FTIR spectroscopy. (United States)

    Henmi, Akiko; Okata, Hiroshi; Anada, Takahisa; Yoshinari, Mariko; Mikami, Yasuto; Suzuki, Osamu; Sasano, Yasuyuki


    Bone mineral is constituted of biological hydroxyapatite crystals. In developing bone, the mineral crystal matures and the Ca/P ratio increases. However, how an increase in the Ca/P ratio is involved in maturation of the crystal is not known. The relationships among organic components and mineral changes are also unclear. The study was designed to investigate the process of calcification during rat calvarial bone development. Calcification was evaluated by analyzing the atomic distribution and concentration of Ca, P, and C with scanning electron microscopy (SEM)-energy-dispersive X-ray (EDX) spectroscopy and changes in the crystal structure with X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Histological analysis showed that rat calvarial bone formation started around embryonic day 16. The areas of Ca and P expanded, matching the region of the developing bone matrix, whereas the area of C became localized around bone. X-ray diffraction and FTIR analysis showed that the amorphous-like structure of the minerals at embryonic day 16 gradually transformed into poorly crystalline hydroxyapatite, whereas the proportion of mineral to protein increased until postnatal week 6. FTIR analysis also showed that crystallization of hydroxyapatite started around embryonic day 20, by which time SEM-EDX spectroscopy showed that the Ca/P ratio had increased and the C/Ca and C/P ratios had decreased significantly. The study suggests that the Ca/P molar ratio increases and the proportion of organic components such as proteins of the bone matrix decreases during the early stage of calcification, whereas crystal maturation continues throughout embryonic and postembryonic bone development.

  13. Memory effect of activated Mg-Al hydrotalcite: in situ XRD studies during decomposition and gas-phase reconstruction. (United States)

    Pérez-Ramírez, Javier; Abelló, Sònia; van der Pers, Niek M


    The thermal decomposition of Mg-Al hydrotalcite and the subsequent reconstruction of the decomposed products in the presence of water vapor (2 vol. % H(2)O in N(2)) have been investigated by in situ XRD. Thermographic analysis and temperature-programmed desorption MS results complemented the diffraction data. Valuable mechanistic and kinetic insights into these processes, which are of prime importance for optimal activation of this type of material for catalytic applications, were obtained. Hydrotalcite decomposition to the mixed oxide proceeds via formation at 423-473 K of an intermediate phase, consisting of a highly disordered, dehydrated, layered structure. The latter evolves by removal of interlayer water on heating, causing a shrinking of the interlayer space (it is up to 45 % smaller than in the as-synthesized hydrotalcite). Above 623 K, Mg(Al)O(x) oxide with the periclase structure is formed. Reversion of the intermediate dehydrated structure to hydrotalcite upon contact with water vapor is complete and very fast at room temperature. Recovery of hydrotalcite from the oxide calcined at 723 K is two orders of magnitude slower than rehydration of the intermediate layered structure and one order of magnitude slower than the typically practiced liquid-phase reconstruction. In contrast to the decomposition, the reconstruction mechanism does not involve an intermediate phase. The gas-phase rehydration and reconstruction was interrupted above 303 K. This is attributed to the poor wetting of the surface of the decomposed materials induced by hampered H(2)O adsorption above room temperature at the water vapor pressure applied. The Avrami-Erofe'ev model describes the reconstruction kinetics well.

  14. 49 CFR 173.171 - Smokeless powder for small arms. (United States)


    ... 49 Transportation 2 2010-10-01 2010-10-01 false Smokeless powder for small arms. 173.171 Section 173.171 Transportation Other Regulations Relating to Transportation PIPELINE AND HAZARDOUS MATERIALS... Class 7 § 173.171 Smokeless powder for small arms. Smokeless powder for small arms which has been...

  15. Magnetic properties of lanthanum orthoferrite fine powders prepared ...

    Indian Academy of Sciences (India)


    Abstract. Fine powders of lanthanum iron oxide, LaFeO3, have been prepared by solid state reaction as well as sol–gel synthesis and nebulized spray pyrolysis. Struc- tures, morphologies and magnetic susceptibility measurements of these powders have been examined. The powders prepared by all the three ...

  16. Plant dried powders as biocatalysts: Hydrolysis of 1- phenylpropanol ...

    African Journals Online (AJOL)

    The hydrolytic ability of plant dried powders, lyophilized or acetone dried, was tested on the hydrolysis of racemic 1-phenylpropanol acetate. Most of the twenty powders tested showed hydrolytic activity, however the best values of conversion and enantioselectivity were reached with the lyophilized powder of nopal (27% ...

  17. Changes in hydroxyapatite powder properties via heat treatment

    Indian Academy of Sciences (India)

    The properties of hydroxyaptite (HA) powder, especially its physical one, are largely influenced by the heat treatment process. Controlling of these changes is vital in deciding the suitability of applying this powder in wet processing routes for green body fabrication. Chemically, the crystallinity of the HA powder was found to ...


    Blainey, A.


    A method is given for enclosing a body of uranium in a sheath of compacted beryllium or zirconium powder and comprises enveloping the body with uncompacted powder and pressing at a temperature above the beta - gamma transition point of uranium, thereby causing the uranium to flow and isotropically compress the powder.

  19. 21 CFR 520.540a - Dexamethasone powder. (United States)


    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Dexamethasone powder. 520.540a Section 520.540a... DRUGS, FEEDS, AND RELATED PRODUCTS ORAL DOSAGE FORM NEW ANIMAL DRUGS § 520.540a Dexamethasone powder. (a) Specifications. Dexamethasone powder is packaged in packets containing 10 milligrams of dexamethasone. (b...

  20. Powder metallurgical processing and metal purity: A case for ...

    Indian Academy of Sciences (India)


    powder metallurgy route, because of many associated advantages (Upadhyaya 1997). The purity of the starting metal or ceramic powder is of significance in controlling the microstructure/properties/processing and performance of such products. The major methods of production of metal powders are: chemical, physical and ...

  1. 21 CFR 520.1720e - Phenylbutazone powder. (United States)


    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Phenylbutazone powder. 520.1720e Section 520.1720e... DRUGS, FEEDS, AND RELATED PRODUCTS ORAL DOSAGE FORM NEW ANIMAL DRUGS § 520.1720e Phenylbutazone powder. (a) Specifications—(1) Each 1.15 grams (g) of powder contains 1 g phenylbutazone. (2) Each 10 g of...

  2. Determination of Dispersion of Zucchini and Cabbage Powders

    Directory of Open Access Journals (Sweden)

    M.I. Pogozhyh


    Full Text Available Particle size of cabbage and zucchini powders was determined by microscopy. It is shown that under the identical conditions of drying, grinding and other stages of the process, the cabbage powder has a higher content of fine fraction. Promising application of cabbage and zucchini powders in restaurant industry is indicated. Case diagram of the received production use is developed.

  3. 21 CFR 520.2087 - Roxarsone soluble powder. (United States)


    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Roxarsone soluble powder. 520.2087 Section 520...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS ORAL DOSAGE FORM NEW ANIMAL DRUGS § 520.2087 Roxarsone soluble powder. (a) Specifications. Each ounce (avoirdupois) of soluble powder contains 21.7 grams of roxarsone...

  4. 21 CFR 520.44 - Acetazolamide sodium soluble powder. (United States)


    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Acetazolamide sodium soluble powder. 520.44 Section 520.44 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... Acetazolamide sodium soluble powder. (a) Specifications. The drug is in a powder form containing acetazolamide...

  5. 21 CFR 520.110 - Apramycin sulfate soluble powder. (United States)


    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Apramycin sulfate soluble powder. 520.110 Section 520.110 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... sulfate soluble powder. (a) Specifications. A water soluble powder used to make a medicated drinking water...

  6. 21 CFR 520.1044c - Gentamicin sulfate soluble powder. (United States)


    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Gentamicin sulfate soluble powder. 520.1044c Section 520.1044c Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... Gentamicin sulfate soluble powder. (a) Specifications. Each gram of gentamicin sulfate soluble powder...

  7. Phase transformation and exchange bias effects in mechanically alloyed Fe/magnetite powders

    Energy Technology Data Exchange (ETDEWEB)

    Crisan, O., E-mail: [National Institute for Materials Physics, P.O. Box MG-7, 077125 Bucharest-Magurele (Romania); Crisan, A.D. [National Institute for Materials Physics, P.O. Box MG-7, 077125 Bucharest-Magurele (Romania)


    Highlights: > Phase evolution in Fe/Fe{sub 3}O{sub 4} nanopowder monitored by synchrotron X-ray diffraction. > Fe/Fe{sub 3}O{sub 4} nanopowder undergo an incomplete redox reaction with formation of FeO. > FeO decomposes gradually into initial constituents at T up to 500 deg. C. > At higher T the redox reaction is reversible, at 900 deg. C only FeO is observed. > For the first time a strong exchange bias effect, related to FeO content, is observed. - Abstract: Nanostructured powders processed by ball milling of a mixture of Fe and Fe{sub 3}O{sub 4} at room temperature are shown to undergo an incomplete redox reaction with formation of FeO during the milling process. This reaction is favored by the high energy introduced during the mechano-alloying process. Concurrent effects of milling such as grain refinement down to the nanometre scale lead at the end of the milling processes to a mixed multiphase powder of nanograins, with Fe and Fe oxide grains inter-dispersed. We show that in the as-milled Fe/Fe{sub 3}O{sub 4} powder, during milling process, wuestite (FeO) is formed as a consequence of the redox reaction. Moreover, with increasing temperature, the system undergoes an inverse phase transformation towards the initial Fe and Fe{sub 3}O{sub 4} phases until about 450 deg. C. Above this temperature the reduction reaction Fe + Fe{sub 3}O{sub 4} = 4FeO is reinitiated, resulting in sharp decrease of Fe and Fe{sub 3}O{sub 4} content from about 550 deg. C and almost complete disappearance of these phases at about 900 deg. C. This transformation was investigated via an energy-dispersive in situ X-ray diffraction experiment using the synchrotron radiation. This study allows direct collection of X-ray patterns after few minutes exposure, at selected temperatures, ranging between 20 deg. C and 1000 deg. C. The structural and magnetic characterizations of the nanograin powders, as-milled and annealed at several temperatures, are studied using XRD, SEM and magnetic measurements

  8. An Investigation on the Sinterability and the Compaction Behavior of Aluminum/Graphene Nanoplatelets (GNPs) Prepared by Powder Metallurgy (United States)

    Saboori, A.; Novara, C.; Pavese, M.; Badini, C.; Giorgis, F.; Fino, P.


    In the present study, the densification response of Al matrix reinforced with different weight percentages (0, 0.5, 1.0, 1.5 and 2.0 wt.%) of graphene nanoplatelets (GNPs) was studied. These composites were produced by a wet method followed by a conventional powder metallurgy. The Raman spectrum of graphene indicates that preparation of the composites through the wet mixing method did not affect the disordering and defect density in the GNPs structure. The nanocomposite powder mixture was consolidated via a cold uniaxial compaction. The samples were sintered at different temperatures (540, 580 and 620 °C) under nitrogen flow so as to assess the sinterability of the nanocomposites. X-ray diffraction (XRD) has been carried out to check the possible reaction between GNPs and aluminum. According to the XRD patterns, it seems that Al4C3 did not form during the fabrication process. The relative density, compressibility, sinterability and Vickers hardness of the nanocomposites were also evaluated. The effects of GNPs on the consolidation behavior of the matrix were studied using the Heckel, Panelli and Ambrosio Filho, and Ge equations. The outcomes show that at early stage of consolidation the rearrangement of particles is dominant, while by increasing the compaction pressure, due to the load partitioning effect of GNPs, the densification rate of the powder mixture decreases. Moreover, the fabricated nanocomposites exhibited high Vickers hardness of 67 HV5, which is approximately 50% higher than monolithic aluminum. The effect of graphene addition on the thermal conductivity of Al/GNPs nanocomposites was evaluated by means of thermal diffusivity measurement, and the results showed that the higher thermal conductivity can be only achieved at lower graphene content.

