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Sample records for situ oxide sintering

  1. Sintering of oxide-supported Pt and Pd nanoparticles in air studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose

    This thesis presents a fundamental study of the sintering of supported nanoparticles in relation to diesel oxidation catalysts. The sintering of supported nanoparticles is an important challenge in relation to this catalyst, as well as many other catalyst systems, and a fundamental understanding...... of Pt, Pd and bimetallic Pt-Pd nanoparticles supported on a flat and homogeneous Al2O3 or SiO2 surface. By using in situ TEM on the planar model catalysts it was possible to directly monitor the detailed dynamical changes of the individual nanoparticles during exposure to oxidizing conditions...

  2. Laser-Induced Reductive Sintering of Nickel Oxide Nanoparticles under Ambient Conditions

    KAUST Repository

    Paeng, Dongwoo; Lee, Daeho; Yeo, Junyeob; Yoo, Jae-Hyuck; Allen, Frances I.; Kim, Eunpa; So, Hongyun; Park, Hee K.; Minor, Andrew M.; Grigoropoulos, Costas P.

    2015-01-01

    © 2015 American Chemical Society. This work is concerned with the kinetics of laser-induced reductive sintering of nonstoichiometric crystalline nickel oxide (NiO) nanoparticles (NPs) under ambient conditions. The mechanism of photophysical reductive sintering upon irradiation using a 514.5 nm continuous-wave (CW) laser on NiO NP thin films has been studied through modulating the laser power density and illumination time. Protons produced due to high-temperature decomposition of the solvent present in the NiO NP ink, oxygen vacancies in the NiO NPs, and electronic excitation in the NiO NPs by laser irradiation all affect the early stage of the reductive sintering process. Once NiO NPs are reduced by laser irradiation to Ni, they begin to coalesce, forming a conducting material. In situ optical and electrical measurements during the reductive sintering process take advantage of the distinct differences between the oxide and the metallic phases to monitor the transient evolution of the process. We observe four regimes: oxidation, reduction, sintering, and reoxidation. A characteristic time scale is assigned to each regime.

  3. Laser-Induced Reductive Sintering of Nickel Oxide Nanoparticles under Ambient Conditions

    KAUST Repository

    Paeng, Dongwoo

    2015-03-19

    © 2015 American Chemical Society. This work is concerned with the kinetics of laser-induced reductive sintering of nonstoichiometric crystalline nickel oxide (NiO) nanoparticles (NPs) under ambient conditions. The mechanism of photophysical reductive sintering upon irradiation using a 514.5 nm continuous-wave (CW) laser on NiO NP thin films has been studied through modulating the laser power density and illumination time. Protons produced due to high-temperature decomposition of the solvent present in the NiO NP ink, oxygen vacancies in the NiO NPs, and electronic excitation in the NiO NPs by laser irradiation all affect the early stage of the reductive sintering process. Once NiO NPs are reduced by laser irradiation to Ni, they begin to coalesce, forming a conducting material. In situ optical and electrical measurements during the reductive sintering process take advantage of the distinct differences between the oxide and the metallic phases to monitor the transient evolution of the process. We observe four regimes: oxidation, reduction, sintering, and reoxidation. A characteristic time scale is assigned to each regime.

  4. In situ Transmission Electron Microscopy of catalyst sintering

    DEFF Research Database (Denmark)

    DeLaRiva, Andrew T.; Hansen, Thomas Willum; Challa, Sivakumar R.

    2013-01-01

    Recent advancements in the field of electron microscopy, such as aberration correctors, have now been integrated into Environmental Transmission Electron Microscopes (TEMs), making it possible to study the behavior of supported metal catalysts under operating conditions at atomic resolution. Here......, we focus on in situ electron microscopy studies of catalysts that shed light on the mechanistic aspects of catalyst sintering. Catalyst sintering is an important mechanism for activity loss, especially for catalysts that operate at elevated temperatures. Literature from the past decade is reviewed...... along with our recent in situ TEM studies on the sintering of Ni/MgAl2O4 catalysts. These results suggest that the rapid loss of catalyst activity in the earliest stages of catalyst sintering could result from Ostwald ripening rather than through particle migration and coalescence. The smallest...

  5. Sintering of beryllium oxide

    International Nuclear Information System (INIS)

    Caillat, R.; Pointud, R.

    1955-01-01

    This study had for origin to find a process permitting to manufacture bricks of beryllium oxide of pure nuclear grade, with a density as elevated as possible and with standardized shape. The sintering under load was the technique kept for the manufacture of the bricks. Because of the important toxicity of the beryllium oxide, the general features for the preliminary study of the sintering, have been determined while using alumina. The obtained results will be able to act as general indication for ulterior studies with sintering under load. (M.B.) [fr

  6. The role of the native oxide shell on the microwave sintering of copper metal powder compacts

    International Nuclear Information System (INIS)

    Mahmoud, Morsi M.; Link, Guido; Thumm, Manfred

    2015-01-01

    Highlights: • Thin oxide native layer had a critical role on microwave sintering of copper. • Explain why microwaves interact with copper powder differently than its bulk. • Abnormal expansion in copper is due to the plastic deformation and crack formation. • In-situ setup gives important insight about the microwave sintering of metals. • Microwave sintering is a promising candidate technology in powder metallurgy. - Abstract: Successful microwave sintering of several metal powders had been reported by many researchers with remarkable improvements in the materials properties and/or in the overall process. However, the concept behind microwave heating of metal powders has not been fully understood till now, as it is well known that bulk metals reflect microwaves. The progress of microwave sintering of copper metal powder compacts was investigated via combining both in-situ electrical resistivity and dilatometry measurements that give important information about microstructural changes with respect to the inter-particle electrical contacts during sintering. The sintering behavior of copper metal powders was depending on the type of the gas used, particle size, the initial green density, the soaking sintering time and the thin oxide layer on the particles surfaces. The thin copper oxide native layer (ceramics) that thermodynamically formed on the particles surfaces under normal handling and ambient environmental conditions had a very critical and important role in the microwave absorption and interaction, the sintering behavior and the microstructural changes. This finding could help to have a fundamental understanding of why MW’s interact with copper metal powder in a different way than its bulk at room temperature, i.e. why a given metal powder could be heated using microwaves while its bulk reflects it

  7. Report on in-situ studies of flash sintering of uranium dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Raftery, Alicia Marie [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-01-24

    Flash sintering is a novel type of field assisted sintering that uses an electric field and current to provide densification of materials on very short time scales. The potential for field assisted sintering techniques to be used in producing nuclear fuel is gaining recognition due to the potential economic benefits and improvements in material properties. The flash sintering behavior has so far been linked to applied and material parameters, but the underlying mechanisms active during flash sintering have yet to be identified. This report summarizes the efforts to investigate flash sintering of uranium dioxide using dilatometer studies at Los Alamos National Laboratory and two separate sets of in-situ studies at Brookhaven National Laboratory’s NSLS-II XPD-1 beamline. The purpose of the dilatometer studies was to understand individual parameter (applied and material) effects on the flash behavior and the purpose of the in-situ studies was to better understand the mechanisms active during flash sintering. As far as applied parameters, it was found that stoichiometry, or oxygen-to-metal ratio, has a significant effect on the flash behavior (time to flash and speed of flash). Composite systems were found to have degraded sintering behavior relative to pure UO2. The critical field studies are complete for UO2.00 and will be analyzed against an existing model for comparison. The in-situ studies showed that the strength of the field and current are directly related to the sample temperature, with temperature-driven phase changes occurring at high values. The existence of an ‘incubation time’ has been questioned, due to a continuous change in lattice parameter values from the moment that the field is applied. Some results from the in-situ experiments, which should provide evidence regarding ion migration, are still being analyzed. Some preliminary conclusions can be made from these results with regard to using field assisted sintering to

  8. In situ observation and neutron diffraction of NiTi powder sintering

    International Nuclear Information System (INIS)

    Chen, Gang; Liss, Klaus-Dieter; Cao, Peng

    2014-01-01

    This study investigated NiTi powder sintering behaviour from elemental powder mixtures of Ni/Ti and Ni/TiH 2 using in situ neutron diffraction and in situ scanning electron microscopy. The sintered porous alloys have open porosities ranging from 2.7% to 36.0%. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH 2 compact leads to less densification yet higher chemical homogenization only after high-temperature sintering. For the first time, direct evidence of the eutectoid phase transformation of NiTi at 620 °C is reported by in situ neutron diffraction. A comparative study of cyclic stress–strain behaviours of the porous NiTi alloys made from Ni/Ti and Ni/TiH 2 compacts indicate that the samples sintered from the Ni/TiH 2 compact exhibited a much higher porosity, larger pore size, lower fracture strength, lower close-to-overall porosity ratio and lower Young’s modulus. Instead of enhanced densification by the use of TiH 2 as reported in the literature, this study shows an adverse effect of TiH 2 on powder densification in NiTi

  9. Study of the oxide reduction and interstitial contents during sintering of different plain carbon steels by in situ mass spectrometry in nitrogen atmosphere

    International Nuclear Information System (INIS)

    Momeni, Mohammad; Gierl, Christian; Danninger, Herbert

    2011-01-01

    Highlights: → Degassing phenomenon was studied in plain steels with different iron base powders. → The integrated area below the MS m12 graph can be used as an indicator of formed CO. → The integrated area is an indicator for in situ carbon loss in the specimen. → Carbon loss and area below the m12 graph can be correlated. - Abstract: Reduction of oxides covering powder particles is an important process during sintering and a prerequisite to form sintering contacts in PM parts. In the present research, degassing and reduction phenomena during sintering of plain carbon steels prepared from different atomised and sponge iron powders were studied by mass spectrometry (MS) in the dilatometer under protective N 2 atmosphere. Interstitial constituents were measured by carbon and oxygen analysis. According to the results, the major part of CO 2 is formed during carbothermic reduction of surface oxides in the low to moderate temperature range ( 600 deg. C, the main product of carbothermic reduction is CO and not CO 2 , but the former cannot be detected by MS in N 2 atmosphere. Signals m44 (CO 2 ) and m12 (C) were however found to be reliable indicators for CO. Similar intensity of mass 12 signals for both ASC and SC up to 1000 deg. C is consistent with equal carbon loss through carbothermic reaction. The integrated areas below the MS signal graphs, and thus the areas of the different degassing peaks obtained in the MS, were used as at least semi-quantitative estimation of the amount of gases formed, bearing in mind that MS is not really a quantitative analytical tool. Although a clearly defined relationship is not visible between oxygen loss and area below the m16 graph, the area for m12 can be used as an indicator for in situ carbon loss in the specimen. Increasing integrated areas for m12 and 16 between 800 and 1300 deg. C with only marginal enhancement of m44 indicates that the major part of oxides are removed as CO, in agreement with Boudouard equilibrium, at

  10. Method of manufacturing gadolinium oxide-incorporated nuclear fuel sintering products

    International Nuclear Information System (INIS)

    Komono, Akira; Seki, Makoto; Omori, Sadayuki.

    1987-01-01

    Purpose: To manufacture nuclear fuel sintering products excellent in burning property and mechanical property. Constitution: In the manufacturing step for nuclear fuel sintering products, specific metal oxides are added for promoting the growth of crystal grains in the sintering. Those metal oxides melted at a temperature lower than the sintering temperature of a mixture of nuclear fuel oxide powder and oxide power, or those metal oxides causing eutectic reaction are used as the metal oxide. Particularly, those compounds having oxygen atom - metal atom ratio (O/M) of not less than 2 are preferably used. As such metal oxides usable herein transition metal oxides, e.g., Nb 2 O 5 , TiO 2 , MoO 3 and WO 3 are preferred, with Nb 2 O 3 and TiO 2 being preferred particularly. (Seki, T.)

  11. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope

    International Nuclear Information System (INIS)

    Majidi, Hasti; Holland, Troy B.; Benthem, Klaus van

    2015-01-01

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior

  12. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Majidi, Hasti [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616 (United States); Holland, Troy B. [Department of Mechanical Engineering, Colorado State University, Fort Collins, CO 80523 (United States); Benthem, Klaus van, E-mail: benthem@ucdavis.edu [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616 (United States)

    2015-05-15

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior.

  13. Sintering process optimization for multi-layer CGO membranes by in situ techniques

    DEFF Research Database (Denmark)

    Kaiser, Andreas; Prasad, A.S.; Foghmoes, Søren Preben Vagn

    2013-01-01

    The sintering of asymmetric CGO bi-layers (thin dense membrane on a porous support; Ce0.9Gd0.1O1.95-delta = CGO) with Co3O4 as sintering additive has been optimized by combination of two in situ techniques. Optical dilatometry revealed that bi-layer shape and microstructure are dramatically...... changing in a narrow temperature range of less than 100 degrees C. Below 1030 degrees C, a higher densification rate in the dense membrane layer than in the porous support leads to concave shape, whereas the densification rate of the support is dominant above 1030 degrees C, leading to convex shape. A fiat...... bi-layer could be prepared at 1030 degrees C, when shrinkage rates were similar. In situ van der Pauw measurements on tape cast layers during sintering allowed following the conductivity during sintering. A strong increase in conductivity and in activation energy E-a for conduction was observed...

  14. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope.

    Science.gov (United States)

    Majidi, Hasti; Holland, Troy B; van Benthem, Klaus

    2015-05-01

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. In-Situ Observation of Sintering Shrinkage of UO2 Compacts Derived from Different Powder Routes

    International Nuclear Information System (INIS)

    Rhee, Young Woo; Oh, Jang Soo; Kim, Dong Joo; Kim, Keon Sik; Kim, Jong Hun; Yang, Jae Ho; Koo, Yang Hyun

    2015-01-01

    In-situ observations on the shrinkage of green pellets with precisely controlled dimensions were carefully conducted by using TOM during H2 atmosphere sintering. The shrinkage retardation in IDR-UO 2 might be attributed to the larger primary particle size of IDRUO 2 than those of ADU- and AUC- UO 2 powders. It would be important to understand the different sintering characteristics of UO 2 powders according to the powder routes, when it comes to designing a new sintering process or choosing a sintering additive for new fuel pellet like PCI (Pellet Cladding Interaction) remedy pellet. In this paper, we have investigated the initial and intermediate sintering shrinkage of UO 2 from different powder routes by in-situ observation of green samples during H2 atmosphere sintering. Effect of powder characteristics of three different UO 2 powders on the initial and intermediate sintering were closely reviewed including crystal structure, powder size, specific surface area, primary crystal size, and O/U ratio

  16. In situ oxide dispersion strengthened tungsten alloys with high compressive strength and high strain-to-failure

    International Nuclear Information System (INIS)

    Huang, Lin; Jiang, Lin; Topping, Troy D.; Dai, Chen; Wang, Xin; Carpenter, Ryan; Haines, Christopher; Schoenung, Julie M.

    2017-01-01

    In this work a novel process methodology to concurrently improve the compressive strength (2078 MPa at a strain rate of 5 × 10"−"4 s"−"1) and strain-to-failure (over 40%) of bulk tungsten materials has been described. The process involves the in situ formation of intragranular tungsten oxide nanoparticles, facilitated by the application of a pressure of 1 GPa at a low sintering temperature of 1200 °C during spark plasma sintering (SPS). The results show that the application of a high pressure of 1 GPa during SPS significantly accelerates the densification process. Concurrently, the second phase oxide nanoparticles with an average grain size of 108 nm, which are distributed within the interiors of the W grains, simultaneously provide strengthening and plasticity by inhibiting grain growth, and generating, blocking, and storing dislocations. - Graphical abstract: In this work a novel process methodology to concurrently improve the compressive strength (2078 MPa at a strain rate of 5 × 10"−"4 s"−"1) and strain-to-failure (over 40%) of bulk W materials has been described. The process involves the in situ formation of intragranular tungsten oxide nanoparticles, facilitated by the application of a pressure of 1 GPa at a low sintering temperature of 1200 °C during spark plasma sintering (SPS).

  17. In-Situ Observation of Sintering Shrinkage of UO{sub 2} Compacts Derived from Different Powder Routes

    Energy Technology Data Exchange (ETDEWEB)

    Rhee, Young Woo; Oh, Jang Soo; Kim, Dong Joo; Kim, Keon Sik; Kim, Jong Hun; Yang, Jae Ho; Koo, Yang Hyun [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2015-10-15

    In-situ observations on the shrinkage of green pellets with precisely controlled dimensions were carefully conducted by using TOM during H2 atmosphere sintering. The shrinkage retardation in IDR-UO{sub 2} might be attributed to the larger primary particle size of IDRUO{sub 2} than those of ADU- and AUC- UO{sub 2} powders. It would be important to understand the different sintering characteristics of UO{sub 2} powders according to the powder routes, when it comes to designing a new sintering process or choosing a sintering additive for new fuel pellet like PCI (Pellet Cladding Interaction) remedy pellet. In this paper, we have investigated the initial and intermediate sintering shrinkage of UO{sub 2} from different powder routes by in-situ observation of green samples during H2 atmosphere sintering. Effect of powder characteristics of three different UO{sub 2} powders on the initial and intermediate sintering were closely reviewed including crystal structure, powder size, specific surface area, primary crystal size, and O/U ratio.

  18. Effect of Ca-Fe oxides additives on NOx reduction in iron ore sintering

    Institute of Scientific and Technical Information of China (English)

    Zhi-yuan Yu; Xiao-hui Fan; Min Gan; Xu-ling Chen

    2017-01-01

    As the emission control regulations get stricter, the NOx reduction in the sintering process becomes an important environmental concern owing to its role in the formation of photochemical smog and acid rain. The NOx emissions from the sintering machine account for 48% of total amount from the iron and steel industry.Thus, it is essential to reduce NOx emissions from the sintering machine, for the achievement of clean production of sinter.Ca-Fe oxides, serving as the main binding phase in the sinter, are therefore used as additives into the sintering mixture to reduce NOx emissions.The results show that the NOx re-duction ratio achieves 27.76% with 8% Ca-Fe oxides additives since the Ca-Fe oxides can advance the ig-nition and inhibit the nitrogen oxidation compared with the conventional condition.Meanwhile, the exist-ence of Ca-Fe oxides was beneficial to the sinter quality since they were typical low melting point com-pounds.The optimal mass fraction of Ca-Fe oxides additives should be less than 8% since the permeability of sintering bed was significantly decreased with a further increase of the Ca-Fe oxides fines, inhibiting the mineralization reaction of sintering mixture.Additionally, the appropriate particle size can be obtained when mixing an equal amount of Ca-Fe oxides additives of -0.5 mm and 0.5-3.0 mm in size.

  19. In situ formation of sintered cordierite–mullite nano–micro composites by utilizing of waste silica fume

    International Nuclear Information System (INIS)

    Khattab, R.M.; EL-Rafei, A.M.; Zawrah, M.F.

    2012-01-01

    Highlights: ► We succeeded to obtain in situ formed sintered cordierite–mullite nano–macro composites from waste and pure materials at 1400 °C. ► Their sinterability was greatly dependent on both firing temperature and composition. ► XRD patterns showed that the optimum temperature required for formation of sintered cordierite–mullite nano–macro composites was achieved at 1400 °C. ► The batch containing 70 wt.% cordierite and 30 wt.% mullite exhibited the best properties. ► Microstructures of the densified composites were composed of nano–macro cordierite–mullite structures. -- Abstract: This study aims at in situ formation of sintered cordierite–mullite nano–macro composites having high technological properties using waste silica fume, calcined ball clay, calcined alumina, and magnesia as starting materials. The starting materials were mixed in different ratios to obtain different cordierite–mullite composite batches in which the cordierite contents ranged from 50 to 100 wt.%. The batches were uni-axially pressed at 100 MPa and sintered at 1350, 1400 and 1450 °C to select the optimum temperature required for cordierite–mullite nano–macro composites formation. The formed phases were identified by X-ray diffraction (XRD) pattern. The sintering parameters in terms of bulk density (BD) and apparent porosity (AP) were determined. The microstructure of composites has been investigated by scanning electron microscope (SEM). Cold crushing strength (CCS) of the sintered batches was evaluated. The result revealed that the cordierite–mullite nano–macro composites were in-situ formed at 1400 °C. The batch containing 70 wt.% cordierite showed good physical and mechanical properties.

  20. Novel approaches for the in situ study of the sintering of nuclear oxide fuel materials and their surrogates

    Energy Technology Data Exchange (ETDEWEB)

    Clavier, Nicolas; Nkou Bouala, Galy Ingrid; Dacheux, Nicolas; Podor, Renaud [Montpellier Univ., Bagnols sur Ceze (France). ICSM - UMR 5257 CEA/CNRS/ENSCM; Lechelle, Jacques [CEA, DNE, DEC, SESC, LLCC, St-Paul lez Durance (France); Martinez, Julien [CEA, DEN, DTEC, SECA, LFC, Bagnols sur Ceze (France)

    2017-07-01

    Sintering is one of the key-points of the processing of ceramic materials. It is then of primary interest for the nuclear fuel cycle, in which it constitutes an important step in the fabrication of either UO{sub 2} or (U,Pu)O{sub 2} pellets used in current PWR reactors. The sintering of actinides oxides not only drives the final density and microstructure of the fuels, but also several characteristics that can impact significantly their behavior in the reactor. Dedicated tools are then needed to monitor the microstructure of such materials and forecast their evolution. In this frame, this paper presents the new potentialities offered by the use of environmental scanning electron microscope at high temperature (HT-ESEM) for the study of nuclear ceramics sintering. First, the results obtained from bulk pellets are detailed, either regarding original fundamental data at the grain level (such as grain boundaries and pores motion), or design of dedicated microstructures through the assessment of grain growth kinetics. Acquisition of sintering maps thanks to the combination of HT-ESEM observations and classical dilatometric measurements are also addressed. In a second part, observations undertaken at the 2-grain scale to monitor the first stage of sintering, dedicated to neck elaboration, are presented, and compared to the results currently provided by numerical models.