  9. Mechanochemical synthesis evaluation of nanocrystalline bone-derived bioceramic powder using for bone tissue engineering

    Directory of Open Access Journals (Sweden)

    Amirsalar Khandan


    Full Text Available Introduction: Bone tissue engineering proposes a suitable way to regenerate lost bones. Different materials have been considered for use in bone tissue engineering. Hydroxyapatite (HA is a significant success of bioceramics as a bone tissue repairing biomaterial. Among different bioceramic materials, recent interest has been risen on fluorinated hydroxyapatites, (FHA, Ca 10 (PO 4 6 F x (OH 2−x . Fluorine ions can promote apatite formation and improve the stability of HA in the biological environments. Therefore, they have been developed for bone tissue engineering. The aim of this study was to synthesize and characterize the FHA nanopowder via mechanochemical (MC methods. Materials and Methods: Natural hydroxyapatite (NHA 95.7 wt.% and calcium fluoride (CaF 2 powder 4.3 wt.% were used for synthesis of FHA. MC reaction was performed in the planetary milling balls using a porcelain cup and alumina balls. Ratio of balls to reactant materials was 15:1 at 400 rpm rotation speed. The structures of the powdered particles formed at different milling times were evaluated by X-ray diffraction (XRD, scanning electron microscopy (SEM and transmission electron microscopy (TEM. Results: Fabrication of FHA from natural sources like bovine bone achieved after 8 h ball milling with pure nanopowder. Conclusion: F− ion enhances the crystallization and mechanical properties of HA in formation of bone. The produced FHA was in nano-scale, and its crystal size was about 80-90 nm with sphere distribution in shape and size. FHA powder is a suitable biomaterial for bone tissue engineering.

  10. Oxidation behavior of Ni powder and Ni powder compact; Ni fun oyobi Ni fun atsufuntai no sanka kyodo

    Energy Technology Data Exchange (ETDEWEB)

    Yamazaki, M.; Ochiai, S.; Watanabe, Y. [Teikyo Univ., Tokyo (Japan)


    With an objective to investigate reactions of metal powder and metal powder compact having open pores with gases, their oxidation behavior was elucidated by taking Ni powder and Ni powder compact as examples. Oxidation rate of the Ni powder can be expressed by the Jander equation, and activation energy for the oxidation was 0.948 times 10 {sup 5} J/mol. Oxidation rate of the Ni powder compact is equal to that of powder not made into compact in the initial stage of the oxidation, but it decreases as time elapses because of occurrence of packing of oxide. Difference in oxidation rate inside and outside the powder compact is very little. The oxidation rate of the powder compact was analyzed by using an improved Jander model. More specifically, a model was used, in which concentration difference of diffused components in the oxides decreases with progress of the oxidation, whereas 1.113 times 10 {sup 5} J/mol was derived as the activation energy of the oxidation. The cause for the activation energy for the oxidation of the powder and powder compact being about half of that for bulk Ni is because of low temperature oxidation of the powder, and tensile stress generated between metal particles and spherical shell shaped oxides, which make production of Ni {sup 2+} more difficult. 5 refs., 4 figs., 1 tab.

  11. Fabricating solid carbon porous electrodes from powders (United States)

    Kaschmitter, J.L.; Tran, T.D.; Feikert, J.H.; Mayer, S.T.


    Fabrication is described for conductive solid porous carbon electrodes for use in batteries, double layer capacitors, fuel cells, capacitive deionization, and waste treatment. Electrodes fabricated from low surface area (graphite and cokes exhibit excellent reversible lithium intercalation characteristics, making them ideal for use as anodes in high voltage lithium insertion (lithium-ion) batteries. Electrodes having a higher surface area, fabricated from powdered carbon blacks, such as carbon aerogel powder, carbon aerogel microspheres, activated carbons, etc. yield high conductivity carbon composites with excellent double layer capacity, and can be used in double layer capacitors, or for capacitive deionization and/or waste treatment of liquid streams. By adding metallic catalysts to high surface area carbons, fuel cell electrodes can be produced. 1 fig.

  12. Powder metallurgy bearings for advanced rocket engines (United States)

    Fleck, J. N.; Killman, B. J.; Munson, H.E.


    Traditional ingot metallurgy was pushed to the limit for many demanding applications including antifriction bearings. New systems require corrosion resistance, better fatigue resistance, and higher toughness. With conventional processing, increasing the alloying level to achieve corrosion resistance results in a decrease in other properties such as toughness. Advanced powder metallurgy affords a viable solution to this problem. During powder manufacture, the individual particle solidifies very rapidly; as a consequence, the primary carbides are very small and uniformly distributed. When properly consolidated, this uniform structure is preserved while generating a fully dense product. Element tests including rolling contact fatigue, hot hardness, wear, fracture toughness, and corrosion resistance are underway on eleven candidate P/M bearing alloys and results are compared with those for wrought 440C steel, the current SSME bearing material. Several materials which offer the promise of a significant improvement in performance were identified.

  13. Adsorption Studies of Radish Leaf Powder

    Directory of Open Access Journals (Sweden)



    Full Text Available Radish leaves (Raphanus sativus powder fractions was subjected to moisture adsorption isotherms at different isothermal temperature conditions from 15-45°C with an equal interval of 10°C. The sorption data obtained in gravimetric static method under 0.11–0.90 water activity conditions were subjected for sorption isotherms and found to be typical sigmoid trend. Experimental data were assessed for the applicability in the prediction through sorption models fitting and found that Polynomial and GAB equations performed well over all fitted models in describing equilibrium moisture content – equilibrium relative humidity (EMC–ERH relationships for shelf stable dehydrated radish leaf powder, over the entire range of temperatures condition under study. The net isosteric heat of sorption, differential entropy and free energy were determined at different temperatures and their dependence was seen with respect to equilibrium moisture content.

  14. Dry powder mixes comprising phase change materials (United States)

    Salyer, Ival O.


    Free flowing, conformable powder-like mix of silica particles and a phase change material (p.c.m.) is disclosed. The silica particles have a critical size of about 7.times.10.sup.-3 to about 7.times.10.sup.-2 microns and the pcm must be added to the silica in an amount of 80 wt. % or less pcm per combined weight of silica and pcm. The powder-like mix can be used in tableware items, medical wraps, tree wraps, garments, quilts and blankets, and in cementitious compositions of the type in which it is beneficial to use a pcm material. The silica-pcm mix can also be admixed with soil to provide a soil warming effect and placed about a tree, flower, or shrub.

  15. Ignition of THKP and TKP pyrotechnic powders :

    Energy Technology Data Exchange (ETDEWEB)

    Maharrey, Sean P.; Erikson, William W; Highley, Aaron M.; Wiese-Smith, Deneille; Kay, Jeffrey J


    We have conducted Simultaneous Thermogravimetric Modulated Beam Mass Spectrometry (STMBMS) experiments on igniter/actuator pyrotechnic powders to characterize the reactive processes controlling the ignition and combustion behavior of these materials. The experiments showed a complex, interactive reaction manifold involving over ten reaction pathways. A reduced dimensionality reaction manifold was developed from the detailed 10-step manifold and is being incorporated into existing predictive modeling codes to simulate the performance of pyrotechnic powders for NW component development. The results from development of the detailed reaction manifold and reduced manifold are presented. The reduced reaction manifold has been successfully used by SNL/NM modelers to predict thermal ignition events in small-scale testing, validating our approach and improving the capability of predictive models.

  16. Uniting Electron Crystallography and Powder Diffraction

    CERN Document Server

    Shankland, Kenneth; Meshi, Louisa; Avilov, Anatoly; David, William


    The polycrystalline and nanocrystalline states play an increasingly important role in exploiting the properties of materials, encompassing applications as diverse as pharmaceuticals, catalysts, solar cells and energy storage. A knowledge of the three-dimensional atomic and molecular structure of materials is essential for understanding and controlling their properties, yet traditional single-crystal X-ray diffraction methods lose their power when only polycrystalline and nanocrystalline samples are available. It is here that powder diffraction and single-crystal electron diffraction techniques take over, substantially extending the range of applicability of the crystallographic principles of structure determination.  This volume, a collection of teaching contributions presented at the Crystallographic Course in Erice in 2011, clearly describes the fundamentals and the state-of-the-art of powder diffraction and electron diffraction methods in materials characterisation, encompassing a diverse range of discipl...

  17. Properties of Waste Tire Rubber Powder

    Directory of Open Access Journals (Sweden)

    M. Bekhiti


    Full Text Available Scrap tires are abundant and alarming waste. The aggregates resulting from the crushing of the waste tires are more and more used in the field of civil engineering (geotechnical, hydraulic works, light concretes, asphaltic concretes, etc.. Depending on the type of the used tires, dimensions and possible separations and treatment, the physical and mechanical characteristics of these aggregates might change. Some physical, chemical and direct shear tests were performed on three gradation classes of waste tire rubber powder. The tests results were combined with data from previous studies to generate empirical relationships between cohesion, friction angle and particle size of waste tire powder rubber. A cubic (third order regression model seems to be more appropriate compared to linear and quadratic models.

  18. Solving Crystal Structures from Powder Diffraction Data

    DEFF Research Database (Denmark)

    Christensen, A. Nørlund; Lehmann, M. S.; Nielsen, Mogens


    High resolution powder data from both neutron and X-ray (synchrotron) sources have been used to estimate the possibility of direct structure determination from powder data. Two known structures were resolved by direct methods with neutron and X-ray data. With synchrotron X-ray data, the measured...... range of data was insufficient for a structure analysis, but the R-factor calculations showed the intensities extracted from the profile data to be of acceptable quality. The results were used to estimate the largest structure that might be solved using routine techniques. It was found that the limit...... would be near twenty atoms in the asymmetric part of a centro-symmetric structure....

  19. Physical and chemical stability of tagatose powder. (United States)

    Grant, Lenese D; Bell, Leonard N


    Tagatose is a reduced-calorie monosaccharide that displays prebiotic properties. Water can interact with powdered tagatose to varying extents, depending upon the storage environment. Adsorbed water can impact the stability of tagatose, altering its functionality and usability as an ingredient. The objective of this study was to evaluate the physical and chemical stability of bulk tagatose powder as a function of relative humidity (RH) and temperature. Powdered tagatose was stored in desiccators at 20, 30, and 40 °C and 33% to 85% RH. Moisture contents (MC), physical characteristics, tagatose degradation profiles, and browning kinetics were monitored for 12 mo. The critical RH associated with deliquescence (RH0) was approximately 85% at 20 °C. MC values below RH0 were all less than 2% (wb). The MC at 85% RH ranged from 55% to 80% (wb), increasing as temperature decreased. At 33% RH and 20 °C tagatose remained a free flowing powder. As either temperature or RH increased, varying degrees of physical caking occurred. At 85% RH, tagatose deliquesced at all temperatures. Browning occurred in all samples at 40 °C. Despite physical caking and browning, measurable tagatose degradation was only observed in the deliquesced sample at 85% RH and 40 °C, where 20% loss occurred in 6 mo. Although extreme RHs and temperatures are required for tagatose degradation to occur, intermediate RHs and temperatures promote physical caking and deliquescence, which create handling problems during product formulation. The exposure of tagatose to elevated relative humidities and temperatures should be avoided to maintain its physical and chemical quality. © 2012 Institute of Food Technologists®

  20. Compaction of amorphous iron–boron powder

    DEFF Research Database (Denmark)

    Hendriksen, Peter Vang; Mørup, Steen; Koch, Christian


    Large scale practical use of bulk amorphous alloys requires the capability of molding the material to a desired design, for instance by compaction of an amorphous powder. This is a difficult task because the sintering temperature is limited by the crystallization temperature of the alloy.1 Here w...... of density and structure on compaction pressure and compaction temperature. Journal of Applied Physics is copyrighted by The American Institute of Physics....



    Mustafacan , Kutsal


    The intentional use of conventional tin-lead (Sn-Pb) solder alloys was restricted with legislations across the world due to the toxic nature and the adverse effects of lead on health and the environment. Consequently, the development of new lead-free solder alloys has become a significant area of research. In addition to these health concerns, the continuing miniaturization trend of the consumer electronics has been pushing the production of solders from bulk form to powder form. In this stud...

  2. Modeling dissolution of sparingly soluble multisized powders


    Almeida, Luís Pereira de; Simões, Sérgio; Brito, Paulo; Portugal, António; Figueiredo, Margarida


    The dissolution of powder drugs, besides being a topic of utmost importance, especially for the sparingly soluble ones, is far from being well-explained. The purpose of the present study is, on the one hand, to obtain experimental dissolution profiles and, on the other hand, to analyze and process the data for dissolution modeling. Three different size fractions of a widely used sparingly soluble drug - ibuprofen - were fully characterized with regard to its particle size distribution, specif...

  3. Powder-Metallurgical Bearings For Turbopumps (United States)

    Bhat, B. N.; Humphries, T. S.; Thom, R. L.; Moxson, V.; Friedman, G. I.; Dolan, F. J.; Shipley, R. J.


    Bearings fabricated by powder metallurgy developed for use in machines subjected to extremes of temperature, rolling-contact cyclic stresses, and oxidizing or otherwise corrosive fluids. Bearings also extend operating lives of other machines in which bearings required to resist extreme thermal, mechanical, and chemical stresses. One alloy exhibiting outstanding properties was MRC-2001. Resistance to fatigue, stress corrosion cracking, and wear found superior to that of 440C stainless steel.

  4. Low-Flow-Rate Dry-Powder Feeder (United States)

    Ramsey, Keith E.


    Apparatus feeds small, precise flow of dry powder through laser beam of optical analyzer, measuring patterns of light created by forward scattering (Fraunhofer diffraction) of laser beam from powder particles. From measurement, statistical distribution of sizes of powder particles computed. Developed for analyzing particle-size distributions of solid-propellant powders. Also adapted to use in pharmaceutical industry, in manufacture of metal powder, and in other applications in which particle-size distributions of materials used to control rates of chemical reactions and/or physical characteristics of processes.

  5. Preparation and utilization of metal oxide fine powder

    Energy Technology Data Exchange (ETDEWEB)



    Metal oxide fine powders are used as new materials in many industrial fields. It is necessary to develop the technology for manufacturing such powders to improve the domestic industry. The purpose of present research is to develop technologies for the preparation and utilization of metal oxide fine powders. This research project is consisted of two main subjects. One is to develop processing technology on ultrafine silica powder of less than 100 nanometer in particle size, the other is on antimony trioxide powder which is used as flame retardant in plastic rubber, and textile industries. (author). 46 refs., 19 tabs., 35 figs.

  6. Modeling of Powder Bed Manufacturing Defects (United States)

    Mindt, H.-W.; Desmaison, O.; Megahed, M.; Peralta, A.; Neumann, J.


    Powder bed additive manufacturing offers unmatched capabilities. The deposition resolution achieved is extremely high enabling the production of innovative functional products and materials. Achieving the desired final quality is, however, hampered by many potential defects that have to be managed in due course of the manufacturing process. Defects observed in products manufactured via powder bed fusion have been studied experimentally. In this effort we have relied on experiments reported in the literature and—when experimental data were not sufficient—we have performed additional experiments providing an extended foundation for defect analysis. There is large interest in reducing the effort and cost of additive manufacturing process qualification and certification using integrated computational material engineering. A prerequisite is, however, that numerical methods can indeed capture defects. A multiscale multiphysics platform is developed and applied to predict and explain the origin of several defects that have been observed experimentally during laser-based powder bed fusion processes. The models utilized are briefly introduced. The ability of the models to capture the observed defects is verified. The root cause of the defects is explained by analyzing the numerical results thus confirming the ability of numerical methods to provide a foundation for rapid process qualification.

  7. New generation concretes including reactive powder concretes

    Directory of Open Access Journals (Sweden)

    Stefania Grzeszczyk


    Full Text Available Based on a broad literature review, this paper presents characteristics of new generation composites on the basis of cements which are applied in engineering structures and in rehabilitation of structures. The role of cement, microfillers, superplasticizers and fibers in the above stated composites i.e. factors which allow for the maximum packing of particles in the cement matrix and a minimum pore volume, and the increase in composite bending strength, have been discussed. Special attention was paid to Reactive Powder Concrete in which coarse aggregate was replaced by ground quartz and sand. Such composites contain active microfillers and the applied new-generation superplasticizers allow us to decrease the water-cement ratio in the composite up to 0.2. Whereas, steel fibre additive allows us to significantly improve the bending strength.The paper presents the properties of the excellent Ductal — a composite from Reactive Powder Concrete, which at compressive strength from 180 to 230 MPa achieves the tensile strength of 30 to 50 MPa. Its application allows us to create slim profiles and tall light and slender, and simultaneously durable and corrosion-resistant structural elements of considerable span. This paper gives a few examples of Ductal application in practice.[b]Keywords[/b]: civil engineering, composite materials, reactive powder concrete

  8. Shewanella strain isolated from black powder

    Energy Technology Data Exchange (ETDEWEB)

    Lutterbach, Marcia T.S.; Contador, Luciana S.; Oliveira, Ana Lucia C.; Galvao, Mariana M. [National Institute of Technology (INT), Rio de Janeiro, RJ (Brazil); Pimenta, Gutemberg S. [PETROBRAS, Rio de Janeiro, RJ (Brazil)


    Black powder is a term frequently used to refer to residues formed by various types of iron sulfides mixed with contaminants eventually present in the natural gas flow. According to some researchers, the occurrence of black powder in gas pipelines, besides its chemical corrosion origin, can be directly related to the sulfate-reducing bacteria (SRB) metabolism in this environment. A black powder sample was inoculated in a Post gate E medium modified with the addition of thioglycolate. The resulting positive culture was kept in the laboratory for four years until its use. A dilution technique was then performed aiming to isolate an SRB strain. The bacterial strain isolated and identified through DNA sequencing was not an SRB but rather a Shewanella sp. Compared to the sulfate-reducing bacteria group-traditionally considered the foremost responsible for microbially-influenced corrosion (MIC) - Shewanella is a facultative anaerobe and has a versatile metabolism. Shewanella is able to reduce ferric iron and sulfite, oxidize hydrogen gas, and produce hydrogen sulfide; therefore, these bacteria can be responsible for MIC and pit formation. The isolated Shewanella was used in a corrosion experiment, and the corrosion products were characterized by X-ray diffraction, identifying iron sulfides, iron oxides, and sulfur. Our results indicate that the strain isolated, S. putrefaciens, plays a key role in corrosion problems in gas pipelines. (author)

  9. Moisture sorption of Thai red curry powder

    Directory of Open Access Journals (Sweden)

    Sudathip Inchuen


    Full Text Available Moisture sorption study was conducted on Thai red curry powder prepared by two different drying methods, viz. microwave and hot-air drying. Moisture sorption isotherms of the red curry powder at 30 C and water activity in the range of 0.113-0.970 were determined by a static gravimetric method. The isotherms exhibited Type III behaviour. The moisture sorption data were fitted to several sorption models and a non-linear regression analysis method was used to evaluate the constants of the sorption equations. The fit was evaluated using the coefficient of determination (R2, the reduced chi-square (2 and the root mean square error (RMSE. The GAB model followed by the Lewiski-3 model gave the best fit to the experimental data. The monolayer moisture content, taken as the safe minimum moisture level in the red curry powder, was determined using the BET equation and was found to range between 0.080 - 0.085 gram water per gram dry matter.

  10. Cinnamon zeylanicum bark extract and powder mediated green synthesis of nano-crystalline silver particles and its bactericidal activity. (United States)

    Sathishkumar, M; Sneha, K; Won, S W; Cho, C-W; Kim, S; Yun, Y-S


    The exploitation of various plant materials for the biosynthesis of nanoparticles is considered a green technology as it does not involve any harmful chemicals. The present study reports the synthesis of silver (Ag) nanoparticles from silver precursor using the bark extract and powder of novel Cinnamon zeylanicum. Water-soluble organics present in the plant materials were mainly responsible for the reduction of silver ions to nano-sized Ag particles. TEM and XRD results confirmed the presence of nano-crystalline Ag particles. The pH played a major role in size control of the particles. Bark extract produced more Ag nanoparticles than the powder did, which was attributed to the large availability of the reducing agents in the extract. Zeta potential studies showed that the surface charge of the formed nanoparticles was highly negative. The EC(50) value of the synthesized nanoparticles against Escherichia coli BL-21 strain was 11+/-1.72 mg/L. Thus C. zeylanicum bark extract and powder are a good bio-resource/biomaterial for the synthesis of Ag nanoparticles with antimicrobial activity.

  11. Temperature dependence and P/Ti ratio in phosphoric acid treatment of titanium dioxide and powder properties. (United States)

    Onoda, H; Matsukura, A


    Titanium dioxide has photocatalytic activity and is used as a white pigment for cosmetics. A certain degree of sebum on the skin is decomposed by the ultraviolet radiation in sunlight. In this work, titanium dioxide was shaken with phosphoric acid to synthesize a white pigment for cosmetics. Titanium dioxide was treated with 0.1 mol/L of phosphoric acid at various P/Ti molar ratios, and then shaken in hot water for 1 h. The chemical composition, powder properties, photocatalytic activity, colour phase, and smoothness of the obtained powder were studied. The obtained materials indicated XRD peaks of titanium dioxide, however the peaks diminished subsequent to phosphoric acid treatment. The samples included small particles with sub-micrometer size. The photocatalytic activity of the obtained powders decreased, decomposing less sebum on the skin. Samples prepared at high P/Ti ratio with high shaking temperature indicated low whiteness in in L*a*b* colour space. The shaking and heating temperature and P/Ti ratio had influence on the smoothness of the obtained materials. Phosphoric acid treatment of titanium dioxide is an effective method to inhibit photocatalytic activity for a white pigment. © 2014 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

  12. Microstructure and Properties of W-Cu Composite/Fe-Based Powder Alloy Vacuum Brazed Joint with Different Filler Metals (United States)

    Xia, C. Z.; Yang, J.; Xu, X. P.; Zou, J. S.


    W-Cu composite and Fe-based powder alloy were brazed with filler metals of Ag-Cu and Cu-Mn-Co alloys in a vacuum furnace. Both of filler metals can join W-Cu composite with Fe-based powder alloy directly in the experiment process. Microstructure, distribution of elements and fracture morphology were observed and analyzed using scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS) methods, and phase composition of bonding area was analyzed by X-ray diffraction (XRD). The obtained results indicated that the smooth faying surface and dense microstructure of brazed joint were formed and the primary microstructure of brazing seam were, respectively, Ag(Cu) solid solution and Cu(Mn) solid solution, which ensured forming the stable connection of brazed joint. The bending strength of Ag-based and Cu-based brazed joint can, respectively, reach to 317 and 704 MPa, where fracture showed a typical ductile fracture characteristic. The fracture of Cu-based brazed joint located at brazing seam area, and the fracture of Ag-based brazed joint occurred in Fe-based powder alloy side.