  1. Effect of Sintering Temperature on the Properties of Aluminium-Aluminium Oxide Composite Materials

    Directory of Open Access Journals (Sweden)

    Dewan Muhammad Nuruzzaman

    2016-12-01

    Full Text Available In this study, aluminium-aluminium oxide (Al-Al2O3 metal matrix composites of different weight percentage reinforcements of aluminium oxide were processed at different sintering temperatures. In order to prepare these composite specimens, conventional powder metallurgy (PM method was used. Three types specimens of different compositions such as 95%Al+5%Al2O3, 90%Al+10%Al2O3 and 85%Al+15%Al2O3 were prepared under 20 Ton compaction load. Then, all the specimens were sintered in a furnace at two different temperatures 550oC and 580oC. In each sintering process, two different heating cycles were used. After the sintering process, it was observed that undistorted flat specimens were successfully prepared for all the compositions. The effects of sintering temperature and weight fraction of aluminium oxide particulates on the density, hardness and microstructure of Al-Al2O3 composites were observed. It was found that density and hardness of the composite specimens were significantly influenced by sintering temperature and percentage aluminium oxide reinforcement. Furthermore, optical microscopy revealed that almost uniform distribution of aluminium oxide reinforcement within the aluminium matrix was achieved.

  2. Sintering of dioxide pellets in an oxidizing atmosphere (CO2)

    International Nuclear Information System (INIS)

    Santos, G.R.T.

    1992-01-01

    This work consists in the study of the sintering process of U O 2 pellets in an oxidizing atmosphere. Sintering tests were performed in an CO 2 atmosphere and the influence of temperature and time on the pellets density and microstructure were verified. The results obtained were compared to those from the conventional sintering process and its efficiency was confirmed. (author)

  3. Nanocrystalline NdFeB magnet prepared by mechanically activated disproportionation and desorption-recombination in-situ sintering

    International Nuclear Information System (INIS)

    Xiaoya, Liu; Yuping, Li; Lianxi, Hu

    2013-01-01

    The process of mechanically activated disproportionation and desorption-recombination in-situ sintering was proposed to synthesize highly densified nanocrystalline NdFeB magnet, and its validity was demonstrated by experimental investigation with the use of a Nd 16 Fe 76 B 8 (atomic ratio) alloy. Firstly, the as-cast alloy was disproportionated by mechanical milling in hydrogen, with the starting micron-sized Nd 2 Fe 14 B phase decomposed into an intimate mixture of nano-structured NdH 2.7 , Fe 2 B and α-Fe phases. The as-disproportionated alloy powders were compacted by cold pressing and then subjected to desorption-recombination in-situ sintering. The microstructure of both the as-disproportionated and the subsequently sintered samples was characterized by X-ray diffraction and electron transmission microscopy, respectively. The magnetic properties of the sintered samples were measured by using vibrating sample magnetometer. The results showed that, by vacuum sintering, not only was the powder compact consolidated, but also the as-disproportionated microstucture transformed into nanocrystalline Nd 2 Fe 14 B phase via the well-known desorption-recombination reaction, thus giving rise to nanocrystalline NdFeB magnet. In the present study, the optimal sintering parameters were found to be 780 °C×30 min. In this case, the coercivity, the remanence, and maximum energy product of the magnet sample achieved 0.8 T, 635.3 kA/m, and 106.3 kJ/m 3 , respectively. - Highlights: ► Nano-structured disproportionated NdFeB alloy powders by mechanical milling in hydrogen. ► Highly densified green magnet compact by cold pressing of as-disproportionated NdFeB alloy powders. ► Nanocrystalline NdFeB magnets by desorption-recombination in-situ sintering under vacuum. ► Magnetic properties significantly improved by relative density enhancement and nanocrystallization of Nd 2 Fe 14 B phase. ► The effects of sintering parameters on magnetic properties and the underlying

  4. Preparation of a sinterable beryllium oxide through decomposition of beryllium hydroxide (1963)

    International Nuclear Information System (INIS)

    Bernier, M.

    1963-01-01

    In the course of the present study, we have attempted to precise the factors which among the ones effective in the course of the preparation of the beryllium hydroxide and oxide and during the sintering have an influence on the final result: the density and homogeneity of the sintered body. Of the several varieties of hydroxides precipitated from a sulfate solution the β-hydroxide only is always contaminated with beryllium sulfate and cannot be purified even by thorough washing. We noticed that those varieties of the hydroxide (gel, α, β) have different decomposition rates; this behaviour is used to identify and even to dose the different species in (α, β) mixtures. The various hydroxides transmit to the resulting oxides the shape they had when precipitated. Accordingly the history of the oxide is revealed by its behaviour during its fabrication and sintering. By comparing the results of the sintering operation with the various measurements performed on the oxide powders we are led to the conclusion that an oxide obtained from beryllium hydroxide is sinterable under vacuum if the following conditions are fulfilled: the particle size must lie between 0.1 and 0.2 μ and the BeSO 4 content of the powder must be less than 0.25 per cent wt (expressed as SO 3 /BeO). The best fitting is obtained with the oxide issued from an α-hydroxide precipitated as very small aggregates and with a low sulfur-content. We have observed that this is also the case for the oxide obtained by direct calcination of beryllium sulfate. (author) [fr

  5. Sintering uranium oxide using a preheating step

    International Nuclear Information System (INIS)

    Jensen, N.J.; Nivas, Y.; Packard, D.R.

    1977-01-01

    Compacted pellets of uranium oxide or uranium oxide with one or more additives are heated in a kiln in a process having a preheating step, a sintering step, a reduction step, and a cooling step in a controlled atmosphere. The process is practiced to give a range of temperature and atmosphere conditions for obtaining optimum fluoride removal from the compacted pellets along with optimum sintering in a single process. The preheating step of this process is conducted in a temperature range of about 600 0 to about 900 0 C and the pellets are held for at least twenty min, and preferably about 60 min, in an atmosphere having a composition in the range of about 10 to about 75 vol % hydrogen with the balance being carbon dioxide. The sintering step is conducted at a temperature in the range of about 900 0 C to 1500 0 C in the presence of an atmosphere having a composition in the range of about 0.5 to about 90 vol % hydrogen with the balance being carbon dioxide. The reduction step reduces the oxygen to metal ratio of the pellets to a range of about 1.98 to 2.10:1 and this is accomplished by gradually cooling the pellets for about 30 to about 120 min from the temperature of the sintering step to about 1100 0 C in an atmosphere of about 10 to 90 vol % hydrogen with the balance being carbon dioxide. Thereafter the pellets are cooled to about 100 0 C under a protective atmosphere, and in one preferred practice the same atmosphere used in the reduction step is used in the cooling step. The preheating, sintering and reduction steps may also be conducted with their respective atmospheres having an initial additional component of water vapor and the water vapor can comprise up to about 20 vol %

  6. An in situ Study of NiTi Powder Sintering Using Neutron Diffraction

    Directory of Open Access Journals (Sweden)

    Gang Chen

    2015-04-01

    Full Text Available This study investigates phase transformation and mechanical properties of porous NiTi alloys using two different powder compacts (i.e., Ni/Ti and Ni/TiH2 by a conventional press-and-sinter means. The compacted powder mixtures were sintered in vacuum at a final temperature of 1373 K. The phase evolution was performed by in situ neutron diffraction upon sintering and cooling. The predominant phase identified in all the produced porous NiTi alloys after being sintered at 1373 K is B2 NiTi phase with the presence of other minor phases. It is found that dehydrogenation of TiH2 significantly affects the sintering behavior and resultant microstructure. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH2 compact leads to less densification, yet higher chemical homogenization, after high temperature sintering but not in the case of low temperature sintering. Moreover, there is a direct evidence of the eutectoid decomposition of NiTi at ca. 847 and 823 K for Ni/Ti and Ni/TiH2, respectively, during furnace cooling. The static and cyclic stress-strain behaviors of the porous NiTi alloys made from the Ni/Ti and Ni/TiH2 compacts were also investigated. As compared with the Ni/Ti sintered samples, the samplessintered from the Ni/TiH2 compact exhibited a much higher porosity, a higher close-to-total porosity, a larger pore size and lower tensile and compressive fracture strength.

  7. Microstructure evolution during pressureless sintering of bulk oxide ceramics

    Directory of Open Access Journals (Sweden)

    Karel Maca

    2009-06-01

    Full Text Available The author’s experience concerning the infl uence of the choice of different pressureless heating schedules on the fi nal microstructure of oxide ceramic materials is summarized in the paper. Alumina, ceria, strontium titanate, as well as tetragonal (3 mol% Y2O3 and cubic (8 mol% Y2O3 zirconia were cold isostatically pressed or injection moulded and pressureless sintered with different heating schedules – namely with Constant-Rate of Heating with different dwell temperatures (CRH, with Rate-Controlled Sintering (RCS and with Two-Step Sintering (TSS. It was examined whether some of these three sintering schedules, with the same fi nal density achieved, can lead to a decrease of the grain size of sintered ceramics. The results showed that only TSS (and only for selected materials brought significant decrease of the grain size.

  8. Densification of LSGM electrolytes using activated microwave sintering

    Science.gov (United States)

    Kesapragada, S. V.; Bhaduri, S. B.; Bhaduri, S.; Singh, P.

    Lanthanum gallate doped with alkaline rare earths (LSGM) powders were densified using an activated microwave sintering process for developing a dense stable electrolyte layer for applications in intermediate temperature-solid oxide fuel cells (IT-SOFCs). Due to heat generation in situ, the process of sintering gets activated with faster kinetics compared to a conventional sintering process. The effect of various microwave process parameters on the microstructure and phase formation was studied. The sintered pellets were characterized using scanning electron microscopy-energy dispersive analysis (SEM-EDAX), and X-ray diffraction (XRD). The density of LSGM pellets microwave sintered at 1350 °C for 20 min is greater than 95% theoretical density with a fine grained microstructure (˜2-3 μm) and without the presence of other phase(s).

  9. Integrated analysis of oxide nuclear fuel sintering

    International Nuclear Information System (INIS)

    Baranov, V.; Kuzmin, R.; Tenishev, A.; Timoshin, I.; Khlunov, A.; Ivanov, A.; Petrov, I.

    2011-01-01

    Dilatometric and thermal-gravimetric investigations have been carried out for the sintering process of oxide nuclear fuel in gaseous Ar - 8% H 2 atmosphere at temperatures up to 1600 0 C. The pressed compacts were fabricated under real production conditions of the OAO MSZ with application of two different technologies, so called 'dry' and 'wet' technologies. Effects of the grain size growth after the heating to different temperatures were observed. In order to investigate the effects produced by rate of heating on properties of sintered fuel pellets, the heating rates were varied from 1 to 8 0 C per minute. Time of isothermal overexposure at maximal temperature (1600 0 C) was about 8 hours. Real production conditions were imitated. The results showed that the sintering process of the fuel pellets produced by two technologies differs. The samples sintered under different heating rates were studied with application of scanning electronic microscopy analysis for determination of mean grain size. A simulation of heating profile for industrial furnaces was performed to reduce the beam cycles and estimate the effects of variation of the isothermal overexposure temperatures. Based on this data, an optimization of the sintering conditions was performed in operations terms of OAO MSZ. (authors)

  10. Effect of process parameters on surface oxides on chromium-alloyed steel powder during sintering

    International Nuclear Information System (INIS)

    Chasoglou, D.; Hryha, E.; Nyborg, L.

    2013-01-01

    The use of chromium in the PM steel industry today puts high demands on the choice and control of the atmosphere during the sintering process due to its high affinity to oxygen. Particular attention is required in order to control the surface chemistry of the powder which in turn is the key factor for the successful sintering and production of PM parts. Different atmosphere compositions, heating rates and green densities were employed while performing sintering trials on water atomized steel powder pre-alloyed with 3 wt.% Cr in order to evaluate the effect on surface chemical reactions. Fracture surfaces of sintered samples were examined using high resolution scanning electron microscopy combined with X-ray microanalysis. The investigation was complemented with thermogravimetric (TG) studies. Reaction products in particulate form containing strong-oxide forming elements such as Cr, Si and Mn were formed during sintering for all conditions. Processing in vacuum results in intensive inter-particle neck development during the heating stage and consequently in the excessive enclosure of surface oxide which is reflected in less good final mechanical properties. Enhanced oxide reduction was observed in samples processed in hydrogen-containing atmospheres independent of the actual content in the range of 3–10 vol.%. An optimum heating rate was required for balancing reduction/oxidation processes. A simple model for the enclosure and growth of oxide inclusions during the sinter-neck development is proposed. The obtained results show that significant reduction of the oxygen content can be achieved by adjusting the atmosphere purity/composition. - Highlights: ► A local atmosphere microclimate is very important for sintering of PM steels. ► High risk of surface oxide enclosure between 800 and 1000 °C. ► Coalescence and agglomeration of enclosed oxides take place during sintering. ► The effect of different process parameters on the oxide reduction is examined. ► A

  11. Nanocrystalline NdFeB magnet prepared by mechanically activated disproportionation and desorption-recombination in-situ sintering

    Energy Technology Data Exchange (ETDEWEB)

    Xiaoya, Liu; Yuping, Li [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Lianxi, Hu, E-mail: hulx@hit.edu.cn [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China)

    2013-03-15

    The process of mechanically activated disproportionation and desorption-recombination in-situ sintering was proposed to synthesize highly densified nanocrystalline NdFeB magnet, and its validity was demonstrated by experimental investigation with the use of a Nd{sub 16}Fe{sub 76}B{sub 8} (atomic ratio) alloy. Firstly, the as-cast alloy was disproportionated by mechanical milling in hydrogen, with the starting micron-sized Nd{sub 2}Fe{sub 14}B phase decomposed into an intimate mixture of nano-structured NdH{sub 2.7}, Fe{sub 2}B and {alpha}-Fe phases. The as-disproportionated alloy powders were compacted by cold pressing and then subjected to desorption-recombination in-situ sintering. The microstructure of both the as-disproportionated and the subsequently sintered samples was characterized by X-ray diffraction and electron transmission microscopy, respectively. The magnetic properties of the sintered samples were measured by using vibrating sample magnetometer. The results showed that, by vacuum sintering, not only was the powder compact consolidated, but also the as-disproportionated microstucture transformed into nanocrystalline Nd{sub 2}Fe{sub 14}B phase via the well-known desorption-recombination reaction, thus giving rise to nanocrystalline NdFeB magnet. In the present study, the optimal sintering parameters were found to be 780 Degree-Sign C Multiplication-Sign 30 min. In this case, the coercivity, the remanence, and maximum energy product of the magnet sample achieved 0.8 T, 635.3 kA/m, and 106.3 kJ/m{sup 3}, respectively. - Highlights: Black-Right-Pointing-Pointer Nano-structured disproportionated NdFeB alloy powders by mechanical milling in hydrogen. Black-Right-Pointing-Pointer Highly densified green magnet compact by cold pressing of as-disproportionated NdFeB alloy powders. Black-Right-Pointing-Pointer Nanocrystalline NdFeB magnets by desorption-recombination in-situ sintering under vacuum. Black-Right-Pointing-Pointer Magnetic properties significantly

  12. In situ process monitoring in selective laser sintering using optical coherence tomography

    Science.gov (United States)

    Gardner, Michael R.; Lewis, Adam; Park, Jongwan; McElroy, Austin B.; Estrada, Arnold D.; Fish, Scott; Beaman, Joseph J.; Milner, Thomas E.

    2018-04-01

    Selective laser sintering (SLS) is an efficient process in additive manufacturing that enables rapid part production from computer-based designs. However, SLS is limited by its notable lack of in situ process monitoring when compared with other manufacturing processes. We report the incorporation of optical coherence tomography (OCT) into an SLS system in detail and demonstrate access to surface and subsurface features. Video frame rate cross-sectional imaging reveals areas of sintering uniformity and areas of excessive heat error with high temporal resolution. We propose a set of image processing techniques for SLS process monitoring with OCT and report the limitations and obstacles for further OCT integration with SLS systems.

  13. Real-Time Observation of Platinum Redispersion on Ceria-Based Oxide by In-situ Turbo-XAS in Fluorescence Mode

    International Nuclear Information System (INIS)

    Nagai, Yasutaka; Dohmae, Kazuhiko; Tanabe, Toshitaka; Shinjoh, Hirofumi; Takagi, Nobuyuki; Ikeda, Yasuo; Guilera, Gemma; Pascarelli, Sakura; Newton, Mark; Matsumoto, Shin'ichi

    2007-01-01

    A real-time observation of the redispersion behavior of sintered Pt on ceria-based oxide was made possible by in-situ time-resolved Turbo-XAS in fluorescence mode. 2 wt% Pt/Ce-Zr-Y mixed oxide samples were prepared, and then treated under an aging condition. The average Pt particle size measured by CO absorption method after aging was 7 nm. Redispersion treatments of the previously aged catalyst were carried out at 600 deg. C within an in-situ XAS cell in a cyclical flow of reducing/oxidizing gases. Pt L3-edge XANES spectra were collected every 1.1 second under in-situ conditions. From a change in the XANES spectra, we observed that the Pt particle size of the aged catalyst decreased from 7 to 5 nm after 60 seconds and then to 3 nm after 1000 seconds

  14. Effect of low temperature in-situ sintering on the impedance and the performance of intermediate temperature solid oxide fuel cell cathodes

    DEFF Research Database (Denmark)

    Nielsen, Jimmi; Hjalmarsson, Per; Hansen, Martin Hangaard

    2014-01-01

    The effect of in-situ sintering temperature and time on the electronic conductivity, impedance and performance of IT-SOFC cathodes were studied. The studied cathodes were for comparison (La0.6Sr0.4)0.99CoO3 (LSC), (La0.6Sr0.4)0.99CoO3:Ce0.9Gd0.1O1.95 (LSC:CGO), La0.58Sr0.4Co0.2Fe0.8O3 (LSCF) and La......0.58Sr0.4Co0.2Fe0.8O3:Ce0.9Gd0.1O1.95 (LSCF:CGO). The LSCF-based cathodes showed poor sintering capabilities compared to the LSC-based cathodes in the studied temperature range of 650–950 °C. The poor necking between individual LSCF grains lower the electronic conductivity. Furthermore, poor cathode....../electrolyte adhesion was seen as an additional high frequency impedance arc, which gradually disappeared as the LSCF cathodes were sintered at increasing temperature. Effects on the impedance shape from poor cathode grain connectivity was shown through impedance simulations to result in a possible increase in the high...

  15. Hot-pressed silicon nitride with various lanthanide oxides as sintering additives

    Science.gov (United States)

    Ueno, K.; Toibana, Y.

    1984-01-01

    The effects of addition of various lanthanide oxides and their mixture with Y2O3 on the sintering of Si3N4 were investigated. The addition of simple and mixed lanthanide oxides promoted the densification of Si3N4 in hot-pressing at 1800 C under 300-400kg/ centimeters squared for 60 min. The crystallization of yttrium and lanthanide-silicon oxynitrides which was observed inn the sintered body containing yttrium-lanthanide mixed oxides as additives led to the formation of a highly refractory Si3N4 ceramic having a bending strength of 82 and 84 kg/millimeters squared at room temperature and 1300 C respectively. In a Y2O3+La2O3 system, a higher molar ratio of La2O3 to Y2O3 gave a higher hardness and strength at high temperatures. It was found that 90 min was an optimum sintering time for the highest strength.

  16. Chemically produced nanostructured ODS-lanthanum oxide-tungsten composites sintered by spark plasma

    International Nuclear Information System (INIS)

    Yar, Mazher Ahmed; Wahlberg, Sverker; Bergqvist, Hans; Salem, Hanadi G.; Johnsson, Mats; Muhammed, Mamoun

    2011-01-01

    High purity W and W-0.9La 2 O 3 (wt.%) nanopowders were produced by a wet chemical route. The precursor was prepared by the reaction of ammonium paratungstate (APT) with lanthanum salt in aqueous solutions. High resolution electron microscopy investigations revealed that the tungstate particles were coated with oxide precipitates. The precursor powder was reduced to tungsten metal with dispersed lanthanum oxide. Powders were consolidated by spark plasma sintering (SPS) at 1300 and 1400 o C to suppress grain growth during sintering. The final grain size relates to the SPS conditions, i.e. temperature and heating rate, regardless of the starting powder particle size. Scanning electron microscopy revealed that oxide phases were mainly accumulated at grain boundaries while the tungsten matrix constituted of nanosized sub-grains. The transmission electron microscopy revealed that the tungsten grains consist of micron-scale grains and finer sub-grains. EDX analysis confirmed the presence of W in dispersed oxide phases with varying chemical composition, which evidenced the presence of complex oxide phases (W-O-La) in the sintered metals.

  17. Optimization of thorium oxalate precipitation conditions relative to thorium oxide sinterability

    International Nuclear Information System (INIS)

    White, G.D.; Bray, L.A.; Hart, P.E.

    1980-01-01

    The effect of thorium oxalate precipitation conditions on derived oxide sinterability was investigated with the objective of producing ThO 2 powder that could be sintered to high density without premilling. Precipitation conditions examined were temperature, digestion time and agitation method which were employed in a two-level factorial experimental design to delineate their effects. The two levels for each of the factors, respectively, were 10 0 C and 70 0 C, 15 min and 360 min, and mechanical stirrer and a homogenizer that imparted both mechanical and ultrasonic agitation. The ThO 2 derived from each of the precipitation trials was characterized with respect to morphology, surface area, and crystallite size as well as sinterability. Only precipitation temperature had a significant effect upon all the properties of the derived oxide powders

  18. Manufacture of sintered bricks of high density from beryllium oxide

    International Nuclear Information System (INIS)

    Pointud, R.; Rispal, Ch.; Le Garec, M.

    1959-01-01

    Beryllium oxide bricks of nuclear purity 100 x 100 x 50 and 100 x 100 x 100 mm of very high density (between 2.85 and 3.00) are manufactured by sintering under pressure in graphite moulds at temperatures between 1,750 and 1,850 deg. C, and under a pressure of 150 kg/cm 2 . The physico-chemical state of the saw material is of considerable importance with regard to the success of the sintering operation. In addition, a study of the sintering of a BeO mixture with 3 to 5 per cent of boron introduced in the form of boric acid, boron carbide or elementary boron shows that high densities can only be obtained by sintering under pressure. For technical reasons of manufacture, only the mixture based on boron carbide is used. The sintering is carried out in graphite moulds at 1500 deg. C under 150 kg/cm 2 pressure, and bricks can be obtained with density between 2,85 and 2,90. Laboratory studies and the industrial manufacture of various sinters are described in detail. (author) [fr

  19. Sintering of uranium oxide of high specific surface area

    International Nuclear Information System (INIS)

    Bel, Alain; Francois, Bernard; Delmas, Roger; Caillat, Roger

    1959-01-01

    The extent to which a uranium oxide powder deriving from ammonium uranate or uranium peroxide lends itself to the sintering process depends largely on its specific surface area. When this is greater than 5 m 2 / g there is an optimum temperature for sintering in hydrogen. This temperature becomes less as the specific area of the powder is greater. Reprint of a paper published in Comptes rendus des seances de l'Academie des Sciences, t. 249, p. 1045-1047, sitting of 21 September 1959 [fr

  20. Ferritic oxide dispersion strengthened alloys by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Allahar, Kerry N., E-mail: KerryAllahar@boisestate.edu [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Burns, Jatuporn [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Jaques, Brian [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Wu, Y.Q. [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Charit, Indrajit [Department of Chemical and Materials Engineering, University of Idaho, McClure Hall Room 405D, Moscow, ID 83844 (United States); Cole, James [Idaho National Laboratory, Idaho Falls, ID 83401 (United States); Butt, Darryl P. [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States)

    2013-11-15

    Spark plasma sintering (SPS) was used to consolidate a Fe–16Cr–3Al (wt.%) powder that was mechanically alloyed with Y{sub 2}O{sub 3} and Ti powders to produce 0.5 Y{sub 2}O{sub 3} and 0.5 Y{sub 2}O{sub 3}–1Ti powders. The effects of mechanical alloying and sintering conditions on the microstructure, relative density and hardness of the sintered oxide dispersion strengthened (ODS) alloys are presented. Scanning electron microscopy indicated a mixed fine-grain and coarse-grain microstructure that was attributed to recrystallization and grain growth during sintering. Analysis of the transmission electron microscopy (TEM) and atom probe tomography (APT) data identified Y–O and Y–O–Ti nanoclusters. Elemental ratios of these nanoclusters were consistent with that observed in hot-extruded ODS alloys. The influence of Ti was to refine the grains as well as the nanoclusters with there being greater number density and smaller sizes of the Y–O–Ti nanoclusters as compared to the Y–O nanoclusters. This resulted in the Ti-containing samples being harder than the Ti-free alloys. The hardness of the alloys with the Y–O–Ti nanoclusters was insensitive to sintering time while smaller hardness values were associated with longer sintering times for the alloys with the Y–O nanoclusters. Pressures greater than 80 MPa are recommended for improved densification as higher sintering temperatures and longer sintering times at 80 MPa did not improve the relative density beyond 97.5%.

  1. Boric oxide or boric acid sintering aid for sintering ceramics

    International Nuclear Information System (INIS)

    Lawler, H.A.

    1979-01-01

    The invention described relates to the use of liquid sintering aid in processes involving sintering of ceramic materials to produce dense, hard articles having industrial uses. Although the invention is specifically discussed in regard to compositions containing silicon carbide as the ceramic material, other sinterable carbides, for example, titanium carbide, may be utilized as the ceramic material. A liquid sintering aid for densifying ceramic material is selected from solutions of H 3 BO 3 , B 2 O 3 and mixtures of these solutions. In sintering ceramic articles, e.g. silicon carbide, a shaped green body is formed from a particulate ceramic material and a resin binder, and the green body is baked at a temperature of 500 to 1000 0 C to form a porous body. The liquid sintering aid of B 2 O 3 and/or H 3 BO 3 is then dispersed through the porous body and the treated body is sintered at a temperature of 1900 to 2200 0 C to produce the sintered ceramic article. (U.K.)

  2. Sintering of beryllium oxide; Frittage de l'oxyde de beryllium

    Energy Technology Data Exchange (ETDEWEB)

    Caillat, R; Pointud, R [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1955-07-01

    This study had for origin to find a process permitting to manufacture bricks of beryllium oxide of pure nuclear grade, with a density as elevated as possible and with standardized shape. The sintering under load was the technique kept for the manufacture of the bricks. Because of the important toxicity of the beryllium oxide, the general features for the preliminary study of the sintering, have been determined while using alumina. The obtained results will be able to act as general indication for ulterior studies with sintering under load. (M.B.) [French] Cette etude a eu pour origine la recherche d'un procede permettant de fabriquer industriellement des briques d'oxyde de beryllium nucleaireraent pures, de densite aussi elevee que possible et de forme standardisee. Le frittage sous charge fut la technique retenue pour la fabrication des briques. En raison de la grande toxicite de l'oxyde de beryllium, les caracteristiques generales du frittage, pour l'etude preliminaire, ont ete determine en utilisant de l'alumine. Les resultats obtenus pourront servir d'indication generale pour des etudes ulterieurs avec frittage sous charge. (M.B.)

  3. ADVANTAGES/DISADVANTAGES FOR ISCO METHODS IN-SITU FENTON OXIDATION IN-SITU PERMANGANATE OXIDATION

    Science.gov (United States)

    The advantages and disadvantages of in-situ Fenton oxidation and in-situ permanganate oxidation will be presented. This presentation will provide a brief overview of each technology and a detailed analysis of the advantages and disadvantages of each technology. Included in the ...

  4. Influence of sintering atmospheres on the aluminium sintering characteristics

    International Nuclear Information System (INIS)

    Mintzer, S.; Bermudez Belkys, S.

    1993-01-01

    This paper describes the aluminium powder (Al) cool compacted (at 95% from theoretical density) which was sintered at 903 K during 4 hours at different atmospheres; oxidizing (air), inert Argon (Ar), Nitrogen (N) and high vacuum. The results obtained show: a) porosity measurements; greater porosity when sintering in Ar and air. b) Metallographic and Scanning observations: many fine pores (< 1 μm) and pore lines distributed at random, at air sintering and greater pores distributed preferentially near the surface, in Ar and N atmospheres. c) Dimensional changes: tendency to contraction of the samples at N and vacuum sintering and expansion in Ar or air. d) Mechanical properties: greater strength and fluence stresses at air and N sintering. The analysis of the results is performed considering sintering modes in presence of an oxide layer and dropped inert gases. (Author)

  5. Sintering of uranium dioxide pellets (UO2) in an oxidizing atmosphere (C O2)

    International Nuclear Information System (INIS)

    Santos, G.R.T.

    1992-01-01

    This work consists in the study of the sintering process of U O 2 pellets in an oxidizing atmosphere. Sintering tests were performed in an CO 2 atmosphere and the influence of temperature and time on the pellets density and microstructure were verified. The results obtained were compared to those from the conventional sintering process and its efficiency was confirmed. (author)

  6. Sintering uranium oxide in the reaction product of hydrogen-carbon dioxide mixtures

    International Nuclear Information System (INIS)

    De Hollander, W.R.; Nivas, Y.

    1975-01-01

    Compacted pellets of uranium oxide alone or containing one or more additives such as plutonium dioxide, gadolinium oxide, titanium dioxide, silica, and alumina are heated to 900 to 1599 0 C in the presence of a mixture of hydrogen and carbon dioxide, either alone or with an inert carrier gas and held at the desired temperature in this atmosphere to sinter the pellets. The sintered pellets are then cooled in an atmosphere having an oxygen partial pressure of 10 -4 to 10 -18 atm of oxygen such as dry hydrogen, wet hydrogen, dry carbon monoxide, wet carbon monoxide, inert gases such as nitrogen, argon, helium, and neon and mixtures of ayny of the foregoing including a mixture of hydrogen and carbon dioxide. The ratio of hydrogen to carbon dioxide in the gas mixture fed to the furnace is controlled to give a ratio of oxygen to uranium atoms in the sintered particles within the range of 1.98:1 to about 2.10:1. The water vapor present in the reaction products in the furnace atmosphere acts as a hydrolysis agent to aid removal of fluoride should such impurity be present in the uranium oxide. (U.S.)

  7. Improved reaction sintered silicon nitride. [protective coatings to improve oxidation resistance

    Science.gov (United States)

    Baumgartner, H. R.

    1978-01-01

    Processing treatments were applied to as-nitrided reaction sintered silicon nitride (RSSN) with the purposes of improving strength after processing to above 350 MN/m2 and improving strength after oxidation exposure. The experimental approaches are divided into three broad classifications: sintering of surface-applied powders; impregnation of solution followed by further thermal processing; and infiltration of molten silicon and subsequent carburization or nitridation of the silicon. The impregnation of RSSN with solutions of aluminum nitrate and zirconyl chloride, followed by heating at 1400-1500 C in a nitrogen atmosphere containing silicon monoxide, improved RSSN strength and oxidation resistance. The room temperature bend strength of RSSN was increased nearly fifty percent above the untreated strength with mean absolute strengths up to 420 MN/m2. Strengths of treated samples that were measured after a 12 hour oxidation exposure in air were up to 90 percent of the original as-nitrided strength, as compared to retained strengths in the range of 35 to 60 percent for untreated RSSN after the same oxidation exposure.

  8. Laser sintering of magnesia with nanoparticles of iron oxide and aluminum oxide

    International Nuclear Information System (INIS)

    García, L.V.; Mendivil, M.I.; Roy, T.K. Das; Castillo, G.A.; Shaji, S.

    2015-01-01

    Highlights: • Laser sintered MgO pellets with nanoparticles of Al 2 O 3 and Fe 2 O 3 . • Characterized these pellets by XRD, SEM and XPS. • Spinel formations were observed in both cases. • Changes in morphology and structure were analyzed. - Abstract: Nanoparticles of iron oxide (Fe 2 O 3 , 20–40 nm) and aluminum oxide (Al 2 O 3 , 50 nm) were mixed in different concentrations (3, 5 and 7 wt%) in a magnesium oxide (MgO) matrix. The mixture pellet was irradiated with 532 nm output from a Q-switched Nd:YAG laser using different laser fluence and translation speed for sintering. The refractory samples obtained were analyzed using X-ray diffraction technique, scanning electron microscopy and X-ray photoelectron spectroscopy. The results showed that the samples irradiated at translation speed of 110 μm/s and energy fluence of 1.7 J/cm 2 with a concentration of 5 and 7 wt% of Fe 2 O 3 presented the MgFe 2 O 4 spinel-type phase. With the addition of Al 2 O 3 nanoparticles, at a translation speed of 110 μm/s and energy fluence of 1.7 J/cm 2 , there were the formations of MgAl 2 O 4 spinel phase. The changes in morphologies and microstructure due to laser irradiation were analyzed

  9. Spark Plasma Sintering and Densification Mechanisms of Antimony-Doped Tin Oxide Nanoceramics

    Directory of Open Access Journals (Sweden)

    Junyan Wu

    2013-01-01

    Full Text Available Densification of antimony-doped tin oxide (ATO ceramics without sintering aids is very difficult, due to the volatilization of SnO2, formation of deleterious phases above 1000°C, and poor sintering ability of ATO particles. In this paper, monodispersed ATO nanoparticles were synthesized via sol-gel method, and then ATO nanoceramics with high density were prepared by spark plasma sintering (SPS technology using the as-synthesized ATO nanoparticles without the addition of sintering aids. The effect of Sb doping content on the densification was investigated, and the densification mechanisms were explored. The results suggest that ATO nanoparticles derived from sol-gel method show good crystallinity with a crystal size of 5–20 nm and Sb is incorporated into the SnO2 crystal structure. When the SPS sintering temperature is 1000°C and the Sb doping content is 5 at.%, the density of ATO nanoceramics reaches a maximum value of 99.2%. Densification mechanisms are explored in detail.

  10. Electric-Loading Enhanced Kinetics in Oxide Ceramics: Pore Migration, Sintering and Grain Growth: Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Chen, I-Wei [Univ. of Pennsylvania, Philadelphia, PA (United States). Dept. of Materials Science & Engineering

    2018-02-02

    Solid oxide fuel cells and solid oxide electrolysis cells rely on solid electrolytes in which a large ionic current dominates. This project was initiated to investigate microstructural changes in such devices under electrochemical forces, because nominally insignificant processes may couple to the large ionic current to yield non-equilibrium phenomena that alter the microstructure. Our studies had focused on yttria-stabilized cubic zirconia (YSZ) widely used in these devices. The experiments have revealed enhanced grain growth at higher temperatures, pore and gas bubble migration at all temperatures, and the latter also lead to enhanced sintering of highly porous ceramics into fully dense ceramics at unprecedentedly low temperatures. These results have shed light on kinetic processes that fall completely outside the realm of classical ceramic processing. Other fast-oxygen oxide ceramics closely related to, and often used in conjunction with zirconia ceramics, have also be investigated, as are closely related scientific problems in zirconia ceramics. These include crystal structures, defects, diffusion kinetics, oxygen potentials, low temperature sintering, flash sintering, and coarsening theory, and all have resulted in greater clarity in scientific understanding. The knowledge is leveraged to provide new insight to electrode kinetics and near-electrode mixed conductivity and to new materials. In the following areas, our research has resulted in completely new knowledge that defines the state-of-the-art of the field. (a) Electrical current driven non-equilibrium phenomena, (b) Enhanced grain growth under electrochemically reducing conditions, (c) Development of oxygen potential polarization in electrically loaded electrolyte, (d) Low temperature sintering and grain growth, and (e) Structure, defects and cation kinetics of fluorite-structured oxides. Our research has also contributed to synthesis of new energy-relevant electrochemical materials and new understanding

  11. Laser sintering of magnesia with nanoparticles of iron oxide and aluminum oxide

    Energy Technology Data Exchange (ETDEWEB)

    García, L.V.; Mendivil, M.I.; Roy, T.K. Das; Castillo, G.A. [Facultad de Ingenieria Mecanica y Electrica, Universidad Autonoma de Nuevo Leon, Av. Pedro de Alba s/n, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66451 (Mexico); Shaji, S., E-mail: sshajis@yahoo.com [Facultad de Ingenieria Mecanica y Electrica, Universidad Autonoma de Nuevo Leon, Av. Pedro de Alba s/n, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66451 (Mexico); CIIDIT, Universidad Autonoma de Nuevo Leon, Apodaca, Nuevo Leon (Mexico)

    2015-05-01

    Highlights: • Laser sintered MgO pellets with nanoparticles of Al{sub 2}O{sub 3} and Fe{sub 2}O{sub 3}. • Characterized these pellets by XRD, SEM and XPS. • Spinel formations were observed in both cases. • Changes in morphology and structure were analyzed. - Abstract: Nanoparticles of iron oxide (Fe{sub 2}O{sub 3}, 20–40 nm) and aluminum oxide (Al{sub 2}O{sub 3}, 50 nm) were mixed in different concentrations (3, 5 and 7 wt%) in a magnesium oxide (MgO) matrix. The mixture pellet was irradiated with 532 nm output from a Q-switched Nd:YAG laser using different laser fluence and translation speed for sintering. The refractory samples obtained were analyzed using X-ray diffraction technique, scanning electron microscopy and X-ray photoelectron spectroscopy. The results showed that the samples irradiated at translation speed of 110 μm/s and energy fluence of 1.7 J/cm{sup 2} with a concentration of 5 and 7 wt% of Fe{sub 2}O{sub 3} presented the MgFe{sub 2}O{sub 4} spinel-type phase. With the addition of Al{sub 2}O{sub 3} nanoparticles, at a translation speed of 110 μm/s and energy fluence of 1.7 J/cm{sup 2}, there were the formations of MgAl{sub 2}O{sub 4} spinel phase. The changes in morphologies and microstructure due to laser irradiation were analyzed.

  12. Constrained Sintering in Fabrication of Solid Oxide Fuel Cells.

    Science.gov (United States)

    Lee, Hae-Weon; Park, Mansoo; Hong, Jongsup; Kim, Hyoungchul; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook

    2016-08-09

    Solid oxide fuel cells (SOFCs) are inevitably affected by the tensile stress field imposed by the rigid substrate during constrained sintering, which strongly affects microstructural evolution and flaw generation in the fabrication process and subsequent operation. In the case of sintering a composite cathode, one component acts as a continuous matrix phase while the other acts as a dispersed phase depending upon the initial composition and packing structure. The clustering of dispersed particles in the matrix has significant effects on the final microstructure, and strong rigidity of the clusters covering the entire cathode volume is desirable to obtain stable pore structure. The local constraints developed around the dispersed particles and their clusters effectively suppress generation of major process flaws, and microstructural features such as triple phase boundary and porosity could be readily controlled by adjusting the content and size of the dispersed particles. However, in the fabrication of the dense electrolyte layer via the chemical solution deposition route using slow-sintering nanoparticles dispersed in a sol matrix, the rigidity of the cluster should be minimized for the fine matrix to continuously densify, and special care should be taken in selecting the size of the dispersed particles to optimize the thermodynamic stability criteria of the grain size and film thickness. The principles of constrained sintering presented in this paper could be used as basic guidelines for realizing the ideal microstructure of SOFCs.

  13. Liquid phase sintered superconducting cermet

    International Nuclear Information System (INIS)

    Ray, S.P.

    1990-01-01

    This patent describes a method of making a superconducting cermet having superconducting properties with improved bulk density, low porosity and in situ stabilization. It comprises: forming a structure of a superconducting ceramic material having the formula RM 2 Cu 3 O (6.5 + x) wherein R is one or more rare earth elements capable of reacting to form a superconducting ceramic, M is one or more alkaline earth metal elements selected from barium and strontium capable of reacting to form a superconducting ceramic, x is greater than 0 and less than 0.5; and a precious metal compound in solid form selected from the class consisting of oxides, sulfides and halides of silver; and liquid phase sintering the mixture at a temperature wherein the precious metal of the precious metal compound is molten and below the melting point of the ceramic material. The liquid phase sintering is carried out for a time less than 36 hours but sufficient to improve the bulk density of the cermet

  14. Method for hot pressing beryllium oxide articles

    Science.gov (United States)

    Ballard, Ambrose H.; Godfrey, Jr., Thomas G.; Mowery, Erb H.

    1988-01-01

    The hot pressing of beryllium oxide powder into high density compacts with little or no density gradients is achieved by employing a homogeneous blend of beryllium oxide powder with a lithium oxide sintering agent. The lithium oxide sintering agent is uniformly dispersed throughout the beryllium oxide powder by mixing lithium hydroxide in an aqueous solution with beryllium oxide powder. The lithium hydroxide is converted in situ to lithium carbonate by contacting or flooding the beryllium oxide-lithium hydroxide blend with a stream of carbon dioxide. The lithium carbonate is converted to lithium oxide while remaining fixed to the beryllium oxide particles during the hot pressing step to assure uniform density throughout the compact.

  15. Formation of peripheral porosity regions around urania in zirconia-urania mixed oxide powder compact sintering

    International Nuclear Information System (INIS)

    Das, P.; Choudhury, R.

    1992-01-01

    Sintering studies of zirconia-urania mixed oxide powder compacts (in stages of 5% urania up to a maximum of 20% addition) were carried out at temperatures between 1000-1400deg C for various soaking periods. The formation of a peripheral porosity region around comparatively coarser urania particle was a characteristic feature in this mixed oxide sintered compact. At even a higher sintering temperature (1800deg C), where extensive solid solution formation takes place, this porosity region demarcates the solutionized particles from the host zirconia apparently acting as a discontinuity in the system. Relative shrinkage difference between the dissimilar particles probably contributes to the porosity regions around the minor second phase at a lower temperature while at higher temperature generation of 'Kirkendall porosity' may be responsible for such an effect. (orig.)

  16. Constrained Sintering in Fabrication of Solid Oxide Fuel Cells

    Science.gov (United States)

    Lee, Hae-Weon; Park, Mansoo; Hong, Jongsup; Kim, Hyoungchul; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook

    2016-01-01

    Solid oxide fuel cells (SOFCs) are inevitably affected by the tensile stress field imposed by the rigid substrate during constrained sintering, which strongly affects microstructural evolution and flaw generation in the fabrication process and subsequent operation. In the case of sintering a composite cathode, one component acts as a continuous matrix phase while the other acts as a dispersed phase depending upon the initial composition and packing structure. The clustering of dispersed particles in the matrix has significant effects on the final microstructure, and strong rigidity of the clusters covering the entire cathode volume is desirable to obtain stable pore structure. The local constraints developed around the dispersed particles and their clusters effectively suppress generation of major process flaws, and microstructural features such as triple phase boundary and porosity could be readily controlled by adjusting the content and size of the dispersed particles. However, in the fabrication of the dense electrolyte layer via the chemical solution deposition route using slow-sintering nanoparticles dispersed in a sol matrix, the rigidity of the cluster should be minimized for the fine matrix to continuously densify, and special care should be taken in selecting the size of the dispersed particles to optimize the thermodynamic stability criteria of the grain size and film thickness. The principles of constrained sintering presented in this paper could be used as basic guidelines for realizing the ideal microstructure of SOFCs. PMID:28773795

  17. Process for obtaining sintered conglomerates with a high density of rare earth oxides and actinides

    International Nuclear Information System (INIS)

    Pasto, A.E.

    1974-01-01

    The invention concerns a method to produce agglomerates of actinide and rare earth oxides possessing a cubic-monoclinic transformation in order to obtain high densities close to the theoretical density, and the articles produced by the method. The process is based on the use of a rare earth or actinide oxide, in particular Eu 2 O 3 , with a cubic-monoclinic phase transformation, the oxide being sintered by hot compression at a temperature 50 deg C to 100 deg C above the transformation temperature. The sintered agglomerates obtained can have a purity of at least 99.9% and a density of practically 100%. These agglomerates are suitable in particular for the formation of nuclear reactor control rods [fr

  18. Cermet sintering on the oase of molybdenum, nickel, aluminium oxide in dry and wet hydrogen medium

    International Nuclear Information System (INIS)

    Fedotov, A.V.; Lutskaya, E.Eh.

    1985-01-01

    Cermet sintering on the base of molybdenum, nickel and aluminium oxide in dry and wer hydrogen medium is studied. It is stated that presence of water vapours permits to decrease sintering temperature of molybdenum containing cermets and to prepare dense nickeliferous cermets. Cermet density can he rather high at final stages of sintering that is probably conditioned by decrease of growth rate of corundum crystals. Pressing pressure activates cermet siptering at intermediate stages and it is low effective at finite stages of condensation. Constancy of relative reduction of void volume is preserved only at final stages of sintering

  19. Evaluation of thermal properties of sintered beryllium oxide produced from Indian beryl ore

    International Nuclear Information System (INIS)

    Nair, Sathi R.; Ghanwat, S.J.; Patro, P.K.; Syambabu, M.; Mawal, N.E.; Mahata, T.; Sinha, P.K.