  13. Investigation of preparation and characteristics of Sn-Bi eutectic powders derived from a high shear mechanical approach

    Energy Technology Data Exchange (ETDEWEB)

    Liang Kun; Tang Xianzhong [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Yu Lijing [Kunming Institute of Physics, Kunming 650223 (China); Wang Ni [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Hu Wencheng, E-mail: [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China)


    Graphical abstract: Highlights: > Sn-Bi eutectic powders were prepared by a high shear mechanical approach. This approach is a green one because no chemical reaction occurs in the process and the high boiling point solvent can be used repeatedly. > The melting point of the as-prepared powders is about 140 deg. C, which is in agreement with the low melting point solder for industrial applications. > The size of Sn-Bi eutectic powders can be controlled by addition of Poly(N-vinylpyrrolidone) (PVP) due to the adsorption. - Abstract: Fusible Sn-Bi eutectic alloy particles were synthesized from bulk Sn-Bi alloy via a high-shear mechanical approach. The morphology, composition, and structure of the as-prepared Sn-Bi alloy particles were characterized by XRD, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, differential scanning calorimetry, thermogravimetry, and Fourier-transform infrared spectroscopy. The particles were found to be spherical and consist of the tetragonal phase of tin as well as the rhombohedral phase of bismuth. In addition, there were large amounts of poly(N-vinylpyrrolidone) coated on the particles.

  14. [Study on adsorption behavior of nanosized barium-strontium titanate powder for lead ion in water using FAAS]. (United States)

    Zhang, Dong; Su, Hui-Dong; Gao, Hong


    Nanosized barium-stroutium titanate (BST) powder, a double salt sorbent, was prepared from BaCl2, SrCl2 and TiCl4 by using oxalate co-precipitate method, and characterized by using transmission electron microscope (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectrophotometer (FTIR). By means of determination with flame atomic absorption spectrometry (FAAS), the adsorption characteristic of lead on the BST powder w as investigated. The results showed that theforms of the BST powders are clubbed, highly pure perovskite, and the average particle diameter is 36 nm. Lead can be adsorbed strongly on nanosized BST. The adsorption capacity of BST nanoparticle towards lead was found to be 13 mg x g(-1) when the pH is 6.0, and 0.5 mol x L(-1) HNO3 is sufficient for complete elution. A new method for the determination of trace lead based on BST nanoparticle separation/preconcentration and FAAS determination was proposed. The detection limit of this method for lead ion is 11 microg x L(-1), and the relative standard deviation is 2.6%. The method has been applied to the determination of trace lead in water samples with satisfactory results.

  15. [Making tablets of powdered milk and the physical properties]. (United States)

    Shibata, Mitsuho; Otsubo, Kazumitsu; Nakane, Shota; Niwa, Toshiyuki; Danjo, Kazumi


    Compressed baby milk powder has proven to be very convenient for parents due to the ease with which it can be handled, and the fact that use of a measuring scoop is not necessary. The purpose of this study was to develop a compressed baby milk powder and analyze the resulting physical properties. The basic production process consisted of the following steps: 1) molding milk powder by low compression pressure, 2) humidification at 25°C·97%RH and 3) drying with use of a desiccant. No chemical additives were used for solidification; therefore the chemical composition of the compressed milk powder is identical to the base milk powder. The important properties of the compressed milk powder are both ready solubility and the strength of the solid. The compressed milk powder obtained at low pressure was too brittle for practical use, but the strength was increased by humidification followed by drying. During the humidification process, the powder particles located close to the surface of the compressed milk powder partially dissolve resulting in bridging structures between the particles, leading to an increase in strength. Both specific surface area and the volume ratio of the compressed milk powder decreased. Testing showed that caking between the particles occurred following humidification, and that the volume of caking affected the ease with which the compressed milk powder dissolves in water.

  16. Experimental observations of dry powder inhaler dose fluidisation. (United States)

    Tuley, Rob; Shrimpton, John; Jones, Matthew D; Price, Rob; Palmer, Mark; Prime, Dave


    Dry powder inhalers (DPIs) are widely used to deliver respiratory medication as a fine powder. This study investigates the physical mechanism of DPI operation, assessing the effects of geometry, inhalation and powder type on dose fluidisation. Patient inhalation through an idealised DPI was simulated as a linearly increasing pressure drop across three powder dose reservoir geometries permitting an analysis of shear and normal forces on dose evacuation. Pressure drop gradients of 3.3, 10 and 30 kPa s(-1)were applied to four powder types (glass, aluminium, and lactose 6 and 16% fines) and high speed video of each powder dose fluidisation was recorded and quantitatively analysed. Two distinct mechanisms are identified, labelled 'fracture' and 'erosion'. 'Fracture' mode occurs when the initial evacuation occurs in several large agglomerates whilst 'erosion' mode occurs gradually, with successive layers being evacuated by the high speed gas flow at the bed/gas interface. The mechanism depends on the powder type, and is independent of the reservoir geometries or pressure drop gradients tested. Both lactose powders exhibit fracture characteristics, while aluminium and glass powders fluidise as an erosion. Further analysis of the four powder types by an annular shear cell showed that the fluidisation mechanism cannot be predicted using bulk powder properties.

  17. Whey protein/polysaccharide-stabilized oil powders for topical application-release and transdermal delivery of salicylic acid from oil powders compared to redispersed powders. (United States)

    Kotzé, Magdalena; Otto, Anja; Jordaan, Anine; du Plessis, Jeanetta


    Oil-in-water (o/w) emulsions are commonly converted into solid-like powders in order to improve their physical and chemical stabilities. The aim of this study was to investigate whether whey protein/polysaccharide-stabilized o/w emulsions could be converted into stable oil powders by means of freeze-drying. Moreover, during this study, the effects of pH and polymer type on release and trans(dermal) delivery of salicylic acid, a model drug, from these oil powders were investigated and compared to those of the respective template emulsions and redispersed oil powders. Physical characterization of the various formulations was performed, such as droplet size analysis and oil leakage, and relationships drawn with regards to release and trans(dermal) delivery. The experimental outcomes revealed that the oil powders could be redispersed in water without changing the release characteristics of salicylic acid. pH and polymer type affected the release of salicylic acid from the oil powders, template emulsions, and redispersed powders similarly. Contrary, the transdermal delivery from the oil powders and from their respective redispersed oil powders was differently affected by pH and polymer type. It was hypothesized that the release had been influenced by the electrostatic interactions between salicylic acid and emulsifiers, whereas the transdermal performance could have been determined by the particle or aggregate sizes of the formulations.

  18. Properties of a epoxy-based powder coating containing modified montmorillonite with cerium; Propriedades de uma tinta em po base epoxi com adicao de montmorilonita modificada com cerio

    Energy Technology Data Exchange (ETDEWEB)

    Beux, A.R.D.; Piazza, D.; Zattera, A.J., E-mail: [Universidade de Caxias do Sul (CCET/UCS), RS (Brazil). Laboratorio de Polimeros; Ferreira, C.A. [Universidade Federal do Rio Grande do Sul (PPGEM/UFRGS), RS (Brazil). Laboratorio de Materiais Polimericos; Scienza, L.C. [Universidade de Caxias do Sul (CCET/UCS), RS (Brazil). Laboratorio de Protecao Superficial e Corrosao


    Organic coatings are widely used to prevent corrosion in metal structures. The incorporation of nanofiller the polymer matrix in order to obtain polymer nanocomposites has been arousing scientific and technological interest, because it provides significant improvements when incorporated into pure polymeric materials or conventional composites. In the present study were been developed epoxy-based powder coating with addition of different concentrations (2, 4 and 8% (w / w)) of the montmorillonite type Cloisite® 15A modified with cerium in the melt state on a double-screw extruder co-rotating. The coatings were characterized by average particle size, time (gel time) gel, X-ray diffraction (XRD), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). Coatings with intercalated structure was observed in the XRD analysis and confirmed by SEM to the observe an increase in the concentration of tactoids an increased filler content. (author)

  19. Bimodal metal micro-nanopowders for powder injection molding (United States)

    Pervikov, Aleksandr; Rodkevich, Nikolay; Glazkova, Elena; Lerner, Marat


    The paper studies a bimodal metal powder composition designed to prepare feedstock for powder injection molding, as well as microstructure and porosity of sintered pats. Two kinds of metal powder compositions are used, in particular, a mixture of micro- and nanopowders and a bimodal powder prepared with dispersion of steel wire. The feedstock is prepared by mixing a bimodal metal powder composition with acetylacetone and paraffin wax. The microstructure of the debound parts is observed by scanning electron microscopy. The sintered parts are characterized by density measurements and metallographic analysis. The technique of the metal powder composition proves to affect the characteristics of sintered parts. Nanoparticles are shown in the interstitial spaces among the microparticles upon mixing micro- and nanopowders, but the regular distribution of nanoparticles on the surface of microparticles is observed in the bimodal powder providing the reduction of the porosity of sintered parts and increasing the density to the proper density of steel.

  20. Capabilities and limitations of using powder rheology and permeability to predict dry powder inhaler performance. (United States)

    Cordts, Eike; Steckel, Hartwig


    Dry powder inhalers play a major role in today's treatment of various respiratory diseases. A lot of effort has been put into the optimization of a device and the appropriate formulation regarding its local lung deposition. However, the complexity and interactions of different factors governing powder dispersion and, therefore, its inhalable fraction challenge research groups around the world. In the current work, binary lactose blends and adhesive ternary powder mixtures containing additional budesonide fines were produced and analyzed with dispersion measurements on the one hand and permeability and aeration measurements conducted with a powder rheometer on the other hand. By comparing the results of the bulk property and dispersion tests, it was expected to gain a better understanding about the effect of excipient fines addition to an adhesive powder mixture. It could be observed that with permeability testing it was possible to clearly differentiate between different amounts of fines within mixtures. However, no correlation between permeability or aeration test values and drug fine particle fraction could be determined for the observed range. Nevertheless, the use of different characterization techniques led to a clearer understanding about the influence of fines addition to an adhesive mixture. It could be demonstrated that after the surface of carrier crystals had been fully saturated, drug particles got incorporated in more stable fines' agglomerates, which resulted in a decrease in fine particle fraction upon dispersion. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Powder dispersion mechanisms within a dry powder inhaler using microscale particle image velocimetry. (United States)

    Kou, Xiang; Wereley, Steven T; Heng, Paul W S; Chan, Lai Wah; Carvajal, M Teresa


    The goal of this work was to evaluate the ability of Particle Image Velocimetry (PIV) to visually assess dry powder dispersion within an inhaler. Herein, the study reports particle movement characterization of entrained low-micron particles within an inhaler to further scheme of potential mechanisms. Carrier based DPI formulations were prepared and placed in a transparent model Rotahaler(®) chamber for the aerosolization experiments. Then using the PIV, a high-speed camera, the dried powder dispersion was directly observed and analyzed for all, neat, binary and ternary systems. Powder dispersion mechanisms proposed include drag force, impact with obstacle and particle-particle collision; these different mechanisms depended on the powder flow properties. A revised ratio of aerodynamic response time (τA) to the mean time between collisions (τC) was found to be 6.8 indicating that particle collisions were of strong influence to particle dispersion. With image analysis techniques, visualization of particle flow pattern and collision regions was possible; suggesting that the various mechanisms proposed did govern the powder dispersion. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Combined XRD and XANES studies of a Re-promoted Co/γ-Al2O3 catalyst at Fischer–Tropsch synthesis conditions

    DEFF Research Database (Denmark)

    Rønning, Magnus; Tsakoumis, Nikolaos E.; Voronov, Alexey


    A cobalt based Fischer–Tropsch catalyst was studied during the initial stages of the reaction at industrially relevant conditions. The catalyst consists of 20wt% cobalt supported on γ-Al2O3 and promoted by 1wt% of rhenium. X-ray diffraction (XRD) in combination with X-ray absorption near edge str...