    2014-01-01

    Beryllium oxide (BeO) ceramics possess many interesting properties such as good thermal conductivity, high electrical resistivity, high chemical and thermal stability, low dielectric constant, low dielectric loss and low neutron absorption coefficient. These properties lead to its wide use in vacuum electronics technology, nuclear technology, microelectronics and photoelectron technology. The above properties depend on the purity of the material as well as density and microstructure of the sintered body. For high temperature application thermal conductivity and thermal expansion are two important parameters. In the present study, high purity fine BeO powder has been prepared by beryllate route starting with crude beryllium hydroxide. The powder has been sintered at 1550℃ and sintered samples have been evaluated for its thermal properties

  20. The effect of sintering time on synthesis of in situ submicron {alpha}-Al{sub 2}O{sub 3} particles by the exothermic reactions of CuO particles in molten pure Al

    Energy Technology Data Exchange (ETDEWEB)

    Dikici, Burak, E-mail: burakdikici@yyu.edu.tr [Yuzuncu Yil University, Department of Mechanical Engineering, 65080 Van (Turkey); Gavgali, Mehmet [Ataturk University, Department of Mechanical Engineering, 25240 Erzurum (Turkey)

    2013-02-25

    Highlights: Black-Right-Pointing-Pointer Al-Cu/Al{sub 2}O{sub 3} composites were prepared successfully by means of hot pressing method. Black-Right-Pointing-Pointer Sintering time of the Al-CuO system effect the reaction rate and formation of Al{sub 2}O{sub 3}. Black-Right-Pointing-Pointer Increase in sintering time accelerates formation of submicron in situ {alpha}-Al{sub 2}O{sub 3} phase. Black-Right-Pointing-Pointer Hardness of the sintered composite for 30 min at 1000 Degree-Sign C increased from 60 to 174 HV. - Abstract: In this study, in situ {alpha}-Al{sub 2}O{sub 3} reinforcing particles have been successfully synthesised in an Al-Cu matrix alloy by means of the conventional Hot Pressing (HP) method. The effect of sintering time on the forming of the {alpha}-Al{sub 2}O{sub 3} phase at 1000 Degree-Sign C was investigated using Differential Thermal Analysis (DTA), X-ray Diffraction (XRD) and a Scanning Electron Microscope (SEM). The sintered composites contained thermodynamically stable {alpha}-Al{sub 2}O{sub 3} particles and {theta}-Al{sub 2}Cu eutectic phases, which were embedded in the Al-Cu matrix. The in situ {alpha}-Al{sub 2}O{sub 3} particles were generally spherical and their mean size was observed to be less than 0.5 {mu}m. The results showed that sintering time influences not only the reaction rate of copper and the formation of Al{sub 2}O{sub 3}. Also, an increase in the sintering time accelerates the formation of submicron in situ {alpha}-Al{sub 2}O{sub 3} particles and decreases the quantity of {theta}-Al{sub 2}Cu intermetallic phase in the liquid aluminium. Additionally, sintering of composite for 30 min at 1000 Degree-Sign C increased the hardness from 60 to 174 HV.

  1. Spark plasma sintering of tungsten-yttrium oxide composites from chemically synthesized nanopowders and microstructural characterization

    International Nuclear Information System (INIS)

    Yar, M.A.; Wahlberg, Sverker; Bergqvist, Hans; Salem, H.G.; Johnsson, Mats; Muhammed, Mamoun

    2011-01-01

    Nano-crystalline W-1%Y 2 O 3 (wt.%) powder was produced by a modified solution chemical reaction of ammonium paratungstate (APT) and yttrium nitrate. The precursor powder was found to consist of particles of bimodal morphology i.e. large APT-like particles up to 20 μm and rectangular yttrium containing ultrafine plates. After thermal processing tungsten crystals were evolved from W-O-Y plate like particles. spark plasma sintering (SPS) was used to consolidate the powder at 1100 and 1200 deg. C for different holding times in order to optimize the sintering conditions to yield high density but with reduced grain growth. Dispersion of yttrium oxide enhanced the sinterability of W powder with respect to lanthanum oxide. W-1%Y 2 O 3 composites with sub-micron grain size showed improved density and mechanical properties as compared to W-La 2 O 3 composites. Sample sintered in two steps showed improved density, due to longer holding time at lower temperature (900 deg. C) and less grain growth due to shorter holding time at higher temperature i.e. 1 min at 1100 deg. C.

  2. Development and sintering of alumina based mixed oxide ceramic products for sensor applications in petroleum industries

    Energy Technology Data Exchange (ETDEWEB)

    Yadava, Y.P.; Muniz, L.B.; Aguiar, L.A.R.; Sanguinetti Ferreira, R.A. [Departamento de Engenharia Mecanica, Universidade Federal de Pernambuco, CEP 50741-530, Recife-PE (Brazil); Albino Aguiar, J. [Departamento de Fisica, Universidade Federal de Pernambuco, CEP 50670-901 Recife-PE (Brazil)

    2005-07-01

    In petroleum production, different types of sensors are required to monitor temperature, pressure, leakage of inflammable gases, etc. These sensors work in very hostile environmental conditions and frequently suffer from abrasion and corrosion problems. Presently perovskite oxide based ceramic materials are increasingly being used for such purposes, due to their highly inert behavior in hostile environment. In the present work, we have developed and characterized alumina based complex perovskite oxide ceramics, Ba{sub 2}AlSnO{sub 5.5}. These ceramics were prepared by solid state reaction process and produced in the form of circular discs by uniaxial pressure compaction technique. Green ceramic bodies were sintered at different sintering temperatures (1200 to 1500 deg. C) in air atmosphere. Structural and microstructural characteristics of sintered Ba{sub 2}AlMO{sub 5.5} were studied by XRD and SEM techniques. Mechanical properties were tested by Vickers microhardness tests. Ceramics sintered in the temperature range 1300 deg. C 1400 deg. C presented best results in terms of microstructural characteristics and mechanical performance. (authors)

  3. Standard specification for sintered gadolinium oxide-uranium dioxide pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2008-01-01

    1.1 This specification is for finished sintered gadolinium oxide-uranium dioxide pellets for use in light-water reactors. It applies to gadolinium oxide-uranium dioxide pellets containing uranium of any 235U concentration and any concentration of gadolinium oxide. 1.2 This specification recognizes the presence of reprocessed uranium in the fuel cycle and consequently defines isotopic limits for gadolinium oxide-uranium dioxide pellets made from commercial grade UO2. Such commercial grade UO2 is defined so that, regarding fuel design and manufacture, the product is essentially equivalent to that made from unirradiated uranium. UO2 falling outside these limits cannot necessarily be regarded as equivalent and may thus need special provisions at the fuel fabrication plant or in the fuel design. 1.3 This specification does not include (1) provisions for preventing criticality accidents or (2) requirements for health and safety. Observance of this specification does not relieve the user of the obligation to be aw...

  4. Physical chemistry and modelling of the sintering of actinide oxides

    International Nuclear Information System (INIS)

    Lechelle, Jacques

    2013-01-01

    This report gives a synthesis of the work I have carried out or to which I have numerically contributed to from 1996 up to 2012 in the Department of Plutonium Uranium and minor Actinides in Cadarache CEA Center. Their main goal is the study and the modeling of the sintering process of nuclear fuels which is the unifying thread of this document. Both in order to take into account the physical and chemical features of the actinide bearing oxide material and in order to combine the different transport phenomena leading to sintering, a sub-granular scale model is under development. Extension to a varying chemical composition as well as exchanges with the gaseous phase are foreseen. A simulation on a larger scale (pellet scale) is ongoing in the framework of a PhD thesis. Validation means have been tested with (U,Pu)O 2 material on the scale of the pellet (Small Angle Neutron Diffusion), on the scale of powder granules (X-Ray High Resolution Micro-Tomography) and with CeO 2 at the 'Institut de Chimie Separative' in Marcoule on a single crystal scale (Environmental Scanning Electron Microscope). The required microstructure homogeneity for nuclear fuels has led to a campaign of experimental studies about the role of Cr 2 O 3 as a sintering aid. Whole of these studies improve our understanding of fuel sintering and hence leads to an improved mastering of this process. (author) [fr

  5. Effect of different sintering aids on thermo-mechanical properties and oxidation of SiC fibers - Reinforced ZrB{sub 2} composites

    Energy Technology Data Exchange (ETDEWEB)

    Sciti, D., E-mail: diletta.sciti@istec.cnr.it [ISTEC-CNR, Institute of Science and Technology for Ceramics, National Research Council, Via Granarolo 64, I-48018 Faenza (Italy); Silvestroni, L. [ISTEC-CNR, Institute of Science and Technology for Ceramics, National Research Council, Via Granarolo 64, I-48018 Faenza (Italy); Saccone, G.; Alfano, D. [CIRA, Italian Aerospace Research Center, 81043 Capua (Italy)

    2013-01-15

    Reinforced zirconium diboride composites containing 15 vol% of Hi Nicalon SiC chopped fibers were hot pressed with addition of various sintering additives, Si{sub 3}N{sub 4}, ZrSi{sub 2} or MoSi{sub 2}. Depending on the sintering aid, different densification temperatures were set in the range 1650-1750 Degree-Sign C. Temperature and additive strongly influenced the matrix/fiber interface, which in turn had a strong impact on the mechanical properties and the oxidation behavior at 1650 Degree-Sign C. Even the workability, performed either by conventional machining or electro discharge machining, varied depending on the sintering additive and the secondary phases formed in the system. The system containing Si{sub 3}N{sub 4} turned out to have the highest mechanical properties, but intermediate oxidation resistance; the composite containing ZrSi{sub 2} had the lowest sintering temperature, but displayed the worst oxidation resistance, and finally the composite containing MoSi{sub 2} showed intermediate mechanical properties, but the highest oxidation resistance and lowest degree of damage upon machining. Preliminary measurements of thermal shock resistance by the water quenching method were also carried out. -- Highlights: Black-Right-Pointing-Pointer We produced SiC fibers reinforced ZrB{sub 2} using different sintering aids. Black-Right-Pointing-Pointer The sintering additives affected properties, oxidation and machinability. Black-Right-Pointing-Pointer The system containing Si{sub 3}N{sub 4} had the highest mechanical properties. Black-Right-Pointing-Pointer The composite containing MoSi{sub 2} had the highest oxidation resistance. Black-Right-Pointing-Pointer ZrB{sub 2}-SiC fibers have higher thermal shock resistance than ZrB{sub 2}-SiC particles.

  6. On the sintering kinetics in UO2

    International Nuclear Information System (INIS)

    Marajofsky, A.

    1998-01-01

    The fabrication process of UO 2 pellets from powders involve pressing and a sintering anneal at high temperature (1650 deg. C to 1750 deg. C) during two or more hours in a hydrogen atmosphere. An alternative method is the oxidative sintering, made at lower temperature (1000 deg. C to 1300 deg. C) in a CO 2 or CO/CO 2 atmosphere. The sintering phenomena consist in the densification of the material by a thermal treatment below the fusion point. For a compact made by pressing a powder, sintering is the process of annulation of the porosity present in the compact or pellet. Several theories describe the sintering phenomena dividing it in three stages, initial, intermediate and final: in all of them the densification is a continuous growing function of time. Nevertheless it has been experimentally reported that a reduction of the density occurs in the third step of the sintering. The phenomena has been called solarization. Solarization has been attributed to the effect of the evolved gases from additives or to the CO 2 atmosphere in oxidative sintering. Thus, it is convenient to distinguish between solarization in oxidative or reducing conditions. Reducing solarization is a consequence of the tendency towards equilibrium of intergranular pores. In oxidative sintering it occurs in the reducing anneal after the sintering and is due to the change in the lattice parameter. This work shows examples of both types of solarization and qualitative interpretation of this phenomena. Both situations show the need of strict control of the sintering and powder production conditions. (author)

  7. Effect of coating density on oxidation resistance and Cr vaporization from solid oxide fuel cell interconnects

    Science.gov (United States)

    Talic, Belma; Falk-Windisch, Hannes; Venkatachalam, Vinothini; Hendriksen, Peter Vang; Wiik, Kjell; Lein, Hilde Lea

    2017-06-01

    Manganese cobalt spinel oxides are promising materials for protective coatings for solid oxide fuel cell (SOFC) interconnects. To achieve high density such coatings are often sintered in a two-step procedure, involving heat treatment first in reducing and then in oxidizing atmospheres. Sintering the coating inside the SOFC stack during heating would reduce production costs, but may result in a lower coating density. The importance of coating density is here assessed by characterization of the oxidation kinetics and Cr evaporation of Crofer 22 APU with MnCo1.7Fe0.3O4 spinel coatings of different density. The coating density is shown to have minor influence on the long-term oxidation behavior in air at 800 °C, evaluated over 5000 h. Sintering the spinel coating in air at 900 °C, equivalent to an in-situ heat treatment, leads to an 88% reduction of the Cr evaporation rate of Crofer 22 APU in air-3% H2O at 800 °C. The air sintered spinel coating is initially highly porous, however, densifies with time in interaction with the alloy. A two-step reduction and re-oxidation heat treatment results in a denser coating, which reduces Cr evaporation by 97%.

  8. A study of emission property and microstructure of rare earth oxide-molybdenum cermet cathode materials made by spark plasma sintering

    International Nuclear Information System (INIS)

    Wang Jinshu; Li Hongyi; Yang Sa; Cui Ying; Zhou Meiling

    2004-01-01

    A fast sintering method, spark plasma sintering (SPS) was used for the synthesis of rare earth oxide-molybdenum cathode material. The secondary emission property, microstructure, and phase constitution of materials have been studied in this paper. The experimental results show that the maximum secondary emission coefficient of this material can be high to 3.84, much higher than that of rare earth oxide-molybdenum cathode made by traditional sintering method. The grain size is less than 1 μm and rare earth distributed evenly in the material. After the material was activated at 1600 deg. C, a 4 μm layer of rare earth oxide which leads to the high secondary emission coefficient of the material, is formed on the surface of the cathode

  9. Effect of High Speed Sintering on the Properties of Zirconia Oxide Materials

    Science.gov (United States)

    2018-03-22

    12. REPORT TYPE 22/03/2018 Poster 4. TITLE AND SUBTITLE Effect of High-Speed Sintering on the Properties ofZirconia-Oxide Materials 6. AUTHOR(S...2018-03/24/2018 Sa. CONTRACT NUMBER Sb. GRANT NUMBER Sc. PROGRAM ELEMENT NUMBER Sd. PROJECT NUMBER Se. TASK NUMBER Sf. WORK UNIT NUMBER 8

  10. Laser sintering of copper nanoparticles

    International Nuclear Information System (INIS)

    Zenou, Michael; Saar, Amir; Ermak, Oleg; Kotler, Zvi

    2014-01-01

    Copper nanoparticle (NP) inks serve as an attractive potential replacement to silver NP inks in functional printing applications. However their tendency to rapidly oxidize has so far limited their wider use. In this work we have studied the conditions for laser sintering of Cu-NP inks in ambient conditions while avoiding oxidation. We have determined the regime for stable, low-resistivity copper (< ×3 bulk resistivity value) generation in terms of laser irradiance and exposure duration and have indicated the limits on fast processing. The role of pre-drying conditions on sintering outcome has also been studied. A method, based on spectral reflectivity measurements, was used for non-contact monitoring of the sintering process evolution. It also indicates preferred spectral regions for sintering. Finally, we illustrated how selective laser sintering can generate high-quality, fine line (<5 µm wide) and dense copper circuits. (paper)

  11. In situ transmission electron microscopy and scanning transmission electron microscopy studies of sintering of Ag and Pt nanoparticles

    International Nuclear Information System (INIS)

    Asoro, M.A.; Ferreira, P.J.; Kovar, D.

    2014-01-01

    Transmission electron microscopy and scanning transmission electron microscopy studies were conducted in situ on 2–5 nm Pt and 10–40 nm Ag nanoparticles to study mechanisms for sintering and to measure relevant sintering kinetics in nanoscale particles. Sintering between two separated particles was observed to initiate by either (1) diffusion of the particles on the sample support or (2) diffusion of atoms or small clusters of atoms to the neck region between the two particles. After particle contact, the rate of sintering was controlled by atomic surface diffusivity. The surface diffusivity was determined as a function of particle size and temperature from experimental measurements of the rate of neck growth of the particles. The surface diffusivities did not show a strong size effect for the range of particle sizes that were studied. The surface diffusivity for Pt nanoparticles exhibited the expected Arrhenius temperature dependence and did not appear to be sensitive to the presence of surface contaminants. In contrast, the surface diffusivity for Ag nanoparticles was affected by the presence of impurities such as carbon. The diffusivities for Ag nanoparticles were consistent with previous measurements of bulk surface diffusivities for Ag in the presence of C, but were significantly slower than those obtained from pristine Ag

  12. Immobilization of Radioactive Rare Earth oxide Waste by Solid Phase Sintering

    International Nuclear Information System (INIS)

    Ahn, Byung Gil; Park, Hwan Seo; Kim, Hwan Young; Lee, Han Soo; Kim, In Tae

    2010-01-01

    In the pyroprocessing of spent nuclear fuels, LiCl-KCl waste salt containing radioactive rare earth chlorides are generated. The radioactive rare earth oxides are recovered by co-oxidative precipitation of rare earth elements. The powder phase of rare earth oxide waste must be immobilized to produce a monolithic wasteform suitable for storage and ultimate disposal. The immobilization of these waste developed in this study involves a solid state sintering of the waste with host borosilicate glass and zinc titanate based ceramic matrix (ZIT). And the rare-earth monazite which synthesised by reaction of ammonium di-hydrogen phosphate with the rare earth oxides waste, were immobilized with the borosilicate glass. It is shown that the developed ZIT ceramic wasteform is highly resistant the leaching process, high density and thermal conductivity.

  13. Investigation of the Sintering Process Using Non-Contact Electromagnetic Acoustic Transducers

    International Nuclear Information System (INIS)

    James C. Foley; David K. Rehbein; Daniel J. Barnard

    2001-01-01

    In-situ characterizations of green state part density and sintering state have long been desired in the powder metal community. Recent advances in non-contact electromagnetic acoustic transducer (EMAT) technology have enabled in-situ monitoring of acoustic amplitude and velocity as sintering proceeds. Samples were made from elemental powders of Al (99.99%), Al (99.7%), Ag, (99.99%), Cu (99.99%) and Fe (99.9%). The powders were pressed in a uniaxial die and examined with acoustic waves for changes in velocity and amplitude during sintering for the samples containing Al, Ag, and Cu. The changes in acoustic properties were correlated with sample microstructures and mechanical properties. Evolution of a series of reverberating echoes during sintering is shown to provide information on the state of sintering, and changes in sintering kinetics as well as having the potential for detection of interior flaws

  14. In-situ anatase phase stabilization of titania photocatalyst by sintering in presence of Zr4+ organic salts

    Science.gov (United States)

    Strini, Alberto; Sanson, Alessandra; Mercadelli, Elisa; Bendoni, Riccardo; Marelli, Marcello; Dal Santo, Vladimiro; Schiavi, Luca

    2015-08-01

    The direct in-situ stabilization of an anatase-based nanocrystalline photocatalyst (Degussa P25) was obtained by sintering the catalyst powder in presence of Zr4+ organic salts. This approach allows the doping of an already-formed nanocrystalline photocatalyst instead of introducing the dopant in the crystal lattice during the catalyst synthesis. The procedure was demonstrated by the production of thick ceramic layers using the screen printing technique. This new method allows to easily stabilize the anatase phase 200 °C higher than the undoped P25 maintaining the same photocatalytic activity. The process was studied using specifically formulated screen-printing inks added with Zr4+ organic salt at 1% and 2% Zr/Ti molar ratio. The anatase phase stability was investigated in the 500-900 °C temperature range analysing the resulting catalysts with XRD, TEM and (S)TEM-EDS. The catalytic activity of the screen-printed layers was assessed by measuring the degradation of toluene in air at ambient concentration (500 nmol m-3) and low UV-A irradiance (180 μW cm-2). The described in-situ stabilization method could be potentially applied to any deposition process involving already formed anatase photocatalyst, allowing higher sintering temperature and then an improved mechanical stability of the active layers without photocatalytic activity degradation.

  15. An easily sintered, chemically stable, barium zirconate-based proton conductor for high-performance proton-conducting solid oxide fuel cells

    KAUST Repository

    Sun, Wenping; Shi, Zhen; Liu, Mingfei; Bi, Lei; Liu, Wei

    2014-01-01

    Yttrium and indium co-doped barium zirconate is investigated to develop a chemically stable and sintering active proton conductor for solid oxide fuel cells (SOFCs). BaZr0.8Y0.2-xInxO3- δ possesses a pure cubic perovskite structure. The sintering

  16. Sintered nuclear fuel compact and method for its production

    International Nuclear Information System (INIS)

    Peehs, M.; Dorr, W.

    1988-01-01

    This patent describes a method of producing a sintered nuclear fuel compact with which reactivity losses in a nuclear reactor having long fuel element cycles are avoided, which comprises, forming a compact of a mixture of powders containing at least one nuclear fuel oxide selected from the group consisting of UO/sub 2/, PuO/sub 2/, ThO/sub 2/, mixed oxide (U, Pu)O/sub 2/ and mixed oxide (U, Th)O/sub 2/, at least one neutron poison selected from the group consisting of UB/sub x/, where x=2; 4 and/or 12 and B/sub 4/C, and sintering the compact of the mixture of powders so that the neutron piston is embedded in a sintered matrix of the nuclear fuel oxide at a treatment temperature in a range from 1000 0 C to 1400 0 C in an oxidizing sintering atmosphere, and then heat treating the sintered compact in a reducing gas atmosphere

  17. Metallographic preparation of sintered oxides, carbides and nitrides of uranium and plutonium

    International Nuclear Information System (INIS)

    Martin, A.; Arles, L.

    1967-12-01

    We describe the methods of polishing, attack and coloring used at the section of plutonium base ceramics studies. These methods have stood the test of experience on the uranium and plutonium carbides, nitrides and carbonitrides as well on the mixed uranium and plutonium oxides. These methods have been particularly adapted to fit to the low dense and sintered samples [fr

  18. Guideline tests on the corrosion of sintered uranium oxide by lead and sodium about 450 deg. C

    International Nuclear Information System (INIS)

    Portnoff, A.; Pointud, R.