  3. XRD, DRS, and SEM stundies of the effects of metal dopants (Pt and Au) on the structural and optical properties of TiO2

    CSIR Research Space (South Africa)

    Moloantoa, JR


    Full Text Available Au and Pt doped TiO2 nanocrystlas were prepared using the sol gel method. Diffuse Reflectance Spectroscopy (DRS) was used to study the characteristics of these precious metals and X-ray diffraction (XRD) with calculated lattice parameters was used...

  4. Combining µXANES and µXRD mapping to analyse the heterogeneity in calcium carbonate granules excreted by the earthworm Lumbricus terrestris

    Energy Technology Data Exchange (ETDEWEB)

    Brinza, Loredana [Diamond Light Source, Harwell Campus, Didcot, Oxon OX11 0DE (United Kingdom); Schofield, Paul F. [Natural History Museum, Cromwell Road, London SW7 5BD (United Kingdom); Hodson, Mark E. [University of York, York YO10 5DD (United Kingdom); Weller, Sophie [University of Oxford, South Parks Road, Oxford OX1 3QR (United Kingdom); Ignatyev, Konstantin; Geraki, Kalotina; Quinn, Paul D.; Mosselmans, J. Frederick W., E-mail: [Diamond Light Source, Harwell Campus, Didcot, Oxon OX11 0DE (United Kingdom)


    A new experimental set-up enabling microfocus fluorescence XANES mapping and microfocus XRD mapping on the same sample at beamline I18 at Diamond Light Source is described. To demonstrate this set-up the heterogeneous mineralogy in calcium carbonate granules excreted by the earthworm Lumbricus terrestris has been analysed. Data analysis methods have been developed which enable µXRD and µXANES two-dimensional maps to be compared. The use of fluorescence full spectral micro-X-ray absorption near-edge structure (µXANES) mapping is becoming more widespread in the hard energy regime. This experimental method using the Ca K-edge combined with micro-X-ray diffraction (µXRD) mapping of the same sample has been enabled on beamline I18 at Diamond Light Source. This combined approach has been used to probe both long- and short-range order in calcium carbonate granules produced by the earthworm Lumbricus terrestris. In granules produced by earthworms cultured in a control artificial soil, calcite and vaterite are observed in the granules. However, granules produced by earthworms cultivated in the same artificial soil amended with 500 p.p.m. Mg also contain an aragonite. The two techniques, µXRD and µXANES, probe different sample volumes but there is good agreement in the phase maps produced.

  5. Ternary ceramic thermal spraying powder and method of manufacturing thermal sprayed coating using said powder

    Energy Technology Data Exchange (ETDEWEB)

    Vogli, Evelina; Sherman, Andrew J.; Glasgow, Curtis P.


    The invention describes a method for producing ternary and binary ceramic powders and their thermal spraying capable of manufacturing thermal sprayed coatings with superior properties. Powder contain at least 30% by weight ternary ceramic, at least 20% by weight binary molybdenum borides, at least one of the binary borides of Cr, Fe, Ni, W and Co and a maximum of 10% by weight of nano and submicro-sized boron nitride. The primary crystal phase of the manufactured thermal sprayed coatings from these powders is a ternary ceramic, while the secondary phases are binary ceramics. The coatings have extremely high resistance against corrosion of molten metal, extremely thermal shock resistance and superior tribological properties at low and at high temperatures.


    Directory of Open Access Journals (Sweden)

    Jaroslav Topič


    Full Text Available Recycled concrete powder (RCP mostly consisting of cement paste could be reused as partial cement replacement. The aim of this paper is to compare hydration and mechanical properties of RCP and two types of silica sand powder (SSP. Comparison of those materials combined with cement can highlight the binder properties of recycled concrete powder. Using of two types of SSP also show an influence of their fines on hydration process and mechanical properties. Particle size analysis and calorimetric measurement were carried out and mechanical properties such as bulk density, dynamic Young’s modulus and compression strength were examine. Calorimetric measurement proves the presence of exposed non-hydrated particles in RCP that can react again. However lower density of old cement paste in RCP overweight the mentioned potential of RCP and mechanical properties are decreasing compared with reference cement paste and cement paste SSP.

  7. Mössbauer and XRD characterization of the effect of heat treatment and the tribological test on the physical and mechanical properties of a Fe-Mn-Al-C alloy (United States)

    Ramos, J.; Piamba, J. F.; Sanchez, H.; Pérez Alcazar, G. A.


    In this study, a Fe-29.0Mn-6.0Al-0.9C-1.8Mo-1.6Si-0.4Cu (Wt. %) alloy was prepared in an induction furnace. The as-cast sample was submitted to homogenization at 1050 °C over 8 hours, which was followed by quenching, and an aging heat treatment at 500 °C for 12 h. Wear tests were performed by using a Pin on Disk Tribometer (ASTM G99) at room temperature to evaluate the mass loss. Optical Microscopy, X-Ray Diffraction, and Transmission Mossbauer Spectroscopy were used to characterize the microstructure and structural properties of the samples. The obtained microstructure of the heat-treated samples was of the austenitic type, and their XRD patterns were refined with the lines of the austenite, martensite, galaxite, and FeO structures. Mössbauer spectra of powders, obtained from the surface of the samples, showed the presence of a broad doublet, which corresponded to the disordered austenite; and a small hyperfine magnetic field distribution associated with the disordered and ferromagnetic martensite. After the tribology test, the surface of the sample was examined, and it was obderved that the austenite, martensite, and galaxite phases were present. The martensite quantity increased and, those of galaxite and austenite decreased, but that of austenite appeared to have larger lattice parameter. The decrease in the galaxite content was a direct consequence of the wear test, which removed matter from the sample surface. The appearance of additional martensite was due to the transformation of the austenite by mechanical work. The additional presence of a new austenite with a bigger lattice parameter and of the Fe oxide was the consequence of the heating process of the sample during the tribological test. The Mossbauer spectrum of this sample confirms the increase of the martensite content. The mechanical properties increased with the heat treatment.

  8. Synthesis, spectroscopic, antimicrobial, XRD, fluorescence of new Ni(II), Cd(II), Hg(II) and U(VI) complexes with 1-(2-furylmethylene)-N-(3-phenylallylidene)methanamine Schiff base (United States)

    El-Wahab, Zeinab H. Abd; Ali, Omyma A. M.; Ismail, Basma A.


    The 1:1 condensation of 2-furfurylamine and cinnamaldehyde under template condition gives the Schiff base ligand 1-(2-furylmethylene)-N-(3-phenylallylidene)methanamine (L). The reaction of the ligand with Ni(II), Cd(II), Hg(II) and U(VI) ions gives a series of novel complexes formulated as [NiLCl(H2O)]Cl·1½H2O, [CdL2(H2O)2]·2NO3·½H2O, [HgL2Cl2] and [UO2L3]·2NO3·H2O. The stoichiometry of the complexes was 1:1 for Ni(II), 1:2 for both Cd(II) and Hg(II) and 1:3 (M:L) for U(VI) complexes. The molar conductance of the complexes lies in the range of 135-250 Ω-1mol-1cm2 indicating their electrolytic behavior except Hg(II) complex. Electronic spectra and magnetic moments suggested varieties of geometries around the central metal atoms. The emission spectra of these complexes indicate the luminescence characteristics of the complexes. The X-ray diffraction (XRD) patterns of Schiff base and its complexes were investigated in powder forms. Thermodynamic parameters were computed from the thermal data using Coats and Redfern method. Structural optimization of the ligand and its Ni(II), Cd(II) and Hg(II) complexes was computed using the density functional theory (DFT), where the B3LYP functional was employed. The synthesized complexes exhibited higher antimicrobial activity than its free Schiff base ligand.

  9. Formation of Nanosized Lamellas of a Hardening Intermetallic Phase in the Powder Ni-based Coating Deposited by Microplasma Spraying on Steel Substrates (United States)

    Alontseva, D.; Ghassemieh, E.; Russakova, A.; Dzhes, A.; Prokhorenkova, N.


    This paper presents new results of studying the structure-phase compositions of Ni-based powder coating, deposited by Microplasma Spraying onto steel substrate by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction (XRD). It is shown that we have managed to obtain the predicted specific structure with nanosized lamellas of intermetallic phases due to the appropriate proper selection of modes of additional microplasma processing. As a result, the microhardness of the coating has been increased by 1.25 times.

  10. Influence of chemistry synthesis temperature of the Panic deposited on PET and powder; Influencia da temperatura de sintese quimica da PANI depositada em PET e na forma de po

    Energy Technology Data Exchange (ETDEWEB)

    Paschoalin, Rafaella T.; Steffens, Clarice [Universidade Federal de Sao Carlos - UFSCar, Sao Carlos, SP (Brazil); Manzoli, Alexandra; Paris, Elaine C.; Herrmann Junior, Paulo S.P., E-mail: [Laboratorio nacional de nanotecnologia para o agronegocio/Embrapa Instrumentacao Agropecuaria, Sao Carlos, SP (Brazil)


    This work was evaluated the influence of synthesis temperature to obtain poly aniline (PANI) by in-situ polymerization on a substrate of poly (terephthalate) (PET). The residual mass of these syntheses was dried under vacuum obtaining a powder of PANI different for each temperature investigated. Thin films of PANI / PET and PANI powder were characterized by the techniques of atomic force microscopy (AFM), X-Ray Diffraction (XRD) UV-Vis- NIR spectroscopy and four-point probe technique. The results of UV-Vis-NIR show the deposition of PANI in the emeraldine oxidation state and show an increase of polymer layer deposited with decreasing synthesis temperature. By means of XRD technique it shows that the polymer was deposited in crystalline form. The results of conductivity of PANI / PET and PANI powder as a function of synthesis temperature showed opposite results, thus the conductivity of PANI deposited on the substrate decreased with increasing temperature and the polymer in powder form increased. (author)

  11. Developing Characterization Procedures for Qualifying both Novel Selective Laser Sintering Polymer Powders and Recycled Powders

    Energy Technology Data Exchange (ETDEWEB)

    Bajric, Sendin [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)


    Selective laser sintering (SLS) is an additive technique which is showing great promise over conventional manufacturing techniques. SLS requires certain key material properties for a polymer powder to be successfully processed into an end-use part, and therefore limited selection of materials are available. Furthermore, there has been evidence of a powder’s quality deteriorating following each SLS processing cycle. The current investigation serves to build a path forward in identifying new SLS powder materials by developing characterization procedures for identifying key material properties as well as for detecting changes in a powder’s quality. Thermogravimetric analyses, differential scanning calorimetry, and bulk density measurements were investigated.