    1958-05-01

    Within the frame of the investigation of behaviour of a fuel element (such as UO 2 ) under irradiation, the authors report the study of the physical-chemical action of the coolant at different temperatures on the body to be irradiated. Thus, sintered uranium oxide has been submitted to corrosion by lead and by sodium during 250 hours at temperatures between 400 and 500 C. The physical characteristics of the UO 2 powder and of different sintered UO 2 pellets produced from this powder under different sintering processes are indicated, as well as the results of a spectrographic analysis of the sintered UO 2 . Corrosion devices, treatments and obtained results are reported for corrosion by lead and by sodium. In the latter case, extraction processes are discussed (using butyl alcohol, or melting in vaseline oil)

  19. Standard test methods for analysis of sintered gadolinium oxide-uranium dioxide pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2006-01-01

    1.1 These test methods cover procedures for the analysis of sintered gadolinium oxide-uranium dioxide pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Section Carbon (Total) by Direct CombustionThermal Conductivity Method C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide Gadolinia Content by Energy-Dispersive X-Ray Spectrometry C1456 Test Method for Determination of Uranium or Gadolinium, or Both, in Gadolinium Oxide-Uranium Oxide Pellets or by X-Ray Fluorescence (XRF) Hydrogen by Inert Gas Fusion C1457 Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction Isotopic Uranium Composition by Multiple-Filament Surface-Ioni...

  20. In-situ anatase phase stabilization of titania photocatalyst by sintering in presence of Zr4+ organic salts

    International Nuclear Information System (INIS)

    Strini, Alberto; Sanson, Alessandra; Mercadelli, Elisa; Bendoni, Riccardo; Marelli, Marcello; Dal Santo, Vladimiro; Schiavi, Luca

    2015-01-01

    Graphical abstract: - Highlights: • Existing commercial (P25) anatase was stabilized in-situ with Zr(IV) doping. • Highly active catalytic layers were obtained by screen-printing. • Increased thermal stability was demonstrated up to 200 °C without activity loss. • Enhanced activity was obtained because of the Zr(IV) doping. • Zirconium diffusion was assessed by STEM-EDS analysis. - Abstract: The direct in-situ stabilization of an anatase-based nanocrystalline photocatalyst (Degussa P25) was obtained by sintering the catalyst powder in presence of Zr 4+ organic salts. This approach allows the doping of an already-formed nanocrystalline photocatalyst instead of introducing the dopant in the crystal lattice during the catalyst synthesis. The procedure was demonstrated by the production of thick ceramic layers using the screen printing technique. This new method allows to easily stabilize the anatase phase 200 °C higher than the undoped P25 maintaining the same photocatalytic activity. The process was studied using specifically formulated screen-printing inks added with Zr 4+ organic salt at 1% and 2% Zr/Ti molar ratio. The anatase phase stability was investigated in the 500–900 °C temperature range analysing the resulting catalysts with XRD, TEM and (S)TEM-EDS. The catalytic activity of the screen-printed layers was assessed by measuring the degradation of toluene in air at ambient concentration (500 nmol m −3 ) and low UV-A irradiance (180 μW cm −2 ). The described in-situ stabilization method could be potentially applied to any deposition process involving already formed anatase photocatalyst, allowing higher sintering temperature and then an improved mechanical stability of the active layers without photocatalytic activity degradation

  1. Flash sintering of ceramic materials

    Science.gov (United States)

    Dancer, C. E. J.

    2016-10-01

    During flash sintering, ceramic materials can sinter to high density in a matter of seconds while subjected to electric field and elevated temperature. This process, which occurs at lower furnace temperatures and in shorter times than both conventional ceramic sintering and field-assisted methods such as spark plasma sintering, has the potential to radically reduce the power consumption required for the densification of ceramic materials. This paper reviews the experimental work on flash sintering methods carried out to date, and compares the properties of the materials obtained to those produced by conventional sintering. The flash sintering process is described for oxides of zirconium, yttrium, aluminium, tin, zinc, and titanium; silicon and boron carbide, zirconium diboride, materials for solid oxide fuel applications, ferroelectric materials, and composite materials. While experimental observations have been made on a wide range of materials, understanding of the underlying mechanisms responsible for the onset and latter stages of flash sintering is still elusive. Elements of the proposed theories to explain the observed behaviour include extensive Joule heating throughout the material causing thermal runaway, arrested by the current limitation in the power supply, and the formation of defect avalanches which rapidly and dramatically increase the sample conductivity. Undoubtedly, the flash sintering process is affected by the electric field strength, furnace temperature and current density limit, but also by microstructural features such as the presence of second phase particles or dopants and the particle size in the starting material. While further experimental work and modelling is still required to attain a full understanding capable of predicting the success of the flash sintering process in different materials, the technique non-etheless holds great potential for exceptional control of the ceramic sintering process.

  2. Contribution to the study of the sintering of uranium oxide; Contribution a l'etude du frittage de l'oxyde d'uranium

    Energy Technology Data Exchange (ETDEWEB)

    Bel, A; Carteret, Y [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1958-07-01

    The sintering ofnium oxide has been considered and the following factors have been particularly taken in consideration: - the particle size and the particles in shape of the initial powder, - the specific area of the initial powder, - the chemical composition of the oxide, - and the medium in which the sintering was carried out. A method of sintering uranium oxide on semi-industrial scale is presented. (author)Fren. [French] On xamine l'influence de differents facteurs sur le frittage de l'oxyde d'uranium. Sont particulierement prises en consideration: - la taille et la forme des grains de la poudre initiale, - la surface specifique de la poudre initiale, - la composition chimique de l'oxyde, - ainsi que la nature de l'atmosphere durant le frittage. D'autre part, une technique de frittage de l'oxyde d'uranium a l'echelle semi-industrielle est presentee. (auteur)

  3. Mechanical properties of thermoelectric n-type magnesium silicide synthesized employing in situ spark plasma reaction sintering

    Science.gov (United States)

    Muthiah, Saravanan; Singh, R. C.; Pathak, B. D.; Dhar, Ajay

    2017-07-01

    Thermoelectric devices employing magnesium silicide (Mg2Si) offer an inexpensive and non-toxic solution for green energy generation compared to other existing conventional thermoelectric materials in the mid-temperature range. However, apart from the thermoelectric performance, their mechanical properties are equally important in order to avoid the catastrophic failure of their modules during actual operation. In the present study, we report the synthesis of Mg2Si co-doped with Bi and Sb employing in situ spark plasma reaction sintering and investigate its broad range of mechanical properties. The mechanical properties of the sintered co-doped Mg2Si suggest a significantly enhanced value of hardness ~5.4  ±  0.2 GPa and an elastic modulus ~142.5  ±  6 GPa with a fracture toughness of ~1.71  ±  0.1 MPa  √m. The thermal shock resistance, which is one of the most vital parameter for designing thermoelectric devices, was found to be ~300 W m-1, which is higher than most of the other existing state-of-the-art mid-temperature thermoelectric materials. The friction and wear characteristics of sintered co-doped Mg2Si have been reported for the first time, in order to realize the sustainability of their thermoelectric modules under actual hostile environmental conditions.

  4. Microstructure and Mechanical Properties of Multiphase Strengthened Al/Si/Al_2O_3/SiO_2/MWCNTs Nano composites Sintered by In Situ Vacuum Hot Pressing

    International Nuclear Information System (INIS)

    Li, J.; Jiang, X.; Zhu, D.; Zhu, M.; Shao, Z.; Johnson, S.; Luo, Z.

    2015-01-01

    Eutectic Al/Si binary alloy is technically one of the most important Al casting alloys due to its high corrosion resistance, evident shrinkage reduction, low thermal expansion coefficient, high fluidity, and good weldability. In this work, multi phased Al/Si matrix nano composites reinforced with Al_2O_3 and multi walled carbon nano tubes (MWCNTs) have been sintered by an in situ vacuum hot-pressing method. The alumina Al_2O_3 nanoparticles were introduced by an in situ reaction of Al with SiO_2. Microstructure and mechanical properties of the sintered Al/Si/Al_2O_3/SiO_2/MWCNTs nano composites with different alumina contents were investigated. The mechanical properties were determined by micro-Vickers hardness and compressive and shear strength tests. The results demonstrated that in situ alumina and MWCNTs had impacts on microstructure and mechanical properties of the nano composites. Based on the mechanical properties and microstructure of the nano composites, strengthening and fracture mechanisms by multiple reinforcements were analyzed

  5. Effect of surface treatments on the bond strength between resin cement and differently sintered zirconium-oxide ceramics.

    Science.gov (United States)

    Yenisey, Murat; Dede, Doğu Ömür; Rona, Nergiz

    2016-01-01

    This study investigated the effects of surface treatments on bond strength between resin cement and differently sintered zirconium-oxide ceramics. 220 zirconium-oxide ceramic (Ceramill ZI) specimens were prepared, sintered in two different period (Short=Ss, Long=Ls) and divided into ten treatment groups as: GC, no treatment; GSil, silanized (ESPE-Sil); GSilPen, silane flame treatment (Silano-Pen); GSb, sandblasted; GSbSil, sandblasted+silanized; GSbCoSil, sandblasted+silica coated (CoJet)+silanized; GSbRoSil, sandblasted+silica coated (Rocatech-Plus)+silanized; GSbDSil, sandblasted+diamond particle abraded (Micron MDA)+silanized; GSbSilPen, sandblasted+silane flame treatment+silanized; GSbLSil, sandblasted+Er:Yag (Asclepion-MCL30) laser treated+silanized. The composite resin (Filtek Z-250) cylinders were cemented to the treated ceramic surfaces with a resin cement (Panavia F2.0). Shear bond strength test was performed after specimens were stored in water for 24h and thermo-cycled for 6000 cycles (5-55 °C). Data were statistically analyzed with two-way analysis of variance (ANOVA) and Tamhane's multiple comparison test (α=0.05). According to the ANOVA, sintering time, surface treatments and their interaction were statistically significant (pzirconium-oxide ceramics. Copyright © 2015 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

  6. Discrimination symbol applying method for sintered nuclear fuel product

    International Nuclear Information System (INIS)

    Ishizaki, Jin

    1998-01-01

    The present invention provides a symbol applying method for applying discrimination information such as an enrichment degree on the end face of a sintered nuclear product. Namely, discrimination symbols of information of powders are applied by a sintering aid to the end face of a molded member formed by molding nuclear fuel powders under pressure. Then, the molded product is sintered. The sintering aid comprises aluminum oxide, a mixture of aluminum oxide and silicon dioxide, aluminum hydride or aluminum stearate alone or in admixture. As an applying means of the sintering aid, discrimination symbols of information of powders are drawn by an isostearic acid on the end face of the molded product, and the sintering aid is sprayed thereto, or the sintering aid is applied directly, or the sintering aid is suspended in isostearic acid, and the suspension is applied with a brush. As a result, visible discrimination information can be applied to the sintered member easily. (N.H.)

  7. Sintering effect on material properties of electrochemical reactors used for removal of nitrogen oxides and soot particles emitted from diesel engines

    DEFF Research Database (Denmark)

    He, Zeming; Andersen, Kjeld Bøhm; Keel, Li

    2010-01-01

    In the present work, 12-layered electrochemical reactors (comprising five cells) with a novel configuration including supporting layer lanthanum strontium manganate (LSM)-yttria stabilised zirconia (YSZ), electrode layer LSM-gadolinia-doped cerium oxide (CGO) and electrolyte layer CGO were...... fabricated via the processes of slurry preparation, tape casting and lamination and sintering. The parameters of porosity, pore size, pore size distribution, shrinkage, flow rate of the sintered reactors and the electrical conductivities of the supporting layer and the electrode in the sintered reactors were...... characterised. The effect of sintering temperature on microstructures and properties of the sintered samples was discussed, and 1,250 °C was determined as the appropriate sintering temperature for reactor production based on the performance requirements for applications. Using the present ceramic processing...

  8. Study and fabrication of solid oxide fuel cells through tape casting and co-sintering

    International Nuclear Information System (INIS)

    Grosjean, A.

    2004-11-01

    This work is dedicated to the devising of a low-cost fabrication process of solid oxide fuel cells (SOFC). Technical requirements impose the shaping method: stripe casting as well as the materials used: Yttria-stabilized zirconia (YSZ), nickel and lanthanum manganite doped with strontium (LSM). In order to comply with environmental requirements the developed process uses an aqueous barbotine solvent. We get electrodes and the electrolyte separately, the use of an absorbent drying process has enabled us to join 3 layers to form an elementary cell with great interfacial homogeneity. The resistance of the cell to sintering has been improved through the symmetrization of the deformations of the cell. In order to interpret the low electrical properties of the cell and its quick damaging, transmission microscopy studies have been performed. These studies have shown 2 facts. First, 2 isolating phases appear at the cathode (at the LSM/YSZ interface) because of a too high sintering temperature and secondly, a quick clustering of nickel grains appears during cell operation that leads to a local loss of the nickel grid percolation. This problem has been solved by increasing the size of nickel oxide grains from 0.5 μm to 3 μm) to stabilize the microstructure. The issue of the reactivity at the LSM/YSZ interfaces was tackled in 2 different ways, we have tried to lower the sintering temperature by using a zirconia nano-powder first and then by replacing zirconia in the electrolyte by gadolinium-doped ceria. The use of zirconia nano-powder has failed to decrease sintering temperature while preserving the electrolyte density and the use of ceria has triggered instabilities that have not yet been solved. Despite all these drawbacks, this process allows the fabrication of an excellent anode/electrolyte interface. (A.C.)

  9. Mechanical characteristics of microwave sintered silicon carbide

    Indian Academy of Sciences (India)

    Unknown

    sintered process, SiC grain gets oxidized producing SiO2 (∼ 32 wt%) and deteriorates the quality of the product substantially. Partially sintered .... product, could be due to oxidation of SiC, e.g. 50% weight gain of a green SiC sample ... because, the charging current is 90° advanced in phase, ideally, with respect to the ...

  10. The age and significance of in-situ sinter at the Te Kopia thermal area, Taupo Volcanic Zone, New Zealand

    Energy Technology Data Exchange (ETDEWEB)

    Martin, Rod; Rodgers, Kerry A. [Auckland Univ., Dept. of Geology, Auckland (New Zealand); Mildenhall, Dallas C. [Institute of Geological and Nuclear Sciences, Lower Hutt (New Zealand); Browne, Patrick R.L. [Auckland Univ., Dept. of Geology, Auckland (New Zealand); Auckland Univ., Geothermal Inst., Auckland (New Zealand)

    2000-06-01

    One hundred pollen grains and spores, recovered from a single sample of in situ silica sinter from the Te Kopia geothermal field, include some from a podocarp forest that grew in a temperate, frost-free climate, unlike that of today, as indicated by the presence of Ascarina. Also present are pollen from taxa introduced within the last 100 years. Ascarina has been absent from the area since at least 1800 B.P. and its presence in the sinter indicates that alkali chloride waters discharged at the surface of Te Kopia before 1800 B.P., and possibly before 3500 B.P. Although palynology is a powerful tool to place age limits on fluctuations in the shallow hydrology of geothermal fields, interpretation must be moderated by considering the present flora and also changes in both local and regional flora, habitat and climate. (Author)

  11. In situ evaluation of supersolidus liquid phase sintering phenomena of stainless steel 316L: Densification and distortion

    Science.gov (United States)

    Bollina, Ravi

    Supersolidus liquid phase sintering (SLPS) is a variant of liquid phase sintering. In SLPS, prealloyed powders are heated between the solidus and liquidus temperature of the alloy. This thesis focuses on processing of stainless steel 316L via SLPS by adding boron. Various amounts of boron were added to study the effect of boron on densification and distortion. The sintering window for water atomized 316L with 0.2% boron ranges from 1430 to 1435°C and 1225 to 1245°C for water atomized 316L with 0.8% boron. The rate of change of liquid content with temperature dVL/dt decreases from 1.5%/°C to 0.1%/°C for in increase in boron content from 0 to 0.8%, giving a wider range and better control during sintering. Further; effect of boron on mechanical properties and corrosion properties was researched. It was possible to achieve tensile strength of 476+/-21 MPa and an yield strength of 250+/-5 MPa with an elongation of 15+/-2 % in water atomized 316L with 0.8% boron. Fracture analysis indicates the presence of a brittle boride phase along the grain boundary causing intergranular fracture resulting in poor ductility. The crux of this thesis discusses the evolution of apparent viscosity and its relation to the microstructure. Beam bending viscometry was successfully used to evaluate the in situ apparent viscosity evolution of water atomized 316L with 0.2 and 0.8% boron additions. The apparent viscosity drops from 174 GPa.s at 1200°C to 4 GPa.s at 1275°C with increasing fractional liquid coverage in the water atomized 316L with 0.8% boron. The apparent viscosity calculated from bending beam and was used as an input into a finite element model (FEM) derived from constitutive equations and gives an excellent, fit between simulation and experiment. The densification behavior of boron doped stainless steel was modelled using Master Sintering Curve (MSC) (based on work of sintering) for the first time. It is proven that MSC can be used to identify change in densification rate

  12. Coupling in-situ X-ray micro- and nano-tomography and discrete element method for investigating high temperature sintering of metal and ceramic powders

    Directory of Open Access Journals (Sweden)

    Yan Zilin

    2017-01-01

    Full Text Available The behaviour of various powder systems during high temperature sintering has been investigated by coupling X-ray microtomography and discrete element method (DEM. Both methods are particularly relevant to analyse particle interactions and porosity changes occurring during sintering. Two examples are presented. The first one deals with a copper powder including artificially created pores which sintering has been observed in situ at the European synchrotron and simulated by DEM. 3D images with a resolution of 1.5 μm have been taken at various times of the sintering cycle. The comparison of the real displacement of particle centers with the displacement derived from the mean field assumption demonstrates significant particle rearrangement in some regions of the sample. Although DEM simulation showed less rearrangement, it has been able to accurately predict the densification kinetics. The second example concerns multilayer ceramic capacitors (MLCCs composed of hundreds of alternated metal electrode and ceramic dielectric layers. The observation of Ni-based MLCCs by synchrotron nanotomography at Argon National Laboratory with a spatial resolution between 10 and 50 nm allowed understanding the origin of heterogeneities formed in Ni layers during sintering. DEM simulations confirmed this analysis and provided clues for reducing these defects.

  13. Current state of the Uranium dioxide sintering theory

    International Nuclear Information System (INIS)

    Baranov, V.; Devyatko, Y.; Tenishev, A.; Khlunov, A.; Khomyakov, O.

    2011-01-01

    The basic approaches to the description of the ceramics sintering phenomenon are considered. It is established that diffusive sintering models incorrectly describe an intermediate stage of this process. The physical model of sintering, considering the substance plastic flow of pressing under the influence of internal stress forces and capillary forces, as the basic mechanism defining the shrinkage of sintering oxide nuclear fuel, is offered. (authors)

  14. Bonding evolution with sintering temperature in low alloyed steels with chromium

    Directory of Open Access Journals (Sweden)

    Fuentes-Pacheco L.

    2009-01-01

    Full Text Available At present, high performance PM steels for automotive applications follow a processing route that comprises die compaction of water-atomized powder, followed by sintering and secondary treatments, and finishing operations. This study examines Cr-alloyed sintered steels with two level of alloying. In chromium-alloyed steels, the surface oxide on the powder is of critical importance for developing the bonding between the particles during sintering. Reduction of this oxide depends mainly on three factors: temperature, dew point of the atmosphere, and carbothermic reduction provided by the added graphite. The transformation of the initial surface oxide evolves sequence as temperature increases during sintering, depending on the oxide composition. Carbothermic reduction is supposed to be the controlling mechanism, even when sintering in hydrogen-containing atmospheres. The effect of carbothermic reduction can be monitored by investigating the behavior of the specimens under tensile testing, and studying the resultant fracture surfaces.

  15. Two step sintering of zirconia-escandia-ceria

    International Nuclear Information System (INIS)

    Grosso, R.L.; Muccillo, E.N.S.

    2011-01-01

    Recent reports show that the ceramic system based on zirconia-scandia-ceria is a good candidate to act as solid electrolyte in solid oxide fuel cells operating at intermediate temperatures (600-800 °C). In this work, commercial ZrO_2 containing 10 mol% scandium oxide and 1 mol% cerium oxide was sintered by the two stage method. This technique was proposed to in order to obtain ceramic materials with high density along with fine grain sizes, because it avoids the grain growth occurring in the last stage of sintering. A number of experimental conditions were fully exploited by varying the dwell temperature (T_2) and the dwell time. The peak temperature (T_1) was chosen from linear shrinkage results. High (>98%) density values were obtained using this method. The medium grain size was evaluated for selected sintered samples. X-ray diffraction patterns reveal a secondary (rhombohedral) phase in sintered samples. The intensity of the secondary phase is a function of T_1 being small for relatively higher peak temperatures. (author)

  16. An easily sintered, chemically stable, barium zirconate-based proton conductor for high-performance proton-conducting solid oxide fuel cells

    KAUST Repository

    Sun, Wenping

    2014-07-25

    Yttrium and indium co-doped barium zirconate is investigated to develop a chemically stable and sintering active proton conductor for solid oxide fuel cells (SOFCs). BaZr0.8Y0.2-xInxO3- δ possesses a pure cubic perovskite structure. The sintering activity of BaZr0.8Y0.2-xInxO3- δ increases significantly with In concentration. BaZr0.8Y0.15In0.05O3- δ (BZYI5) exhibits the highest total electrical conductivity among the sintered oxides. BZYI5 also retains high chemical stability against CO2, vapor, and reduction of H2. The good sintering activity, high conductivity, and chemical stability of BZYI5 facilitate the fabrication of durable SOFCs based on a highly conductive BZYI5 electrolyte film by cost-effective ceramic processes. Fully dense BZYI5 electrolyte film is successfully prepared on the anode substrate by a facile drop-coating technique followed by co-firing at 1400 °C for 5 h in air. The BZYI5 film exhibits one of the highest conductivity among the BaZrO3-based electrolyte films with various sintering aids. BZYI5-based single cells output very encouraging and by far the highest peak power density for BaZrO3-based proton-conducting SOFCs, reaching as high as 379 mW cm-2 at 700 °C. The results demonstrate that Y and In co-doping is an effective strategy for exploring sintering active and chemically stable BaZrO3-based proton conductors for high performance proton-conducting SOFCs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. In-situ anatase phase stabilization of titania photocatalyst by sintering in presence of Zr{sup 4+} organic salts

    Energy Technology Data Exchange (ETDEWEB)

    Strini, Alberto, E-mail: alberto.strini@itc.cnr.it [Istituto per le Tecnologie della Costruzione (ITC-CNR), via Lombardia, 49, I-20098 San Giuliano Milanese (MI) (Italy); Sanson, Alessandra; Mercadelli, Elisa [Istituto di Scienza e Tecnologia dei Materiali Ceramici (ISTEC-CNR), via Granarolo, 64, I-48018 Faenza (RA) (Italy); Bendoni, Riccardo [Istituto di Scienza e Tecnologia dei Materiali Ceramici (ISTEC-CNR), via Granarolo, 64, I-48018 Faenza (RA) (Italy); Dipartimento di Scienze e Tecnologie Chimiche e Centro NAST - Università di Roma Tor Vergata, via della Ricerca Scientifica, I-00133 Roma (Italy); Marelli, Marcello; Dal Santo, Vladimiro [CNR–Istituto di Scienze e Tecnologie Molecolari, via Golgi, 19, I-20133 Milano (Italy); Schiavi, Luca [Istituto per le Tecnologie della Costruzione (ITC-CNR), via Lombardia, 49, I-20098 San Giuliano Milanese (MI) (Italy)

    2015-08-30

    Graphical abstract: - Highlights: • Existing commercial (P25) anatase was stabilized in-situ with Zr(IV) doping. • Highly active catalytic layers were obtained by screen-printing. • Increased thermal stability was demonstrated up to 200 °C without activity loss. • Enhanced activity was obtained because of the Zr(IV) doping. • Zirconium diffusion was assessed by STEM-EDS analysis. - Abstract: The direct in-situ stabilization of an anatase-based nanocrystalline photocatalyst (Degussa P25) was obtained by sintering the catalyst powder in presence of Zr{sup 4+} organic salts. This approach allows the doping of an already-formed nanocrystalline photocatalyst instead of introducing the dopant in the crystal lattice during the catalyst synthesis. The procedure was demonstrated by the production of thick ceramic layers using the screen printing technique. This new method allows to easily stabilize the anatase phase 200 °C higher than the undoped P25 maintaining the same photocatalytic activity. The process was studied using specifically formulated screen-printing inks added with Zr{sup 4+} organic salt at 1% and 2% Zr/Ti molar ratio. The anatase phase stability was investigated in the 500–900 °C temperature range analysing the resulting catalysts with XRD, TEM and (S)TEM-EDS. The catalytic activity of the screen-printed layers was assessed by measuring the degradation of toluene in air at ambient concentration (500 nmol m{sup −3}) and low UV-A irradiance (180 μW cm{sup −2}). The described in-situ stabilization method could be potentially applied to any deposition process involving already formed anatase photocatalyst, allowing higher sintering temperature and then an improved mechanical stability of the active layers without photocatalytic activity degradation.