  12. Powder metallurgy and mechanical alloying effects on the formation of thermally induced martensite in an FeMnSiCrNi SMA

    Directory of Open Access Journals (Sweden)

    Pricop Bogdan


    Full Text Available By ingot metallurgy (IM, melting, alloying and casting, powder metallurgy (PM, using as-blended elemental powders and mechanical alloying (MA of 50 % of particle volume, three types of FeMnSiCrNi shape memory alloy (SMA specimens were fabricated, respectively. After specimen thickness reduction by hot rolling, solution treatments were applied, at 973 and 1273 K, to thermally induce martensite. The resulting specimens were analysed by X-ray diffraction (XRD and scanning electron microscopy (SEM, in order to reveal the presence of ε (hexagonal close-packed, hcp and α’ (body centred cubic, bcc thermally induced martensites. The reversion of thermally induced martensites, to γ (face centred cubic, fcc austenite, during heating, was confirmed by dynamic mechanical analysis (DMA, which emphasized marked increases of storage modulus and obvious internal friction maxima on DMA thermograms. The results proved that the increase of porosity degree, after PM processing, increased internal friction, while MA enhanced crystallinity degree.

  13. Production of high-coercivity materials based on BaFe12O19 by crystallization of plasma-sputtered powders (United States)

    Lepeshev, A. A.; Karpov, I. V.; Uschakov, A. V.


    Ferrite powders BaFe12O19 were studied in the present work after plasma heating and rapid quenching in differentenvironment: in air, in water and on the copper disk. X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), vibration magnetometry (VSM) and Mossbauer spectroscopy (NGR) showed that the powder produced after quenching on the copper disk was in amorphous-crystalline state. The correlation between the annealing temperature and the value of magnetic parameters (coercive field and saturation magnetization) was established. Annealing at 1200 K for 2 h increases the coercive force up to 6.3 kOe. The processes of crystallization from the amorphous phase, that improve the magnetic properties of barium ferrite, are discussed. Highlights We studied the barium ferrite powdersafter plasma heating and rapid quenching. We studied the processes of crystallization from the amorphous phase. We studied theprocesses ofthermal annealing for the barium ferrite.

  14. Structural behavior and microstructural hard metal sintered at 1350 deg C from the powder of nanometer WC with 10 wt% Co

    Energy Technology Data Exchange (ETDEWEB)

    Batista, A.C.; Perpetuo, G.J.; Leocadio, R.R.V., E-mail: [Rede Tematica de Engenharia de Materiais (REDEMAT), Ouro Preto, Minas Gerais (Brazil); Oliveira, H.C.P. de [Instituto Superior Tecnico (IST), Lisboa (Portugal). Departamento de Materiais


    The hard metal (WC-10%Co), processed via powder metallurgy, using powder of nanometer WC, were characterized from the point of view to the microstructural and structural techniques, X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray (EDS) for mapping and punctual. To analyze the behavior of hard metal after the sintering process performed in resistive furnace at 1350°C for 1 hour under vacuum of 10-2 mbar, the analysis identified the formation of WC grains, the pore distribution and behavior and evolution of the phases WC and Co, generating phases η (Co{sub 3}W{sub 3}C and Co{sub 6}W{sub 6}C). (author)

  15. Obtaining beta phase in Ti through processing in high energy mill powders of Ti and Nb; Obtencao de fase beta no Ti atraves de processamento em moinho de alta energia de pos de Ti e Nb

    Energy Technology Data Exchange (ETDEWEB)

    Milanez, Mateus; Ferretto, Aline; Rocha, Marcio Roberto da; Arnt, Angela Coelho [Universidade do Extremo Sul Catarinense (UNESC), Criciuma, SC (Brazil). Departamento de Engenharia de Materiais; Milanez, Alexandre [Faculdade SATC (FASATC), Criciuma, SC (Brazil). Departamento de Engenharia Mecanica; Schaeffer, Lirio [Universidade Federal do Rio Grande do Sul (LdTM/UFRGS), RS (Brazil). Lab. de Transformacao Mecanica


    An orthopedic implant, ideal, must meet the requirements of biocompatibility, have good mechanical properties among others. Titanium and Niobium exhibit biocompatibility and the β-Ti phase relationships have the highest strength / weight among all titanium alloys, presenting lower values of elastic modulus. The alloy has mechanically produced specific microstructural characteristics and improved mechanical properties compared with conventional powder metallurgy. In this study, a titanium alloy with different additions of niobium was used. The metal powders were mixed via mechanical alloy in high energy mill (attritor). The powder samples were analyzed by X-ray diffraction (X-RD) and property held by adhesive wear testing with a Pin-on-Disk. The present study revealed that through the high-energy milling is possible the atomic interaction between Ti and Nb particles and the mechanical properties are affected by the concentration of Nb. (author)

  16. Large Bore Powder Gun Qualification (U)

    Energy Technology Data Exchange (ETDEWEB)

    Rabern, Donald A. [Los Alamos National Laboratory; Valdiviez, Robert [Los Alamos National Laboratory


    A Large Bore Powder Gun (LBPG) is being designed to enable experimentalists to characterize material behavior outside the capabilities of the NNSS JASPER and LANL TA-55 PF-4 guns. The combination of these three guns will create a capability to conduct impact experiments over a wide range of pressures and shock profiles. The Large Bore Powder Gun will be fielded at the Nevada National Security Site (NNSS) U1a Complex. The Complex is nearly 1000 ft below ground with dedicated drifts for testing, instrumentation, and post-shot entombment. To ensure the reliability, safety, and performance of the LBPG, a qualification plan has been established and documented here. Requirements for the LBPG have been established and documented in WE-14-TR-0065 U A, Large Bore Powder Gun Customer Requirements. The document includes the requirements for the physics experiments, the gun and confinement systems, and operations at NNSS. A detailed description of the requirements is established in that document and is referred to and quoted throughout this document. Two Gun and Confinement Systems will be fielded. The Prototype Gun will be used primarily to characterize the gun and confinement performance and be the primary platform for qualification actions. This gun will also be used to investigate and qualify target and diagnostic modifications through the life of the program (U1a.104 Drift). An identical gun, the Physics Gun, will be fielded for confirmatory and Pu experiments (U1a.102D Drift). Both guns will be qualified for operation. The Gun and Confinement System design will be qualified through analysis, inspection, and testing using the Prototype Gun for the majority of process. The Physics Gun will be qualified through inspection and a limited number of qualification tests to ensure performance and behavior equivalent to the Prototype gun. Figure 1.1 shows the partial configuration of U1a and the locations of the Prototype and Physics Gun/Confinement Systems.

  17. Powder processing of hybrid titanium neural electrodes (United States)

    Lopez, Jose Luis, Jr.

    A preliminary investigation into the powder production of a novel hybrid titanium neural electrode for EEG is presented. The rheological behavior of titanium powder suspensions using sodium alginate as a dispersant are examined for optimal slip casting conditions. Electrodes were slip cast and sintered at 950°C for 1 hr, 1000°C for 1, 3, and 6 hrs, and 1050°C for 1 hr. Residual porosities from sintering are characterized using Archimedes' technique and image analysis. The pore network is gel impregnated by submerging the electrodes in electrically conductive gel and placing them in a chamber under vacuum. Gel evaporation of the impregnated electrodes is examined. Electrodes are characterized in the dry and gelled states using impedance spectrometry and compared to a standard silver- silver chloride electrode. Power spectral densities for the sensors in the dry and gelled state are also compared. Residual porosities for the sintered specimens were between 50.59% and 44.81%. Gel evaporation tests show most of the impregnated gel evaporating within 20 min of exposure to atmospheric conditions with prolonged evaporation times for electrodes with higher impregnated gel mass. Impedance measurements of the produced electrodes indicate the low impedance of the hybrid electrodes are due to the increased contact area of the porous electrode. Power spectral densities of the titanium electrode behave similar to a standard silver-silver chloride electrode. Tests suggest the powder processed hybrid titanium electrode's performance is better than current dry contact electrodes and comparable to standard gelled silver-silver chloride electrodes.

  18. Ampicillin Trihydrate from Synchrotron Powder Diffraction Data

    Energy Technology Data Exchange (ETDEWEB)

    Burley,J.; van de Streek, J.; Stephens, P.


    The crystal structure of ampicillin trihydrate {l_brace}systematic name: 6-[D(-)-{alpha}-aminophenylacetamido]penicillanic acid trihydrate{r_brace}, C{sub 16}H{sub 19}N{sub 3}O{sub 4}S{center_dot}3H{sub 2}O, a broad-spectrum {beta}-lactam antibiotic of the aminopenicillin type, has been determined from synchrotron X-ray powder diffraction data. The three water molecules form an infinite hydrogen-bonded chain through the crystal structure, with hydrogen bonds to the NH{sub 3}{sup +}, COO{sup -}, C{double_bond}O and NH groups of the ampicillin molecules.

  19. Conversion of Nitrocellulose to Smokeless Powder (United States)


    Z.Ges.Schless-Sprengstoffw. 30,36l-1*-(l935) New Nitrocellulose Powders and Explosives g. S.ölückmann. Kunststoffe 25:25-29,120-23(1935) The Viscosity and... Kunststoffe 2^,32-5^(193^-) New Solvents and Plasticizers for Nitrocellulose 22. T.Tomonarl. J.Soc.Chem.Ind..Japan 37,Supp.775-7(1934) Classification of...L.Rutsteln. Kunststoffe 11,25-23(1921) The Viscosity of Nitrocellulose R.Robertson. Trans.Far.3oc. 16,66-71 (1921) Nitrocellulose F.Soroxton

  20. Surface free energy characterization of powders (United States)

    Yildirim, Ismail


    Microcalorimetric measurements and contact angle measurements were conducted to study the surface chemistry of powdered minerals. The contact angle measurements were conducted on both flat and powdered talc samples, and the results were used to determine the surface free energy components using Van Oss-Chaudhury-Good (OCG) equation. It was found that the surface hydrophobicity of talc increases with decreasing particle size. At the same time, both the Lifshitz-van der Waals (gammasLW) and the Lewis acid-base (gammas AB) components (and, hence, the total surface free energy (gammas)) decrease with decreasing particle size. Heats of immersion measurements were conducted using a flow microcalorimeter on a number of powdered talc samples. The results were then used to calculate the contact angles using a rigorous thermodynamic relation. The measured heat of immersion values in water and calculated contact angles showed that the surface hydrophobicity of talc samples increase with decreasing particle size, which agrees with the direct contact angle measurements. The microcalorimetric and direct contact angle measurements showed that acid-base interactions play a crucial role in the interaction between talc and liquid. Using the Van Oss-Chaudhury-Good's surface free energy components model, various talc powders were characterized in terms of their acidic and basic properties. It was found that the magnitude of the Lewis electron donor, gamma s-, and the Lewis electron acceptor, gamma s+, components of surface free energy is directly related to the particle size. The heats of adsorption of butanol on various talc samples from n-heptane solution were also determined using a flow microcalorimeter. It was found that the total surface free energy (gammas) at the basal plane surface of talc is much lower than the total surface free energy at the edge surface. Furthermore, the effects of the surface free energies of solids during separation from each other by flotation and

  1. [Easyhaler--ideal dry powder inhaler]. (United States)

    Andrzej, Emeryk; Małgorzata, Bartkowiak-Emeryk


    Dry powder inhalers (DPI) differ among each other in many technical aspects, size and value of lung deposition as well as clinical efficacy of inhaled drugs. Easyhaler is a reservoir, multi-dose, high-resistance DPI and it is easy to operate. The device needs low inspiratory flows which are possible to achieve even by asthmatic children over 5-year-old and emitted dose and fine particle fraction are practically stable within the range of optimal inspiratory flows. Currently budesonid, formoterol and salbutamol are available in Easyhaler device form. Easyhaler is accepted by majority of patients with asthma or COPD.