  18. IN-SITU FENTON OXIDATION: A CRITICAL ANALYSIS

    Science.gov (United States)

    In-situ Fenton oxidation (ISFO) is a rapidly emerging technology which involves the injection of hydrogen peroxide (H2O2) and other chemical reagents into the subsurface for the purpose of oxidizing and transforming contaminants. ISFO is being applied at an increasing number of ...

  19. Non-pressurized sintered silicon carbide with titanium carbide reinforcement

    International Nuclear Information System (INIS)

    Adler, J.

    1992-01-01

    A non-pressurized compression of SiC-TiC composite materials can be achieved via liquid phase sintering by the application of oxidic additives. Materials with TiC proportions up to 40% by volume of TiC and densities of 97 to 98% TD were produced at sintering temperatures around 1875 C. With SiC sintered in the liquid phase an increase of toughness at fracture of 80% compared with conventionally non-pressurized sintered SiC was achieved with B/C additive. No further increase could be achieved by the addition of TiC particles. However, the oxidation resistance at 1200 C was worsened. (orig.) [de

  20. Electrical sintering of silver nanoparticle ink studied by in-situ TEM probing.

    Directory of Open Access Journals (Sweden)

    Magnus Hummelgård

    Full Text Available Metallic nanoparticle inks are used for printed electronics, but to reach acceptable conductivity the structures need to be sintered, usually using a furnace. Recently, sintering by direct resistive heating has been demonstrated. For a microscopic understanding of this Joule heating sintering method, we studied the entire process in real time inside a transmission electron microscope equipped with a movable electrical probe. We found an onset of Joule heating induced sintering and coalescence of nanoparticles at power levels of 0.1-10 mW/μm³. In addition, a carbonization of the organic shells that stabilize the nanoparticles were found, with a conductivity of 4 10⁵ Sm⁻¹.

  1. High temperature oxidation-sulfidation behavior of Cr-Al2O3 and Nb-Al2O3 composites densified by spark plasma sintering

    International Nuclear Information System (INIS)

    Saucedo-Acuna, R.A.; Monreal-Romero, H.; Martinez-Villafane, A.; Chacon-Nava, J.G.; Arce-Colunga, U.; Gaona-Tiburcio, C.; De la Torre, S.D.

    2007-01-01

    The high temperature oxidation-sulfidation behavior of Cr-Al 2 O 3 and Nb-Al 2 O 3 composites prepared by mechanical alloying (MA) and spark plasma sintering (SPS) has been studied. These composite powders have a particular metal-ceramic interpenetrating network and excellent mechanical properties. Oxidation-sulfidation tests were carried out at 900 deg. C, in a 2.5%SO 2 + 3.6%O 2 + N 2 (balance) atmosphere for 48 h. The results revealed the influence of the sintering conditions on the specimens corrosion resistance, i.e. the Cr-Al 2 O 3 and Nb-Al 2 O 3 composite sintered at 1310 deg. C/4 min showed better corrosion resistance (lower weight gains) compared with those found for the 1440 deg. C/5 min conditions. For the former composite, a protective Cr 2 O 3 layer immediately forms upon heating, whereas for the later pest disintegration was noted. Thus, under the same sintering conditions the Nb-Al 2 O 3 composites showed the highest weight gains. The oxidation products were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy

  2. Mechanism of mechanochemical synthesis of complex oxides and the peculiarities of their nano-structurization determining sintering

    Directory of Open Access Journals (Sweden)

    Zyryanov V.V.

    2005-01-01

    Full Text Available A mechanism of superfast mechanosynthesis reaction for oxide systems is proposed on the base of a dynamics study. The threshold effect and linear dependence of the chemical response on the effective temperature of the reaction zone are established. Major factors are determined: molecular mass of reagents, enthalpy and difference of reagents in Mohs’s hardness, which also influence the composition of the primary product. Primary acts are characterized by a superfast roller mechanism of mass transfer with the formation of a transient dynamic state (D*. Secondary acts slowly approximate the composition of the product to the composition of the starting mixture by diffusion mass transfer in a deformation mixing regime with a contribution of a rotation (roller mechanism. The list of structure types for complex oxides derived by mechanosynthesis includes perovskites, fluorites, pyrochlors, sheelites, and some other ones. Powders of crystal products display multilevel structurization. In all studied complex oxides strong disordering of the “anti-glass” type was observed. The mechanism of sintering was studied in BaTiO3 powders of different origin and in metastable complex oxides derived by mechanosynthesis. The major contribution in shrinkage belongs to rearrangements of crystalline particles as a whole. Structure transformations accompany, as a rule, sintering of inhomogeneous powders derived by mechanosynthesis.

  3. In situ synthesis of Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composite by vacuum sintering mechanically alloyed TiAl powder coated with CNTs

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jian [Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China); Zhao, Naiqin, E-mail: nqzhao@tju.edu.cn [State Key Laboratory of Hydraulic Engineering Simulation and Safety, Tianjin (China); Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China); Nash, Philip [Thermal Processing Technology Center, Illinois Institute of Technology, IL (United States); Liu, Enzuo; He, Chunnian; Shi, Chunsheng; Li, Jiajun [Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China)

    2013-11-25

    Highlights: •Using zwitterionic surfactant to enhance the dispersion of the CNTs on the powder surface. •CNTs as carbon source decreased the formation temperature of Ti{sub 2}AlC. •Al{sub 2}O{sub 3} was generated in situ from the oxygen atoms introduced in the drying procedure. •Nanosized Ti{sub 3}Al was precipitated at 1250 °C and distribute in the TiAl matrix homogeneously. •Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composite was synthesized in situ by sintering pre-alloy Ti–Al coated with CNTs. -- Abstract: Bulk Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composites were in situ synthesized by vacuum sintering mechanically alloyed Ti–50 at.% Al powders coated with carbon nanotubes (CNTs). The pre-alloyed Ti–50 at.% Al powder was obtained by ball milling Ti and Al powders. The multi-walled carbon nanotubes as the carbon resource were covered on the surface of the pre-alloyed powders by immersing them into a water solution containing the CNTs. A zwitterionic surfactant was used to enhance the dispersion of the CNTs on the powder surface. The samples were cold pressed and sintered in vacuum at temperatures from 950 to 1250 °C, respectively. The results show that the reaction of forming Ti{sub 2}AlC can be achieved below 950 °C, which is 150 °C lower than in the Ti–Al–TiC system and 250 °C lower than for the Ti–Al–C system due to the addition of CNTs. Additionally, the reinforcement of Al{sub 2}O{sub 3} particles was introduced in situ in Ti{sub 2}AlC/TiAl by the drying process and subsequent sintering of the composite powders. Dense Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composites were obtained by sintering at 1250 °C and exhibited a homogeneous distribution of Ti{sub 2}AlC, Al{sub 2}O{sub 3} and precipitated Ti{sub 3}Al particles and a resulting high hardness.

  4. Recycling of mill scale in sintering process

    Directory of Open Access Journals (Sweden)

    El-Hussiny N.A.

    2011-01-01

    Full Text Available This investigation deals with the effect of replacing some amount of Baharia high barite iron ore concentrate by mill scale waste which was characterized by high iron oxide content on the parameters of the sintering process., and investigation the effect of different amount of coke breeze added on sintering process parameters when using 5% mill scale waste with 95% iron ore concentrate. The results of this work show that, replacement of iron ore concentrate with mill scale increases the amount of ready made sinter, sinter strength and productivity of the sinter machine and productivity at blast furnace yard. Also, the increase of coke breeze leads to an increase the ready made sinter and productivity of the sintering machine at blast furnace yard. The productivity of the sintering machine after 5% decreased slightly due to the decrease of vertical velocity.

  5. Effect of processing conditions on microstructural features in Mn–Si sintered steels

    Energy Technology Data Exchange (ETDEWEB)

    Oro, Raquel, E-mail: raqueld@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden); Hryha, Eduard, E-mail: hryha@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden); Campos, Mónica, E-mail: campos@ing.uc3m.es [Department of Materials Science and Engineering, IAAB, Universidad Carlos III de Madrid, Av. Universidad 30, 28911 Leganés, Madrid (Spain); Torralba, José M., E-mail: torralba@ing.uc3m.es [Department of Materials Science and Engineering, IAAB, Universidad Carlos III de Madrid, Av. Universidad 30, 28911 Leganés, Madrid (Spain); IMDEA Materials Institute, c/Eric Kandel, 2, 28906 Getafe, Madrid (Spain)

    2014-09-15

    Sintering of steels containing oxidation sensitive elements is possible if such elements are alloyed with others which present lower affinity for oxygen. In this work, a master alloy powder containing Fe–Mn–Si–C, specifically designed to create a liquid phase during sintering, has been used for such purpose. The effect of processing conditions such as sintering temperature and atmosphere was studied with the aim of describing the microstructural evolution as well as the morphology and distribution of oxides in the sintered material, evaluating the potential detrimental effect of such oxides on mechanical properties. Chemical analyses, metallography and fractography studies combined with X-ray photoelectron spectroscopy analyses on the fracture surfaces were used to reveal the main mechanism of fracture and their correlation with the chemical composition of the different fracture surfaces. The results indicate that the main mechanism of failure in these steels is brittle fracture in the surrounding of the original master alloy particles due to degradation of grain boundaries by the presence of oxide inclusions. Mn–Si oxide inclusions were observed on intergranular decohesive facets. The use of reducing atmospheres and high sintering temperatures reduces the amount and size of such oxide inclusions. Besides, high heating and cooling rates reduce significantly the final oxygen content in the sintered material. A model for microstructure development and oxide evolution during different stages of sintering is proposed, considering the fact that when the master alloy melts, the liquid formed can dissolve some of the oxides as well as the surface of the surrounding iron base particles. - Highlights: • Oxide distribution in steels containing oxidation-sensitive elements • Mn, Si introduced in a master alloy powder, mixed with a base iron powder • Selective oxidation of Mn and Si on iron grain boundaries • Decohesive fracture caused by degradation of grain

  6. Effect of processing conditions on microstructural features in Mn–Si sintered steels

    International Nuclear Information System (INIS)

    Oro, Raquel; Hryha, Eduard; Campos, Mónica; Torralba, José M.

    2014-01-01

    Sintering of steels containing oxidation sensitive elements is possible if such elements are alloyed with others which present lower affinity for oxygen. In this work, a master alloy powder containing Fe–Mn–Si–C, specifically designed to create a liquid phase during sintering, has been used for such purpose. The effect of processing conditions such as sintering temperature and atmosphere was studied with the aim of describing the microstructural evolution as well as the morphology and distribution of oxides in the sintered material, evaluating the potential detrimental effect of such oxides on mechanical properties. Chemical analyses, metallography and fractography studies combined with X-ray photoelectron spectroscopy analyses on the fracture surfaces were used to reveal the main mechanism of fracture and their correlation with the chemical composition of the different fracture surfaces. The results indicate that the main mechanism of failure in these steels is brittle fracture in the surrounding of the original master alloy particles due to degradation of grain boundaries by the presence of oxide inclusions. Mn–Si oxide inclusions were observed on intergranular decohesive facets. The use of reducing atmospheres and high sintering temperatures reduces the amount and size of such oxide inclusions. Besides, high heating and cooling rates reduce significantly the final oxygen content in the sintered material. A model for microstructure development and oxide evolution during different stages of sintering is proposed, considering the fact that when the master alloy melts, the liquid formed can dissolve some of the oxides as well as the surface of the surrounding iron base particles. - Highlights: • Oxide distribution in steels containing oxidation-sensitive elements • Mn, Si introduced in a master alloy powder, mixed with a base iron powder • Selective oxidation of Mn and Si on iron grain boundaries • Decohesive fracture caused by degradation of grain

  7. Photoacoustic spectroscopy investigation of sintered zinc-tin-oxide ceramics

    Directory of Open Access Journals (Sweden)

    Ivetić Tamara B.

    2007-01-01

    Full Text Available In this paper the changes that occurred in differently activated ZnO-SnO2 and sintered samples were investigated using photoacoustic spectroscopy. ZnO and SnO2 powders, mixed in the molar ratio 2:1, were mechanically activated in a planetary ball mill for 10-160 min. The mixtures were pres­sed and isothermally sintered at 1300°C for two hours. X-ray diffraction analysis of the obtained sintered samples was performed in order to investigate changes of the phase composition and confirmed only the presence of a pure zinc stannate (Zn2SnO4 phase in all the sintered samples as a result of the solid state reaction and reaction sintering between the starting ZnO and SnO2 powders. The microstructure of the sintered sam­ples was examined by scanning electron microscopy and showed that mechanical activation leads to the formation of a structure with reduced particle size which accelerates spinel formation. Grain growth of the spinel phase slows down the densification process and together with the agglomerates formed during mechanical activation causes the appearance of a porous microstructure. The photoacoustic (PA phase and amplitude spectra of the sintered samples were recorded as a function of the chopped frequency of the laser beam used (red laser with a power of 25 mW, λ=632 nm in a thermal-transmission detection configuration. PA experimental data were analyzed using the Rosenzweig-Gersho thermal-piston model, which enabled determination of the thermal diffusivity, ZT (m2s-1, diffusion coefficient of the minority free carriers D (m2s-1 and the optical absorption coefficient (m-1. The detected differences of the measured thermal-electrical properties of the obtained Zn2SnO4 ceramics indicate changes in the material induced by the different preparation procedure of the starting powders before the sintering process.

  8. In-Situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes

    Science.gov (United States)

    2010-12-28

    DATES COVERED (From - To) 1/29/10-9/30/10 4. TITLE AND SUBTITLE In situ optical studies of oxidation/reduction kinetics on SOFC cermet anodes 5a...0572 In-situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes Department of Chemistry and Biochemistry Montana State University...of Research In-situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes Principal Investigator Robert Walker Organization

  9. Determination of the initial oxidation behavior of Zircaloy-4 by in-situ TEM

    International Nuclear Information System (INIS)

    Harlow, Wayne; Ghassemi, Hessam; Taheri, Mitra L.

    2016-01-01

    The corrosion behavior of Zircaloy-4 (Zry-4), specifically by oxidation, is a problem of great importance as this material is critical for current nuclear reactor cladding. The early formation behavior and structure of the oxide layer during oxidation was studied using in-situ TEM techniques that allowed for Zry-4 to be monitored during corrosion. These environmental exposure experiments were coupled with precession electron diffraction to identify and quantify the phases present in the samples before and after the oxidation. Following short-term, high temperature oxidation, the dominant phase was revealed to be monoclinic ZrO 2 in a columnar structure. These samples oxidized in-situ contained structures that correlated well with bulk Zry-4 subjected to autoclave treatment, which were used for comparison and validation of this technique. By using in-situ TEM the effect of microstructure features, such as grain boundaries, on oxidation behavior of an alloy can be studied. The technique presented herein holds the potential to be applied any alloy system to study these effects. - Highlights: • In-situ TEM was used to oxidize samples of Zircaloy-4. • Similar behavior was found in the in-situ oxidized and autoclave-oxidized samples. • Precession diffraction was used to characterize oxide phase and texture.

  10. SINTERING OF NASCENT CALCIUM OXIDE

    Science.gov (United States)

    The paper discusses the measurement of the sintering rate of CaO in a nitrogen atmosphere at temperatures of 700-1100 C. CaO prepared from ultrapure CaCO3 was compared with an impure CaO derived from limestone. Both materials yielded an initial surface area of 104 sq m/g. The rat...

  11. In Situ Study of Thermal Stability of Copper Oxide Nanowires at Anaerobic Environment

    Directory of Open Access Journals (Sweden)

    Lihui Zhang

    2014-01-01

    Full Text Available Many metal oxides with promising electrochemical properties were developed recently. Before those metal oxides realize the use as an anode in lithium ion batteries, their thermal stability at anaerobic environment inside batteries should be clearly understood for safety. In this study, copper oxide nanowires were investigated as an example. Several kinds of in situ experiment methods including in situ optical microscopy, in situ Raman spectrum, and in situ transmission electron microscopy were adopted to fully investigate their thermal stability at anaerobic environment. Copper oxide nanowires begin to transform as copper(I oxide at about 250°C and finish at about 400°C. The phase transformation proceeds with a homogeneous nucleation.

  12. Hydrothermal Cold Sintering

    Science.gov (United States)

    Kang, Xiaoyu

    Solid state sintering transforms particle compact to a physically robust and dense polycrystalline monolith driven by reduction of surface energy and curvature. Since bulk diffusion is required for neck formation and pore elimination, sintering temperature about 2/3 of melting point is needed. It thus places limitations for materials synthesis and integration, and contributes to significant energy consumption in ceramic processing. Furthermore, since surface transport requires lower temperature than bulk processes, grain growth is often rapid and can be undesired for physical properties. For these reasons, several techniques have been developed including Liquid Phase Sintering (LPS), Hot Pressing (HP) and Field Assisted Sintering Technique (FAST), which introduce either viscous melt, external pressure or electric field to speed up densification rates at lower temperature. However, because of their inherent reliability on bulk diffusion, temperatures required are often too high for integrating polymers and non-noble metals. Reduction of sintering temperature below 400 °C would require a different densification mechanism that is based on surface transport with external forces to drive volume shrinkage. Densification method combining uniaxial pressure and solution under hydrothermal condition was first demonstrated by Kanahara's group at Kochi University in 1986 and was brought to our attention by the work of Kahari, etc, from University of Oulu on densification of Li2MoO 4 in 2015. This relatively new process showed promising ultra-low densification temperature below 300 °C, however little was known about its fundamental mechanism and scope of applications, which became the main focus of this dissertation. In this work, a uniaxial hydraulic press, a standard stainless steel 1/2 inch diameter die with heating band were utilized in densifying metal oxides. Applied pressure and sintering temperature were between 100 MPa and 700 MPa and from room temperature to 300

  13. Process Developed for Generating Ceramic Interconnects With Low Sintering Temperatures for Solid Oxide Fuel Cells

    Science.gov (United States)

    Zhong, Zhi-Min; Goldsby, Jon C.

    2005-01-01

    Solid oxide fuel cells (SOFCs) have been considered as premium future power generation devices because they have demonstrated high energy-conversion efficiency, high power density, and extremely low pollution, and have the flexibility of using hydrocarbon fuel. The Solid-State Energy Conversion Alliance (SECA) initiative, supported by the U.S. Department of Energy and private industries, is leading the development and commercialization of SOFCs for low-cost stationary and automotive markets. The targeted power density for the initiative is rather low, so that the SECA SOFC can be operated at a relatively low temperature (approx. 700 C) and inexpensive metallic interconnects can be utilized in the SOFC stack. As only NASA can, the agency is investigating SOFCs for aerospace applications. Considerable high power density is required for the applications. As a result, the NASA SOFC will be operated at a high temperature (approx. 900 C) and ceramic interconnects will be employed. Lanthanum chromite-based materials have emerged as a leading candidate for the ceramic interconnects. The interconnects are expected to co-sinter with zirconia electrolyte to mitigate the interface electric resistance and to simplify the processing procedure. Lanthanum chromites made by the traditional method are sintered at 1500 C or above. They react with zirconia electrolytes (which typically sinter between 1300 and 1400 C) at the sintering temperature of lanthanum chromites. It has been envisioned that lanthanum chromites with lower sintering temperatures can be co-fired with zirconia electrolyte. Nonstoichiometric lanthanum chromites can be sintered at lower temperatures, but they are unstable and react with zirconia electrolyte during co-sintering. NASA Glenn Research Center s Ceramics Branch investigated a glycine nitrate process to generate fine powder of the lanthanum-chromite-based materials. By simultaneously doping calcium on the lanthanum site, and cobalt and aluminum on the

  14. Microwave sintering of nano size powder β-TCP bioceramics

    Directory of Open Access Journals (Sweden)

    Mirhadi B.

    2014-01-01

    Full Text Available A nano sized beta tricalcium phosphate (β-TCP powder was conventional sintered (CS and microwave sintered (MW, in order to obtain dense β-TCP ceramics. In this work the effect of microwave sintering conditions on the microstructure, phase composition and mechanical properties of materials based on tricalcium phosphate (TCP was investigated by SEM (scanning electron microscopyand XRD(X-ray diffraction and then compared with conventional sintered samples. Nano-size β-TCP powders with average grain size of 80 nm were prepared by the wet chemical precipitation method with calcium nitrate and diammonium hydrogen phosphate as calcium and phosphorus precursors, respectively. The precipitation process employed was also found to be suitable for the production of submicrometre β-TCP powder in situ. The β-TCP samples microwave (MW sintered for 15 min at 1100°C, with average grain size of 3μm, showed better densification, higher density and certainly higher hardness than samples conventionally sintered for 2 h at the same temperature. By comparing sintered and MW sintered β-TCP samples, it was concluded that MW sintered β-TCP samples have superior mechanical properties.

  15. Excimer laser sintering of indium tin oxide nanoparticles for fabricating thin films of variable thickness on flexible substrates

    International Nuclear Information System (INIS)

    Park, Taesoon; Kim, Dongsik

    2015-01-01

    Technology to fabricate electrically-conducting, transparent thin-film patterns on flexible substrates has possible applications in flexible electronics. In this work, a pulsed-laser sintering process applicable to indium tin oxide (ITO) thin-film fabrication on a substrate without thermal damage to the substrate was developed. A nanosecond pulsed laser was used to minimize thermal penetration into the substrate and to control the thickness of the sintered layer. ITO nanoparticles (NPs) of ~ 20 nm diameter were used to lower the process temperature by exploiting their low melting point. ITO thin film patterns were fabricated by first spin coating the NPs onto a surface, then sintering them using a KrF excimer laser. The sintered films were characterized using field emission scanning electron microscopy. The electrical resistivity and transparency of the film were measured by varying the process parameters. A single laser pulse could generate the polycrystalline structure (average grain size ~ 200 nm), reducing the electrical resistivity of the film by a factor of ~ 1000. The sintering process led to a minimum resistivity of 1.1 × 10 −4 Ω·m without losing the transparency of the film. The thickness of the sintered layer could be varied up to 150 nm by adjusting the laser fluence. Because the estimated thermal penetration depth in the ITO film was less than 200 nm, no thermal damage was observed in the substrate. This work suggests that the proposed process, combined with various particle deposition methods, can be an effective tool to form thin-film ITO patterns on flexible substrates. - Highlights: • Excimer laser sintering can fabricate ITO thin films on flexible substrates. • The laser pulse can form a polycrystalline structure without thermal damage. • The laser sintering process can reduce the electrical resistivity substantially. • The thickness of the sintered layer can be varied effectively

  16. Excimer laser sintering of indium tin oxide nanoparticles for fabricating thin films of variable thickness on flexible substrates

    Energy Technology Data Exchange (ETDEWEB)

    Park, Taesoon; Kim, Dongsik, E-mail: dskim87@postech.ac.kr

    2015-03-02

    Technology to fabricate electrically-conducting, transparent thin-film patterns on flexible substrates has possible applications in flexible electronics. In this work, a pulsed-laser sintering process applicable to indium tin oxide (ITO) thin-film fabrication on a substrate without thermal damage to the substrate was developed. A nanosecond pulsed laser was used to minimize thermal penetration into the substrate and to control the thickness of the sintered layer. ITO nanoparticles (NPs) of ~ 20 nm diameter were used to lower the process temperature by exploiting their low melting point. ITO thin film patterns were fabricated by first spin coating the NPs onto a surface, then sintering them using a KrF excimer laser. The sintered films were characterized using field emission scanning electron microscopy. The electrical resistivity and transparency of the film were measured by varying the process parameters. A single laser pulse could generate the polycrystalline structure (average grain size ~ 200 nm), reducing the electrical resistivity of the film by a factor of ~ 1000. The sintering process led to a minimum resistivity of 1.1 × 10{sup −4} Ω·m without losing the transparency of the film. The thickness of the sintered layer could be varied up to 150 nm by adjusting the laser fluence. Because the estimated thermal penetration depth in the ITO film was less than 200 nm, no thermal damage was observed in the substrate. This work suggests that the proposed process, combined with various particle deposition methods, can be an effective tool to form thin-film ITO patterns on flexible substrates. - Highlights: • Excimer laser sintering can fabricate ITO thin films on flexible substrates. • The laser pulse can form a polycrystalline structure without thermal damage. • The laser sintering process can reduce the electrical resistivity substantially. • The thickness of the sintered layer can be varied effectively.

  17. The physical chemistry and materials science behind sinter-resistant catalysts.

    Science.gov (United States)

    Dai, Yunqian; Lu, Ping; Cao, Zhenming; Campbell, Charles T; Xia, Younan

    2018-06-18

    Catalyst sintering, a main cause of the loss of catalytic activity and/or selectivity at high reaction temperatures, is a major concern and grand challenge in the general area of heterogeneous catalysis. Although all heterogeneous catalysts are inevitably subjected to sintering during their operation, the immediate and drastic consequences can be mitigated by carefully engineering the catalytic particles and their interactions with the supports. In this tutorial review, we highlight recent progress in understanding the physical chemistry and materials science involved in sintering, including the discussion of advanced techniques, such as in situ microscopy and spectroscopy, for investigating the sintering process and its rate. We also discuss strategies for the design and rational fabrication of sinter-resistant catalysts. Finally, we showcase recent success in improving the thermal stability and thus sinter resistance of supported catalytic systems.

  18. Solidification of HLLW into sintered ceramics

    International Nuclear Information System (INIS)

    O-Oka, K.; Ohta, T.; Masuda, S.; Tsunoda, N.

    1979-01-01

    Simulated HLLW from the PNC reprocessing plant at Tokai was solidified into sintered ceramics by normal sintering or hot-pressing with addition of some oxides. Among various ceramic products obtained so far, the most preferable was nepheline-type sintered solids formed with addition of SiO 2 and Al 2 O 3 to the simulated waste calcine. The solid shows advantageous properties in leach rate and mechanical strength, which suggest that the ceramic solids were prepared with additions of ZrO 2 or MnO 2 , and some of them showed good characteristics

  19. Microstructures and mechanical properties of 9Cr oxide dispersion strengthened steel produced by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Xie, Rui [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); School of Metallurgy, Northeastern University, Shenyang 110819 (China); Lu, Zheng, E-mail: luz@atm.neu.edu.cn [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); Lu, Chenyang; Li, Zhengyuan [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); Ding, Xueyong [School of Metallurgy, Northeastern University, Shenyang 110819 (China); Liu, Chunming [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China)

    2017-02-15

    Highlights: • A 9Cr-ODS steel was produced by mechanical alloying and spark plasma sintering. • Bimodal grain size distribution was observed. • Formation mechanism of bimodal grain size distribution was discussed. • The size and number density of nanoscale particles were obtained by SAXS and HRTEM. • The contribution of nano-sized particles to yield strength is dominating. - Abstract: 9Cr oxide dispersion strengthened (ODS) steel was fabricated by mechanical alloying (MA) and spark plasma sintering (SPS). The nano-sized particles, grain size distribution and mechanical properties of 9Cr-ODS steel sintered at 950 °C were studied by synchrotron radiation small angle X-ray scattering (SAXS), high-resolution transmission electron microscopy (HRTEM), electron backscatter diffraction (EBSD) and tensile experiment. The results showed that bimodal grain size distribution in the matrix is observed, which is attributed to the heterogeneous recrystallization process during the SPS. High-density nano-sized Y{sub 2}Ti{sub 2}O{sub 7} and some large oxides of Cr{sub 2}Mn(Ti)O{sub 4} are formed in 9Cr-ODS steel. The number density and average size of Y{sub 2}Ti{sub 2}O{sub 7} obtained from SAXS are 4.72 × 10{sup 22}/m{sup 3} and 4.4 nm, respectively. The yield strengths of 9Cr-ODS steel fabricated by SPS are compared with the typical 9Cr-ODS steel produced by HIP.

  20. Microwave sintering of hydroxyapatite-based composites

    International Nuclear Information System (INIS)

    Fang, Y.; Roy, D.M.; Cheng, J.; Roy, R.; Agrawal, D.K.

    1993-01-01

    Composites of hydroxyapatite/partially stabilized zirconia (HAp/PSZ) and hydroxyapatite/silicon carbide whiskers (HAp/SiC) were sintered at 1100-1200 degrees C by microwave at 2.45 GHz. Characterization of the sintered composites was carried out by density, microstructure, phase composition, and fracture toughness measurements. The results show that although not yet fully densified, a much higher sintered density in the HAp/PSZ composite was achieved by microwave sintering than by conventional sintering at the same temperature. A relative density of 93% was achieved by 20 min. microwave processing at 1200 degrees C. Comparatively, 2 h conventional sintering of the same material at 1200 degrees C led to only 75.5% relative density. K IC of this microwave sintered HAp/PSZ of 93% density was found to be 3.88 MPa√m, which is 250% of the value for pure HAp of the same density. A further increase in K IC could be expected if full or nearly full densification was achieved. Sintering of PSZ particles in the HAp/PSZ composite was also observed in the microwave processed sample. Microwave sintering of HAp/SiC was not successful in the current study due to the oxidation of SiC in air at high temperature. 8 refs., 4 figs., 1 tab

  1. Effect of sintering atmosphere on the hardness of ThO2

    Science.gov (United States)

    Baena, Angela; Cardinaels, Thomas; Van Eyken, Jelle; Puzzolante, Jean Louis; Binnemans, Koen; Verwerft, Marc

    2016-08-01

    The hardness and toughness of ThO2 sintered under reducing and oxidizing conditions has been investigated and, quite unexpectedly, a significant difference in hardness was observed for the entire range of porosities studied. Reducing conditions systematically yielded higher hardness values than oxidizing conditions. Extrapolated to zero porosity, the hardness for ThO2 is H0 = 10.5 ± 0.3 GPa for oxidizing conditions and H0 = 12.4 ± 0.7 GPa for reducing conditions. Toughness values have been derived from Vickers indentations; differences in toughness were insignificant and only a single value is proposed: KIC = 0.97 ± 0.12 MPa √m. The difference in hardness is attributed to the presence of point defects, also acting as color centers and causing grey coloration of ThO2 sintered under reducing conditions. Furthermore, and of interest for nuclear fuel production, is the finding that ThO2 sintered under reducing conditions is significantly easier to grind compared to material sintered under oxidizing conditions.

  2. The influence of green microstructure and sintering parameters on precipitation process during copper-nickel-zinc ferrites sintering

    International Nuclear Information System (INIS)

    Barba, A.; Clausell, C.; Jarque, J. C.; Monzo, M.

    2014-01-01

    Microstructural changes that occur during heat treatment of copper-nickel-zinc ferrites have been studied. The process of precipitation of the two types of crystals that occur during the sintering process has been analyzed. It is found that this process depends on dry relative density of the press specimens and on the following sintering parameters: sintering temperature, sintering time and cooling rate of the thermal cycle. Crystal precipitates characterization have been done by scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) analysis, X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). These techniques have allowed to determine the nature of these crystals, which in this case correspond to zinc and copper oxides. It has been used two chemical reactions to explain the bulk precipitation and subsequent re-dissolution of these crystal precipitates during sintering. (Author)

  3. Mechanical characteristics of microwave sintered silicon carbide

    Indian Academy of Sciences (India)

    In firing of products by conventionally sintered process, SiC grain gets oxidized producing SiO2 (∼ 32 wt%) and deteriorates the quality of the product substantially. Partially sintered silicon carbide by such a method is a useful material for a varieties of applications ranging from kiln furniture to membrane material.

  4. Effect of sintering atmosphere on the hardness of ThO_2

    International Nuclear Information System (INIS)

    Baena, Angela; Cardinaels, Thomas; Van Eyken, Jelle; Puzzolante, Jean Louis; Binnemans, Koen; Verwerft, Marc

    2016-01-01

    The hardness and toughness of ThO_2 sintered under reducing and oxidizing conditions has been investigated and, quite unexpectedly, a significant difference in hardness was observed for the entire range of porosities studied. Reducing conditions systematically yielded higher hardness values than oxidizing conditions. Extrapolated to zero porosity, the hardness for ThO_2 is H_0 = 10.5 ± 0.3 GPa for oxidizing conditions and H_0 = 12.4 ± 0.7 GPa for reducing conditions. Toughness values have been derived from Vickers indentations; differences in toughness were insignificant and only a single value is proposed: K_I_C = 0.97 ± 0.12 MPa √m. The difference in hardness is attributed to the presence of point defects, also acting as color centers and causing grey coloration of ThO_2 sintered under reducing conditions. Furthermore, and of interest for nuclear fuel production, is the finding that ThO_2 sintered under reducing conditions is significantly easier to grind compared to material sintered under oxidizing conditions. - Highlights: • Reducing sintering conditions increase the hardness of polycrystalline ThO_2. • Systematic series of hardness versus porosity of ThO_2 were obtained. • Reducing sintering conditions improve grinding of ThO_2.

  5. In situ observation techniques of protective oxide layer

    International Nuclear Information System (INIS)

    Doi, Takashi; Adachi, Takeharu; Usuki, Noriaki

    2015-01-01

    In situ analyzing techniques for investigating a surface and interface change during corrosion and oxidation of metals by using Raman scattering spectroscopy (Raman), X-ray diffraction (XRD) and X-ray photoemission spectroscopy (XPS) are present. The Raman spectra revealed that a crystal structure and distribution of corrosion products varied during corrosion progress at elevated temperature and high pressure electrolyte. Time dependent XRD measurements made clear the behavior of the electrochemical reduction of a rust and the iso thermal transformation of a scale on a steel. It was demonstrated that XPS was capable of the in-situ measurements for initial stage of high temperature oxidation. (author)

  6. Improvement of the electrochromic response of a low-temperature sintered dye-modified porous electrode using low-resistivity indium tin oxide nanoparticles

    International Nuclear Information System (INIS)

    Watanabe, Yuichi; Suemori, Kouji; Hoshino, Satoshi

    2016-01-01

    An indium tin oxide (ITO) nanoparticle-based porous electrode sintered at low temperatures was investigated as a transparent electrode for electrochromic displays (ECDs). The electrochromic (EC) response of the dye-modified ITO porous electrode sintered at 150 °C, which exhibited a generally low resistivity, was markedly superior to that of a conventional dye-modified TiO 2 porous electrode sintered at the same temperature. Moreover, the EC characteristics of the dye-modified ITO porous electrode sintered at 150 °C were better than those of the high-temperature (450 °C) sintered conventional dye-modified TiO 2 porous electrode. These improvements in the EC characteristics of the dye-modified ITO porous electrode are attributed to its lower resistivity than that of the TiO 2 porous electrodes. In addition to its sufficiently low resistivity attained under the sintering conditions required for flexible ECD applications, the ITO porous film had superior visible-light transparency and dye adsorption capabilities. We conclude that the process temperature, resistivity, optical transmittance, and dye adsorption capability of the ITO porous electrode make it a promising transparent porous electrode for flexible ECD applications.

  7. Preparation of Nd–Fe–B sintered magnets from HDDR-processed powder

    Energy Technology Data Exchange (ETDEWEB)

    Takagi, Kenta, E-mail: k-takagi@aist.go.jp [Green Innovative Magnetic Materials Research Center, National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan); Akada, Misaho [Magnetic Materials R& D Center, Research Associations of Magnetic Materials for High-Efficiency Motors (MagHEM), Nagoya 463-8560 (Japan); Soda, Rikio; Ozaki, Kimihiro [Green Innovative Magnetic Materials Research Center, National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan)

    2015-11-01

    The electric-current sintering technique was used to fully densify hydrogenation–disproportionation–desorption–recombination (HDDR)-processed Nd–Fe–B powder at temperatures below the grain growth temperature in order to produce high-coercive bulk magnets. However, the sintered magnets exhibited anomalous coercivity reduction that depended on sintered density. Reheating examination of the sintered magnets revealed that the reduced coercivity was increased in proportion to the heating temperature, resulting in complete recovery of coercivity. As a result, the combination of electric-current sintering and post-annealing produced sintered magnets with a coercivity of 15 kOe. Scanning and transmission electron microscopy revealed no evidence that associated the anomalous coercivity reduction and recovery with grain boundary morphology. On the other hand, various HDDR powders with different particle sizes were sintered, and finer powders yielded lower coercivity after sintering, implying that the anomalous coercivity reduction was associated with particle surface oxides of the raw powder. - Highlights: • We conduct a sintering of HDDR-processed Nd–Fe–B powder without coercivity reduction. • Rapid current sintering allows densification of this powder without grain growth. • However, the sintered magnets show an anomalous coercivity reduction phenomenon. • It is found that post-annealing completely recovers the reduced coercivity. • The anomalous coercivity reduction would be due to surface oxide of the raw powder.

  8. Effects of sintering atmosphere and initial particle size on sintering of gadolinia-doped ceria

    International Nuclear Information System (INIS)

    Batista, Rafael Morgado

    2014-01-01

    The effects of the sintering atmosphere and initial particle size on the sintering of ceria containing 10 mol% gadolinia (GdO 1.5 ) were systematically investigated. The main physical parameter was the specific surface area of the initial powders. Nanometric powders with three different specific surface areas were utilized, 210 m 2 /g, 36,2 m 2 /g e 7,4 m 2 /g. The influence on the densification, and micro structural evolution were evaluated. The starting sintering temperature was verified to decrease with increasing on the specific surface area of raw powders. The densification was accelerated for the materials with smaller particle size. Sintering paths for crystallite growth were obtained. Master sintering curves for gadolinium-doped ceria were constructed for all initial powders. A computational program was developed for this purpose. The results for apparent activation energy showed noticeable dependence with specific surface area. In this work, the apparent activation energy for densification increased with the initial particle size of powders. The evolution of the particle size distributions on non isothermal sintering was investigated by WPPM method. It was verified that the grain growth controlling mechanism on gadolinia doped ceria is the pore drag for initial stage and beginning of intermediate stage. The effects of the sintering atmosphere on the stoichiometry deviation of ceria, densification, microstructure evolution, and electrical conductivity were analyzed. Inert, oxidizing, and reducing atmospheres were utilized on this work. Deviations on ceria stoichiometry were verified on the bulk materials. The deviation verified was dependent of the specific surface area and sintering atmosphere. Higher reduction potential atmospheres increase Ce 3+ bulk concentration after sintering. Accelerated grain growth and lower electrical conductivities were verified when reduction reactions are significantly present on sintering. (author)

  9. Short Communication on "In-situ TEM ion irradiation investigations on U3Si2 at LWR temperatures"

    Science.gov (United States)

    Miao, Yinbin; Harp, Jason; Mo, Kun; Bhattacharya, Sumit; Baldo, Peter; Yacout, Abdellatif M.

    2017-02-01

    The radiation-induced amorphization of U3Si2 was investigated by in-situ transmission electron microscopy using 1 MeV Kr ion irradiation. Both arc-melted and sintered U3Si2 specimens were irradiated at room temperature to confirm the similarity in their responses to radiation. The sintered specimens were then irradiated at 350 °C and 550 °C up to 7.2 × 1015 ions/cm2 to examine their amorphization behavior under light water reactor (LWR) conditions. U3Si2 remains crystalline under irradiation at LWR temperatures. Oxidation of the material was observed at high irradiation doses.

  10. Effect of temperature on electrical conductance of inkjet-printed silver nanoparticle ink during continuous wave laser sintering

    International Nuclear Information System (INIS)

    Lee, Dae-Geon; Kim, Dong Keun; Moon, Yoon-Jae; Moon, Seung-Jae

    2013-01-01

    To determine the effect of temperature on the specific electrical conductance of inkjet-printed ink during continuous wave laser sintering, the temperature of the sintered ink was estimated. The ink, which contained 34 wt.% silver nanoparticles with an average size of approximately 50 nm, was inkjet-printed onto a liquid crystal display glass substrate. The printed ink was irradiated with a 532 nm continuous wave laser for 60 s with various laser intensities. During laser irradiation, the in-situ electrical conductance of the sintered ink was measured to estimate the transient thermal conductivity of the ink. The electrical conductance and thermal conductivity of the ink was coupled to obtain the transient temperature by applying the Wiedemann–Franz law to a two-dimensional transient heat conduction equation. The electrical conductance of laser-sintered ink was highly dependent on the sintering temperature of the ink. - Highlights: • The in-situ electrical conductance was measured during the laser sintering process. • Wiedemann–Franz law coupled the electrical conductance with transient temperature. • The transient temperature of the laser-sintered Ag nanoparticle ink was estimated

  11. Polycrystalline oxides formation during transient oxidation of (001) Cu-Ni binary alloys studied by in situ TEM and XRD

    International Nuclear Information System (INIS)

    Yang, J.C.; Li, Z.Q.; Sun, L.; Zhou, G.W.; Eastman, J.A.; Fong, D.D.; Fuoss, P.H.; Baldo, P.M.; Rehn, L.E.; Thompson, L.J.

    2009-01-01

    The nucleation and growth of Cu 2 O and NiO islands due to oxidation of Cu x Ni 1-x (001) films were monitored, at various temperatures, by in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM) and in situ synchrotron X-ray diffraction (XRD). In remarkable contrast to our previous observations of Cu and Cu-Au oxidation, irregular-shaped polycrystalline oxide islands formed with respect to the Cu-Ni alloy film, and an unusual second oxide nucleation stage was noted. In situ XRD experiments revealed that NiO formed first epitaxially, then other orientations appeared, and finally polycrystalline Cu 2 O developed as the oxidation pressure was increased. The segregation of Ni and Cu towards or away, respectively, from the alloy surface during oxidation could disrupt the surface and cause polycrystalline oxide formation.

  12. Pressure sintering and creep deformation: a joint modeling approach

    International Nuclear Information System (INIS)

    Notis, M.R.

    1979-10-01

    Work related to microchemical and microstructural aspects of the joint modeling of pressure sintering and creep in ceramic oxides is reported. Quantitative techniques for the microchemical analysis of ceramic oxides and for the examination of impurity segregation effects in polycrystalline ceramic materials were developed. This has included fundamental absorption corrections for the oxygen anion species as a function of foil thickness. The evolution in microstructure during the transition from intermediate stage to final stage densification during hot pressing of cobalt oxide and preliminary studies with doped oxides were studied. This work shows promise in using time-integrated microstructural effects to elucidate the role of impurities in the sintering of ceramic materials

  13. Method of sintering ceramic materials

    Science.gov (United States)

    Holcombe, Cressie E.; Dykes, Norman L.