  2. Powder neutron diffractometers HRPT and DMCG

    Energy Technology Data Exchange (ETDEWEB)

    Fischer, P.; Doenni, A.; Staub, U.; Zolliker, M. [Lab. for Neutron Scattering ETH Zurich, Zurich (Switzerland) and Paul Scherrer Institute, Villigen (Switzerland)


    Basic properties and applications of SINQ powder neutron diffractometers are described. For optimum use of the continuous neutron beams these instruments are equipped with position sensitive detectors, and both high-intensity and high-resolution modes of operation are possible. HRPT attaining resolutions {delta}d/d{<=}10{sup -3}, d=lattice spacing, at a thermal neutron channel of the target station and DMCG at a cold neutron guide coated with m=2 supermirrors, are complementary concerning the applications: the former will be mainly used for structural studies and the latter to investigate magnetic ordering phenomena. (author) figs., tabs., refs.

  3. Characterization of calcium phosphate powders originating from Phyllacanthus imperialis and Trochidae Infundibulum concavus marine shells

    Energy Technology Data Exchange (ETDEWEB)

    Tămăşan, M., E-mail: [Babeş-Bolyai University, Faculty of Physics and Interdisciplinary Research Institute on Bio-Nano-Sciences, Cluj-Napoca (Romania); Ozyegin, L.S. [Marmara University, Istanbul (Turkey); Oktar, F.N. [Marmara University, Faculty of Engineering, Department of Bioengineering, Göztepe Campus, Kadıköy 34722, Istanbul (Turkey); Marmara University, School of Health Related Professions, Department of Medical Imaging Technics, Haydarpaşa Campus, Tıbbiye Street, 49, Üsküdar 34668, Istanbul (Turkey); Marmara University, Nanotechnology and Biomaterials Application and Research Centre, Göztepe Campus, Kadıköy 34722, Istanbul (Turkey); Simon, V. [Babeş-Bolyai University, Faculty of Physics and Interdisciplinary Research Institute on Bio-Nano-Sciences, Cluj-Napoca (Romania)


    The study reports the preparation and characterization of powders consisting of the different phases of calcium phosphates that were obtained from the naturally derived raw materials of sea-shell origins reacted with H{sub 3}PO{sub 4}. Species of sea origin, such as corals and nacres, attracted a special interest in bone tissue engineering area. Nacre shells are built up of calcium carbonate in aragonite form crystallized in an organic matrix. In this work two natural marine origin materials (shells of echinoderm Sputnik sea urchin — Phyllacanthus imperialis and Trochidae Infundibulum concavus mollusk) were involved in the developing powders of calcium phosphate based biomaterials (as raw materials for bone-scaffolds) by hotplate and ultrasound methods. Thermal analyses of the as-prepared materials were made for an assessment of the thermal behavior and heat treatment temperatures. Samples from both sea shells each of them prepared by the above mentioned methods were subjected to thermal treatments at 450 °C and 850 °C in order to evaluate the crystalline transformations of the calcium phosphate structures in the heating process. By X-ray diffraction analyses various calcium phosphate phases were identified. In Sputnik sea urchins originated samples were found predominantly brushite and calcite as a small secondary phase, while in Trochidae I. concavus samples mainly monetite and HA phases were identified. Thermal treatment at 850 °C resulted flat-plate whitlockite crystals — β-MgTCP [(Ca, Mg){sub 3} (PO{sub 4}){sub 2}] for both samples regardless the preparation method (ultrasound or hotplate) or the targeted Ca/P molar ratio according with XRD patterns. Scanning electron microscopy and Fourier transformed infrared spectroscopy were involved more in the characterization of these materials and the good correlations of the results of these methods were made. - Highlights: ► Calcium phosphate powders are obtained from the crushed shells of 2

  4. Preparation and characterization of Cu and Zn modified nickel manganite NTC powders and thick film thermistors

    Energy Technology Data Exchange (ETDEWEB)

    Aleksic, O.S. [Institute for Multidisciplinary Research, University of Belgrade, 11000 Beograd (Serbia); Nikolic, M.V., E-mail: [Institute for Multidisciplinary Research, University of Belgrade, 11000 Beograd (Serbia); Lukovic, M.D.; Nikolic, N. [Institute for Multidisciplinary Research, University of Belgrade, 11000 Beograd (Serbia); Radojcic, B.M. [Faculty of Electronic Engineering, University of Belgrade, 11000 Beograd (Serbia); Radovanovic, M. [Faculty of Technical Sciences, University of Novi Sad, Novi Sad (Serbia); Djuric, Z. [Institute of Technical Sciences of SASA, 11000 Beograd (Serbia); Mitric, M. [The ' Vinca' Institute of Nuclear Science, Laboratory for Theoretical Physics of Condensed Matter, University of Belgrade (Serbia); Nikolic, P.M. [Institute of Technical Sciences of SASA, 11000 Beograd (Serbia)


    Highlights: Black-Right-Pointing-Pointer Simple ball milling/thermal treatment procedure of starting oxide powders. Black-Right-Pointing-Pointer Good thermistor characteristics (thermal constant, activation energy). Black-Right-Pointing-Pointer Low resistivity drift obtained for Zn and Cu modified nickel manganite thermistors. Black-Right-Pointing-Pointer Candidates for temperature and heat loss sensor applications. - Abstract: A simple ball milling/thermal treatment procedure was applied to obtain fine thermistor powders. Three different powder compositions were analyzed-Cu{sub 0.2}Ni{sub 0.5}Zn{sub 1.0}Mn{sub 1.3}O{sub 4}, Cu{sub 0.25}Ni{sub 0.5}Zn{sub 1.0}Mn{sub 1.25}O{sub 4} and Cu{sub 0.4}Ni{sub 0.5}Mn{sub 2.1}O{sub 4}. XRD analysis showed that all three powder compositions had a cubic spinel structure. Correlation between the sintering temperature, structure and resulting electrical properties was analyzed on bulk samples. Thick film pastes were composed and segmented thick film thermistors were screen printed on alumina, dried and fired. SEM analysis revealed a typical dendrite structure with small grains and a developed surface area. Thick film sheet resistance was measured on a test matrix and the resistance decreased with increasing Cu content. The temperature dependence of sample resistance was measured in a climatic chamber enabling calculation of the material constant and activation energy. Aging of the obtained segmented thermistors was analyzed and the resistivity drift was 0.23% for the Cu{sub 0.2}Ni{sub 0.5}Zn{sub 1.0}Mn{sub 1.3}O{sub 4} NTC thick film thermistor confirming greater stability of thermistors containing Zn and Cu that in combination with the determined good thermistor characteristics make them good candidates for temperature and heat loss sensor applications.

  5. Effect of grinding time of synthesized gadolinium doped ceria (GDC10 powders on the performance of solid oxide fuel cell

    Directory of Open Access Journals (Sweden)

    Fatma Aydin


    Full Text Available Ceria-based materials are prospective electrolytes for low and intermediate temperature solid oxide fuel cells. In the present work, fully dense CeO2 ceramics doped with 10 mol% gadolinium (Gd0.1Ce0.9O1.95 were prepared with a sol–gel method and commercially purchased GDC10 electrolyte powders were processed. Particle sizes of synthesized electrolyte powders were minimized by ball-milling method. Grinding of the samples were performed in different times intervals (12 h, 15 h, 18 h, 20 h, 25 h, 30 h, 35 h, 40 h and 45 h. Then, these powders were prepared to obtain of solid oxide fuel cells (SOFCs. Performances of these cells having an active area of 1 cm2 were tested using a fuel cell test station that measured in different temperatures (650 and 700 °C. In the present study, gadolinium doped ceria (GDC10 synthesiszed powders were investigated by using XRD and SEM images. Performance values of synthesized GDC10's in different temperature were compared to by commercial GDC10. Commercial GDC10's performance at 650 °C were tested, and maximum current density of 0.413 W/cm2 and maximum current density of 0.949 A/cm2 were obtained. Commercial GDC10 at 650 °C has better result. However, synthesized GDC10's performance at 700 °C demonstrated better results than commercial GDC10's. The performance tests of samples which are 20 h mill showed that they have the maximum power density of was obtained as 0.480 W/cm2 and maximum current density of as 1.231 A/cm2.

  6. An Efficient Approach to Address Issues of Graphene Nanoplatelets (GNPs Incorporation in Aluminium Powders and Their Compaction Behaviour

    Directory of Open Access Journals (Sweden)

    Zeeshan Baig


    Full Text Available The exceptional potential of the graphene has not been yet fully translated into the Al matrix to achieve high-performance Al nanocomposite. This is due to some critical issues faced by graphene during its processing such as the dispersion uniformity, structure damage, compatibility/wettability, and low graphene embedding content in Al matrix. In the present work, a new integrative method was adopted and named as “solvent dispersion and ball milling” (SDBM to address the issues above efficiently in a single approach. This strategy involves effective graphene nanoplatelets (GNPs solvent dispersion via surfactant decoration and solution ball milling employed to polyvinyl alcohol (PVA coated Al with various GNPs content (0.5, 1 and 1.5 wt. %. Flaky Al powder morphology attained by optimizing ball milling parameters and used for further processing with GNPs. Detailed powders characterizations were conducted to investigate morphology, graphene dispersion, group functionalities by FTIR (Fourier transform infrared spectroscopy spectroscopy and crystallinity by powder XRD (X-ray diffractionanalysis. Compaction behaviour and spring back effect of the GNPs/Al powders was also investigated at different compaction pressure (300 to 600 Mpa and varying GNPs fractions. In response, green and sintered relative density (% along with effect on the hardness of the nanocomposites samples were examined. Conclusively, in comparison with the unreinforced Al, GNP/Al nanocomposite with 1.5 wt. % GNPs exhibited the highest hardness gives 62% maximum increase than pure Al validates the effectiveness of the approach produces high fraction uniformly dispersed GNPs in Al matrix.

  7. Structural, optical, and magnetic properties of Fe doped In{sub 2}O{sub 3} powders

    Energy Technology Data Exchange (ETDEWEB)

    Krishna, N. Sai [Thin Films Laboratory, School of Advanced Sciences, VIT University, Vellore 632 014, Tamilnadu (India); Kaleemulla, S., E-mail: [Thin Films Laboratory, School of Advanced Sciences, VIT University, Vellore 632 014, Tamilnadu (India); Amarendra, G. [Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102, Tamilnadu (India); UGC-DAE-CSR, Kalpakkam Node, Kokilamedu 603 104, Tamilnadu (India); Rao, N. Madhusudhana; Krishnamoorthi, C.; Kuppan, M.; Begam, M. Rigana [Thin Films Laboratory, School of Advanced Sciences, VIT University, Vellore 632 014, Tamilnadu (India); Reddy, D. Sreekantha [Department of Physics and Sungkyunkwan Advanced Institute of Nanotechnology (SAINT), Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Omkaram, I. [Department of Electronics and Radio Engineering, Kyung Hee University, Yongin-si, Gyeonggi-do 446-701 (Korea, Republic of)


    Highlights: • Synthesis of Fe doped In{sub 2}O{sub 3} powders using a solid state reaction. • Characterization of the samples using XRD, UV–vis-NIR, FT-IR, and VSM. • All Fe doped In{sub 2}O{sub 3} powders exhibited the cubic structure of In{sub 2}O{sub 3}. • All the Fe doped In{sub 2}O{sub 3} samples exhibited room temperature ferromagnetism. - Abstract: Iron doped indium oxide dilute magnetic semiconductor (In{sub 1−x}Fe{sub x}){sub 2}O{sub 3} (x = 0.00, 0.03, 0.05, and 0.07) powders were synthesized by standard solid state reaction method followed by vacuum annealing. The effect of Fe concentration on structural, optical, and magnetic properties of the (In{sub 1−x}Fe{sub x}){sub 2}O{sub 3} powders have been systematically studied. X-ray diffraction patterns confirmed the polycrystalline cubic structure of all the samples. An optical band gap increases from 3.12 eV to 3.16 eV while Fe concentration varying from 0.03 to 0.07. Magnetic studies reveal that virgin/undoped In{sub 2}O{sub 3} is diamagnetic. However, all the Fe-doped In{sub 2}O{sub 3} samples are ferromagnetic. The saturation magnetization (M{sub s}) of ferromagnetic (In{sub 1−x}Fe{sub x}){sub 2}O{sub 3} (x = 0.03, 0.05, and 0.07) samples increases from 11.56 memu/g to 148.64 memu/g with x = 0.03–0.07. The observed ferromagnetism in these samples was attributed to magnetic nature of the dopant (Fe) as well as defects created in the samples during vacuum annealing.

  8. Characterizing local Garden Croton (‘pokok puding’ leaf powder as low cost biomaterial for Chromium(VI uptake

    Directory of Open Access Journals (Sweden)

    Palsan Sannasi


    Full Text Available This paper reports the first ever characterization of the use of raw Garden Croton (locally known as ‘pokok puding’ leaf powder as low cost biomaterial for Cr(VI removal. Biosorption experiments were carried out at ambient temperature to study the effects of initial pH (1-7, contact time (15, 30, 45, 60 min, leaf powder’s particle size (≤ 150, 151-300, 301-500 μm, and initial Cr(VI concentrations (10, 20, 40, 60, 80 and 100 mg/L towards Cr(VI uptake. Optimum Cr(VI uptake was observed at pH 1 (2.41 mg/g and 2 (2.19 mg/g (p > 0.05. The leaf powder in the 151-300 μm size displayed better Cr(VI uptake up to 2.77 mg/g (77.78%; Co = 100 mg/L at pH 2, after 30 min (p < 0.05. Equilibrium metal uptake fitted best (R2 = 0.927 to the Freundlich isotherm model (Kf = 0.21 mg/g, n = 1.23 indicating biosorption onto a heterogeneous surface of active sites. Morphological and elemental analyses by SEM/EDX and FTIR confirmed Cr retention, and presence of active chemical moieties. Interestingly, XRD revealed that Cr was immobilized within the biomass leaf powder in both forms, i.e. hexavalent, Cr(VI as chromatite (CaCrO4 and trivalent Cr(III, as chromium(III oxide (Cr2O3. Overall findings support the feasibility of the leaf powder as potential biomaterial for water pollution abatement.

  9. 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: [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)


    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.

  10. Physical properties of yoghurt powder produced by spray drying. (United States)

    Koç, Banu; Sakin-Yılmazer, Melike; Kaymak-Ertekin, Figen; Balkır, Pınar


    The study is an extension of an optimization study, which was planned to determine the optimum spray drying conditions (the feed, outlet and inlet air temperatures) for producing yoghurt powder. The resulting yoghurt powder at each condition was subjected to the measurement of physical properties, moisture content, and reconstitution properties. All the reconstitution properties of yoghurt powders produced under 20 different spray drying conditions according to CCRD experimental design were affected by the drying outlet temperature only. Furthermore, the bulk (bulk and tapped densities, porosity, flowability, hygroscopicity and degree of caking) and particle properties (particle size distribution, particle density and morphology) of yoghurt powder obtained from optimum spray drying conditions were also determined. The bulk, tapped and particle densities of yoghurt powder were 538, 746 and 1177 kg/m(3), respectively. The mean diameter (D4.3) and the span value of yoghurt powder were 3.053 and 2.487 μm, respectively.


    Directory of Open Access Journals (Sweden)

    Valmikanathan Onbattuvelli


    Full Text Available Silicon carbide (SiC exhibits many functional properties that are relevant to applications in electronics, aerospace, defense and automotive industries. However, the successful translation of these properties into final applications lies in the net-shaping of ceramics into fully dense microstructures. Increasing the packing density of the starting powders is one effective route to achieve high sintered density and dimensional precision. The present paper presents an in-depth study on the effects of nanoparticle addition on the powder injection molding process (PIM of SiC powder-polymer mixtures. In particular, bimodal mixtures of nanoscale and sub-micrometer particles are found to have significantly increased powder packing characteristics (solids loading in the powder-polymer mixtures. The influence of nanoparticle addition on the multi-step PIM process is examined. The above results provide new perspectives which could impact a wide range of materials, powder processing techniques and applications.

  12. Production of functional pita bread using date seed powder. (United States)

    Platat, Carine; Habib, Hosam M; Hashim, Isameldin Bashir; Kamal, Hina; AlMaqbali, Fatima; Souka, Usama; Ibrahim, Wissam H


    Functional foods represent a novel approach to prevent diet-related diseases. Due to its excellent nutritional and antioxidant properties, date seed was used to develop functional pita bread. Flour was replaced by 5, 10, 15 and 20 % date seed powder. Regular and whole wheat pita breads were the references. Results clearly showed that date seed powder containing bread contained comparable dietary fibers levels as in whole wheat bread and higher levels of flavonoids and phenolics. Date seed powder containing breads were particularly rich in flavan-3-ols whereas reference breads did not contain any of them and only a limited amount of other phenolic compounds. They also exhibited a much higher antioxidant capacity. Additionally, compared to regular bread, acrylamide level was significantly lower in 5 % date seed powder containing bread, and lower in all date seed powder containing breads compared to whole wheat bread. Date seed powder supplemented bread appears as a promising functional ingredient to prevent chronic diseases.

  13. Transient liquid-phase bonding using coated metal powders

    Energy Technology Data Exchange (ETDEWEB)

    Zhuang, W.D.; Eagar, T.W. [Massachusetts Inst. of Tech., Cambridge, MA (United States). Dept. of Materials Science and Engineering


    Powder particles coated with a small amount of melting point depressant (MPD) reveal different sintering behavior in comparison to an uncoated powder mixture of the same composition. Interlayers consisting of the coated powder particles were used in the transient liquid-phase (TLP) bonding process. The coating material and the thickness of the deposit are important parameters that influence shrinkage. The amount of MPD was controlled such that the volume fraction of the liquid was very small but existed at all contacts, thus improving densification of the interlayer. Ni-20Cr and 304L stainless steel powders coated with Ni-10P were applied to join 304 stainless steels. Fully dense joints with mechanical properties comparable to those of the base metals were obtained with Ni-20Cr powder interlayers, whereas joints with 304L stainless steel powder interlayers showed inferior mechanical properties due to residual porosity in the joints.

  14. Preparation of nanosized non-oxide powders using diatomaceous earth

    Directory of Open Access Journals (Sweden)

    Šaponjić A.


    Full Text Available In this paper the nanosized non-oxide powders were prepared by carbothermal reduction and subsequent nitridation of diatomaceous earth which is a waste product from coal exploitation. Our scope was to investigate the potential use of diatomaceous earth as a main precursor for low-cost nanosized non-oxide powder preparation as well as to solve an environmental problem. The influence of carbon materials (carbonized sucrose, carbon cryogel and carbon black as a reducing agent on synthesis and properties of low-cost nanosized nonoxide powders was also studied. The powders were characterized by specific surface area, X-ray and SEM investigations. It was found that by using diatomaceous earth it is was possible to produce either a mixture of non-oxide powders (Si3N4/SiC or pure SiC powders depending on temperature.

  15. Quality changes of Antarctic krill powder during long term storage

    DEFF Research Database (Denmark)

    Nielsen, Nina Skall; Lu, Henna Fung Sieng; Bruheim, Inge


    Krill is a valuable sustainable resource of omega-3 fatty acids and protein, which may be processed into a krill powder for human consumption. The objective of this study was to investigate the stability of krill powder when stored for up to 12 months at room temperature. In addition, the effect......) is a shrimp-like marine crustacean. It is rich in omega-3 fatty acids, primarily bound in phospholipids in the sn-2 position of the molecule, making it highly bioavailable. Krill may be processed into powder also rich in protein and astaxanthin. Stability of krill powder, stored for up to 12 months at room...... and a concomitant decrease in antioxidants, tocopherol, and astaxanthin was observed. In addition, there was a minor decrease in phospholipids and n-3 fatty acids; however, storage at vacuum improved the oxidative stability of krill powder. Practical applications: For the use of krill powder in human nutrition...

  16. Ni Based Powder Reconditioning and Reuse for LMD Process (United States)

    Renderos, M.; Girot, F.; Lamikiz, A.; Torregaray, A.; Saintier, N.

    LMD is an additive manufacturing process based on the injection of metallic powder into a melt-pool created by a heat laser source on a substrate. One of the benefits of this technology is the reduction of the wasted material since it is a near-shape process. Moreover one of the main drawbacks is the relatively low efficiency of the trapped powder, which can be loss than 5% in some cases. The non-trapped powder represents a significant cost in the LMD process, since powder metal material is very expensive and usually is not reused. This article proposes a methodology of the reconditioning and posterior reuse of a nickel base powder commonly used in the aerospace industry, with the main objectives of cost saving, higher environmental cleanup and increase of the overall efficiency in the LMD process. The results are checked by the development of a prototype part built up from reused powder.

  17. Method for preparing metal powder, device for preparing metal powder, method for processing spent nuclear fuel (United States)

    Park, Jong-Hee [Clarendon Hills, IL


    A method for producing metal powder is provided the comprising supplying a molten bath containing a reducing agent, contacting a metal oxide with the molten bath for a time and at a temperature sufficient to reduce the metal in the metal oxide to elemental metal and produce free oxygen; and isolating the elemental metal from the molten bath.

  18. Risky business: pre-powdered gloves or powder-free gloves in the operating suite? (United States)

    Spicer, M; Richardson, M


    Two of the emerging issues for the health-care sector in the 1990s are occupational health and safety, and iatrogenic issues. Both of these issues are implicated in the use of pre-powdered latex gloves. Hospital health-care workers are exposed to latex in many ways: gloves, intravenous sets, ventilator circuits, dental products, resuscitation equipment, anaesthetic equipment. Post-operative complications, delayed wound healing, scar formation, and the potential for misdiagnosis, in the presence of starch powder, have been well documented in the literature with the need for through glove rinsing prior to surgery. Another route for glove powder to enter wounds is through a barrier breach. For an institution to ensure it provides the most durable and effective barrier for healthcare worker protection and patient safety, knowledge is needed regarding the various factors which lead to glove barrier failure. The primary aim of the study was to evaluate the in-use durability of the surgical gloves in current use against powder-free gloves. Descriptive statistics were used to analyse the data, in addition a cost analysis was calculated. The results of this study demonstrated clinically important differences between existing glove products in terms of barrier quality.

  19. Laser-driven synthesis of SiC ceramic powders

    Energy Technology Data Exchange (ETDEWEB)

    Curcio, F.; Ghiglione, G.; Musci, M.; Nannetti, C.


    Ultrafine silicon carbide ceramic powders were produced by irradiating silane and acethylene mixtures with a CW carbon dioxide laser. The process and powder characteristics were studied against the most important experimental parameters. Sintering tests were done in order to evaluate the performance of the laser produced powders: densifications up to 99% of the theoretical value were achieved and metallographic analyses evidenced the superior quality of the best obtained specimens.

  20. Microwave Sintering of Electroless Ni Plated WC Powders


    EROL, Ayhan; YONETKEN, Ahmet


    Nickel matrix reinforced with WC has been manufactured by microwave sintering at various temperatures. A uniform nickel layer on WC powders was deposited prior to sintering using electroless plating technique, allowing close surface contact than can be achieved using conventional methods such as mechanical alloying. The reactivity between WC powders to form compounds is controlled through Ni layer existing on the starting powders. A composite consisting of quaternary additions, a ceramic phas...