    1992-01-01

    A method for sintering ceramic materials is described. A ceramic article is coated with layers of protective coatings such as boron nitride, graphite foil, and niobium. The coated ceramic article is embedded in a container containing refractory metal oxide granules and placed within a microwave oven. The ceramic article is heated by microwave energy to a temperature sufficient to sinter the ceramic article to form a densified ceramic article having a density equal to or greater than 90% of theoretical density.

  14. Effect of sintering atmosphere on the hardness of ThO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Baena, Angela; Cardinaels, Thomas [Belgian Nuclear Research Centre (SCK-CEN), Institute for Nuclear Materials Science, Fuel Materials Group, Boeretang 200, B-2400, Mol (Belgium); KU Leuven, Department of Chemistry, Celestijnenlaan 200F, P.O. Box 2404, B-3001, Heverlee (Belgium); Van Eyken, Jelle; Puzzolante, Jean Louis [Belgian Nuclear Research Centre (SCK-CEN), Institute for Nuclear Materials Science, Fuel Materials Group, Boeretang 200, B-2400, Mol (Belgium); Binnemans, Koen [KU Leuven, Department of Chemistry, Celestijnenlaan 200F, P.O. Box 2404, B-3001, Heverlee (Belgium); Verwerft, Marc, E-mail: marc.verwerft@sckcen.be [Belgian Nuclear Research Centre (SCK-CEN), Institute for Nuclear Materials Science, Fuel Materials Group, Boeretang 200, B-2400, Mol (Belgium)

    2016-08-15

    The hardness and toughness of ThO{sub 2} sintered under reducing and oxidizing conditions has been investigated and, quite unexpectedly, a significant difference in hardness was observed for the entire range of porosities studied. Reducing conditions systematically yielded higher hardness values than oxidizing conditions. Extrapolated to zero porosity, the hardness for ThO{sub 2} is H{sub 0} = 10.5 ± 0.3 GPa for oxidizing conditions and H{sub 0} = 12.4 ± 0.7 GPa for reducing conditions. Toughness values have been derived from Vickers indentations; differences in toughness were insignificant and only a single value is proposed: K{sub IC} = 0.97 ± 0.12 MPa √m. The difference in hardness is attributed to the presence of point defects, also acting as color centers and causing grey coloration of ThO{sub 2} sintered under reducing conditions. Furthermore, and of interest for nuclear fuel production, is the finding that ThO{sub 2} sintered under reducing conditions is significantly easier to grind compared to material sintered under oxidizing conditions. - Highlights: • Reducing sintering conditions increase the hardness of polycrystalline ThO{sub 2}. • Systematic series of hardness versus porosity of ThO{sub 2} were obtained. • Reducing sintering conditions improve grinding of ThO{sub 2}.

  15. Performance of in situ chemical oxidation field demonstrations at DOE sites

    International Nuclear Information System (INIS)

    Cline, S.R.; West, O.R.; Siegrist, R.L.; Holden, W.L.

    1997-01-01

    Researchers at the Oak Ridge National Laboratory (ORNL) have been investigating the use of in situ chemical oxidation to remediate organic contaminants (VOCs, SVOCs, and PCBs) in soils and groundwater at the laboratory and field scales. Field scale design parameters (e.g., oxidant loading rates and oxidant delivery techniques) are often dictated by site conditions (e.g., soil properties and initial contaminant concentrations). Chemical destruction of organic compounds can be accomplished using a variety of oxidants. Recent research has involved field scale in situ chemical oxidation demonstrations using H 2 O 2 and KMnO 4 in conjunction with soil mixing as the oxidant delivery mechanism. A description of some of these fields activities and future field-scale work is presented here

  16. New materials through a variety of sintering methods

    Science.gov (United States)

    Jaworska, L.; Cyboroń, J.; Cygan, S.; Laszkiewicz-Łukasik, J.; Podsiadło, M.; Novak, P.; Holovenko, Y.

    2018-03-01

    New sintering techniques make it possible to obtain materials with special properties that are impossible to obtain by conventional sintering techniques. This issue is especially important for ceramic materials for application under extreme conditions. Following the tendency to limit critical materials in manufacturing processes, the use of W, Si, B, Co, Cr should be limited, also. One of the cheapest and widely available materials is aluminum oxide, which shows differences in phase composition, grain size, hardness, strain and fracture toughness of the same type of powder, sintered via various methods. In this paper the alumina was sintered using the conventional free sintering process, microwave sintering, Spark Plasma Sintering (SPS), high pressure-high temperature method (HP-HT) and High Pressure Spark Plasma Sintering (HP SPS). Phase composition analysis, by X-ray diffraction of the alumina materials sintered using various methods, was carried out. For the conventional sintering method, compacts are composed of α-Al2O3 and θ-Al2O3. For compacts sintered using SPS, microwave and HP-HT methods, χ-Al2O3 and γ-Al2O3 phases were additionally present. Mechanical and physical properties of the obtained materials were compared between the methods of sintering. On the basis of images from scanning electron microscope quantitative analysis was performed to determine the degree of grain growth of alumina after sintering.

  17. Microwave assisted sintering of gadolinium doped barium cerate electrolyte for intermediate temperature solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Arumugam Senthil, E-mail: senthu.ramp@gmail.com [Department of Physics, PSG College of Technology, Coimbatore, 641 004, Tamilnadu (India); Balaji, Ramamoorthy [Department of Physics, PSG College of Technology, Coimbatore, 641 004, Tamilnadu (India); Jayakumar, Srinivasalu [Department of Physics, PSG Institute of Technology and Applied Research, Coimbatore, 641 062, Tamilnadu (India); Pradeep, Chandran [Department of Physics, Indian Institute of Technology, Madras, 600 036, Tamilnadu (India)

    2016-10-01

    In Solid Oxide Fuel Cell (SOFC), electrolyte plays a vital role to increase the energy conversion efficiency. The main hurdle of such electrolyte in fuel cell is its higher operating temperature (1000 °C) which results in design limitation and higher fabrication cost. In order to reduce the operating temperature of SOFC, a suitable electrolyte has been prepared through co-precipitation method followed by microwave sintering of solid ceramic. The calcination temperature for the as-prepared powder was identified using Differential Scanning Calorimetry. The crystal structure of the sample was found to exhibit its orthorhombic perovskite structure. The particle size was determined using High-Resolution Transmission Electron Microscope with uniform in shape and size, match with XRD results and confirmed from structural analysis. Thus, the sample prepared via co-precipitation method and the solid ceramic sintered through microwave can be a promising electrolyte for fuel cells operated at intermediate temperature. - Highlights: • To synthesis the composite electrolyte by chemical method and sinter using microwave. • To reduce the operating temperature of electrolyte for high ionic conductivity in SOFC's. • To study the phase purity and to develop nanocomposite at reduced temperature.

  18. Liquid crystalline polymer nanocomposites reinforced with in-situ reduced graphene oxide

    Directory of Open Access Journals (Sweden)

    D. Pedrazzoli

    2015-08-01

    Full Text Available In this work liquid-crystalline polymer (LCP nanocomposites reinforced with in-situ reduced graphene oxide are investigated. Graphene oxide (GO was first synthesized by the Hummers method, and the kinetics of its thermal reduction was assessed. GO layers were then homogeneously dispersed in a thermotropic liquid crystalline polymer matrix (Vectran®, and an in-situ thermal reduction of GO into reduced graphene oxide (rGO was performed. Even at low rGO amount, the resulting nanocomposites exhibited an enhancement of both the mechanical properties and the thermal stability. Improvements of the creep stability and of the thermo-mechanical behavior were also observed upon nanofiller incorporation. Furthermore, in-situ thermal reduction of the insulating GO into the more electrically conductive rGO led to an important surface resistivity decrease in the nanofilled samples.

  19. A study on sintering aids for Sm{sub 0.2}Ce{sub 0.8}O{sub 1.9} electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xinge; Deces-Petit, Cyrille; Yick, Sing; Robertson, Mark; Kesler, Olivera; Maric, Radenka; Ghosh, Dave [Institute for Fuel Cell Innovation, National Research Council Canada, 3250 East Mall, Vancouver, BC (Canada V6T 1W5)

    2006-11-08

    In this study, an addition of Co oxide or Cu oxide to Sm{sub 0.2}Ce{sub 0.8}O{sub 1.9} (SDC) was studied to improve the sinterability of SDC. It has been found that both Co and Cu oxide are very effective as sintering aids, and the SDC sintering temperature can be reduced from 1400{sup o}C without aids to below 1000{sup o}C with only 1at.% of either Cu oxide or Co oxide. As compared to the pure SDC, a slight decrease of ionic conductivity was observed in SDC with Cu sintering aid. There is no obvious effect on electrochemical property of SDC with Co sintering aid under 2.5at.%. (author)

  20. Sintering of Synroc D

    International Nuclear Information System (INIS)

    Robinson, G.

    1982-01-01

    Sintering has been investigated as a method for the mineralization and densification of high-level nuclear defense waste powder. Studies have been conducted on Synroc D composite powder LS04. Optimal densification has been found to be highly dependent on the characteristics of the starting material. Powder subjected to milling, which was believed to reduce the level of agglomeration and possibly particle size, was found to densify better than powder not subjected to this milling. Densities of greater than 95% of theoretical could be achieved for samples sintered at 1150 to 1200 0 C. Mineralogy was found to be as expected for Synroc D for samples sintered in a CO 2 /CO atmosphere where the Fe +2 /Fe +3 ratio was maintained at 1.0 to 5.75. In a more oxidizing, pure CO 2 atmosphere a new phase, not previously identified in Synroc D, was found

  1. Modeling sintering of multilayers under influence of gravity

    DEFF Research Database (Denmark)

    Frandsen, Henrik Lund; Olevsky, Eugene; Tadesse Molla, Tesfaye

    2013-01-01

    , which describes the combined effect of sintering and gravity of thin multilayers, is derived and later compared with experimental results. It allows for consideration of both uniaxial and biaxial stress states. The model is based on the Skorohod-Olevsky viscous sintering framework, the classical...... laminate theory and the elastic-viscoelastic correspondence principle. The modeling approach is then applied to illustrate the effect of gravity during sintering of thin layers of cerium gadolinium oxide (CGO), and it is found to be significant. © 2012 The American Ceramic Society....

  2. Low temperature spark plasma sintering of YIG powders

    International Nuclear Information System (INIS)

    Fernandez-Garcia, L.; Suarez, M.; Menendez, J.L.

    2010-01-01

    A transition from a low to a high spin state in the magnetization saturation between 1000 and 1100 o C calcination temperature is observed in YIG powders prepared by oxides mixture. Spark plasma sintering of these powders between 900 and 950 o C leads to dense samples with minimal formation of YFeO 3 , opening the way to co-sintering of YIG with metals or metallic alloys. The optical properties depend on the sintering stage: low (high) density samples show poor (bulk) optical absorption.

  3. Studies on O/M ratio determination in uranium oxide, plutonium oxide and uranium-plutonium mixed oxide

    International Nuclear Information System (INIS)

    Sampath, S.; Chawla, K.L.

    1975-01-01

    Thermogravimetric studies were carried out in unsintered and sintered samples of uranium oxide, plutonium oxide and uranium-plutonium mixed oxide under different atmospheric conditions (air, argon and moist argon/hydrogen). Moisture loss was found to occur below 200 0 C for uranium dioxide samples, upto 700 0 C for sintered plutonium dioxide and negligible for sintered samples. The O/M ratios for non-stoichiometric uranium dioxide (sintered and unsintered), plutonium dioxide and mixed uranium and plutonium oxides (sintered) could be obtained with a precision of +- 0.002. Two reference states UOsub(2.000) and UOsub(2.656) were obtained for uranium dioxide and the reference state MOsub(2.000) was used for other cases. For unsintered plutonium dioxide samples, accurate O/M ratios could not be obtained of overlap of moisture loss with oxygen loss/gain. (author)

  4. CALCIUM OXIDE SINTERING IN ATMOSPHERES CONTAINING WATER AND CARBON DIOXIDE

    Science.gov (United States)

    The paper gives results of measurements of the effects of water vapor and CO2 on the sintering rate of nascent CaO, as a function of partial pressure and temperature using CaO prepared by rapid decomposition of CaCO3 and CA(OH)2. Each gas strongly catalyzed the sintering process ...

  5. Low sintering temperature glass waste forms for sequestering radioactive iodine

    Science.gov (United States)

    Nenoff, Tina M.; Krumhansl, James L.; Garino, Terry J.; Ockwig, Nathan W.

    2012-09-11

    Materials and methods of making low-sintering-temperature glass waste forms that sequester radioactive iodine in a strong and durable structure. First, the iodine is captured by an adsorbant, which forms an iodine-loaded material, e.g., AgI, AgI-zeolite, AgI-mordenite, Ag-silica aerogel, ZnI.sub.2, CuI, or Bi.sub.5O.sub.7I. Next, particles of the iodine-loaded material are mixed with powdered frits of low-sintering-temperature glasses (comprising various oxides of Si, B, Bi, Pb, and Zn), and then sintered at a relatively low temperature, ranging from 425.degree. C. to 550.degree. C. The sintering converts the mixed powders into a solid block of a glassy waste form, having low iodine leaching rates. The vitrified glassy waste form can contain as much as 60 wt % AgI. A preferred glass, having a sintering temperature of 500.degree. C. (below the silver iodide sublimation temperature of 500.degree. C.) was identified that contains oxides of boron, bismuth, and zinc, while containing essentially no lead or silicon.

  6. High temperature oxidation-sulfidation behavior of Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composites densified by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Saucedo-Acuna, R.A. [Instituto e Ingenieria y Tecnologia, Universidad Autonoma de Cd. Juarez, Av. Del Charro 450 Norte, Col. Partido Romero, C.P. 32310, Cd. Juarez, Chihuahua (Mexico); Monreal-Romero, H.; Martinez-Villafane, A. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); Chacon-Nava, J.G. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico)], E-mail: jose.chacon@cimav.edu.mx; Arce-Colunga, U. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); Universidad Autonoma de Tamaulipas, Matamoros 8 y 9 Col. Centro C.P. 87110, Cd. Victoria, Tamaulipas (Mexico); Gaona-Tiburcio, C. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); De la Torre, S.D. [Centro de Investigacion e Innovacion Tecnologica (CIITEC)-IPN, D.F. Mexico (Mexico)

    2007-12-15

    The high temperature oxidation-sulfidation behavior of Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composites prepared by mechanical alloying (MA) and spark plasma sintering (SPS) has been studied. These composite powders have a particular metal-ceramic interpenetrating network and excellent mechanical properties. Oxidation-sulfidation tests were carried out at 900 deg. C, in a 2.5%SO{sub 2} + 3.6%O{sub 2} + N{sub 2}(balance) atmosphere for 48 h. The results revealed the influence of the sintering conditions on the specimens corrosion resistance, i.e. the Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composite sintered at 1310 deg. C/4 min showed better corrosion resistance (lower weight gains) compared with those found for the 1440 deg. C/5 min conditions. For the former composite, a protective Cr{sub 2}O{sub 3} layer immediately forms upon heating, whereas for the later pest disintegration was noted. Thus, under the same sintering conditions the Nb-Al{sub 2}O{sub 3} composites showed the highest weight gains. The oxidation products were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy.

  7. In Situ Atom Probe Deintercalation of Lithium-Manganese-Oxide.

    Science.gov (United States)

    Pfeiffer, Björn; Maier, Johannes; Arlt, Jonas; Nowak, Carsten

    2017-04-01

    Atom probe tomography is routinely used for the characterization of materials microstructures, usually assuming that the microstructure is unaltered by the analysis. When analyzing ionic conductors, however, gradients in the chemical potential and the electric field penetrating dielectric atom probe specimens can cause significant ionic mobility. Although ionic mobility is undesirable when aiming for materials characterization, it offers a strategy to manipulate materials directly in situ in the atom probe. Here, we present experimental results on the analysis of the ionic conductor lithium-manganese-oxide with different atom probe techniques. We demonstrate that, at a temperature of 30 K, characterization of the materials microstructure is possible without measurable Li mobility. Also, we show that at 298 K the material can be deintercalated, in situ in the atom probe, without changing the manganese-oxide host structure. Combining in situ atom probe deintercalation and subsequent conventional characterization, we demonstrate a new methodological approach to study ionic conductors even in early stages of deintercalation.

  8. Mechanical, tribological and biological properties of novel 45S5 Bioglass® composites reinforced with in situ reduced graphene oxide.

    Science.gov (United States)

    Li, Zhong; Khun, Nay Win; Tang, Xiu-Zhi; Liu, Erjia; Khor, Khiam Aik

    2017-01-01

    45S5 Bioglass ® (45S5) is one of the most widely used biomaterials in ceramic-based bone graft substitutes by virtue of its excellent biocompatibility and bioactivity. However, the fracture toughness and wear resistance of 45S5 have to be improved to extend its applications in load bearing orthopedic implants. The current study reports the first use of graphene nanoplatelet (GNP) to enhance the fracture toughness and wear resistance of 45S5. Composite powders with four different loadings of graphene oxide (GO), i.e. 0, 0.1, 0.5 and 1wt%, were sintered by spark plasma sintering (SPS) at a relatively low temperature of 550°C, during which in situ thermal reduction of GO took place. It was found that by adding 0.5wt% GO to the 45S5 powder, the fracture toughness of the sintered pellets was increased by 130.2% while friction coefficient and specific wear rate were decreased by 21.3% and 62.0%, respectively. Furthermore, the viability of MG63 cells grown on the GNP-incorporated pellets was comparably high to that of the cells grown on the pure 45S5 pellets. As compared with the pure 45S5 leachates, the media conditioned by the GNP/45S5 pellets fabricated from the composite powder with 1wt% GO could enhance both the proliferation and viability of MG63 cells. It is thus envisioned that the GNP-reinforced 45S5 is a highly promising material for fabricating mechanically strong and biocompatible load-bearing bone implants. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Reaction and Transport Processes Controlling In Situ Chemical Oxidation of DNAPLs

    National Research Council Canada - National Science Library

    Siegrist, Robert L; Crimi, Michelle; Munakata-Marr, Junko; Illangasekare, Tissa; Dugan, Pamela; Heiderscheidt, Jeff; Jackson, Shannon; Petri, Ben; Sahl, Jason; Seitz, Sarah

    2006-01-01

    In situ chemical oxidation involves the introduction of chemical oxidants into the subsurface to destroy organic contaminants in soil and ground water, with the goal being to reduce the mass, mobility...

  10. Influence of spark plasma sintering conditions on the sintering and functional properties of an ultra-fine grained 316L stainless steel obtained from ball-milled powder

    Energy Technology Data Exchange (ETDEWEB)

    Keller, C., E-mail: clement.keller@insa-rouen.fr [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Tabalaiev, K.; Marnier, G. [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Noudem, J. [Laboratoire de Cristallographie des Matériaux, CNRS-UMR 6508, Université de Caen, ENSICAEN, 7 bd du Maréchal Juin, 14050 Caen (France); Sauvage, X. [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Hug, E. [Laboratoire de Cristallographie des Matériaux, CNRS-UMR 6508, Université de Caen, ENSICAEN, 7 bd du Maréchal Juin, 14050 Caen (France)

    2016-05-17

    In this work, 316L samples with submicrometric grain size were sintered by spark plasma sintering. To this aim, 316L powder was first ball-milled with different conditions to obtain nanostructured powder. The process control agent quantity and milling time were varied to check their influence on the crystallite size of milled powder. Samples were then sintered by spark plasma sintering using different sets of sintering parameters (temperature, dwell time and pressure). For each sample, grain size and density were systematically measured in order to investigate the influence of the sintering process on these two key microstructure parameters. Results show that suitable ball-milling and subsequent sintering can be employed to obtain austenitic stainless steel samples with grain sizes in the nanometer range with porosity lower than 3%. However, ball-milling and subsequent sintering enhance chromium carbides formation at the sample surface in addition to intragranular and intergranular oxides in the sample as revealed by X-ray diffraction and transmission electron microscopy. It has been shown that using Boron nitride together with graphite foils to protect the mold from powder welding prevent such carbide formation. For mechanical properties, results show that the grain size refinement strongly increases the hardness of the samples without deviation from Hall-Petch relationship despite the oxides formation. For corrosion resistance, grain sizes lower than a few micrometers involve a strong decrease in the pitting potential and a strong increase in passivation current. As a consequence, spark plasma sintering can be considered as a promising tool for ultra-fine grained austenitic stainless steel.

  11. Deformation behavior of sintered nanocrystalline silver layers

    International Nuclear Information System (INIS)

    Zabihzadeh, S.; Van Petegem, S.; Duarte, L.I.; Mokso, R.; Cervellino, A.; Van Swygenhoven, H.

    2015-01-01

    The microstructure of porous silver layers produced under different low temperature pressure-assisted sintering conditions is characterized and linked with the mechanical behavior studied in situ during X-ray diffraction. Peak profile analysis reveals important strain recovery and hardening mechanism during cyclic deformation. The competition between both mechanisms is discussed in terms of porosity and grain size

  12. Characteristics Of The Porous Body Sintered By Nano-Sized Fe-Cr-Al Alloy Powder

    Directory of Open Access Journals (Sweden)

    Lee Su-In

    2015-06-01

    Full Text Available Porous metal with uniform honeycomb structure was successfully produced by sintering using Fe-Cr-Al nano powder, which was prepared by the pulsed wire evaporation (PWE in ethanol. Its process consisted of the several steps; 1 coating on the surface of polyurethane sponge with the liquid droplets generated from the ethanol-based slurry where the Fe-Cr-Al nano powders were uniformly dispersed, 2 heat treatment of debinding to remove the polyurethane sponge and 3 sintering of the porous green body formed by Fe-Cr-Al nano powders. The strut thickness of porous Fe-Cr-Al was increased by the increase of spraying times in ESP step. Also, The shrinkages and the oxidation resistance of the sintered porous body was increased with increase of sintering temperature. The optimal sintering temperature was shown to 1450°C in views to maximize the oxidation resistance and sinterability.

  13. Effects of pressure and temperature on sintering of Cr-doped Al2O3 by pulsed electric current sintering process

    Science.gov (United States)

    Dang, K. Q.; Nanko, M.

    2011-03-01

    The aluminium oxide crystal, Al2O3, which contains a small amount of chromium, Cr, is called ruby. Pulsed electric current sintering (PECS) was applied to sinter ruby polycrystals. Cr2O3-Al2O3 powder mixture prepared by drying an aqueous slurry containing amounts of Al2O3 and Cr(NO3)3 was consolidated by PECS process. The PECS process was performed in vacuum at sintering temperature raging from 1100 to 1300°C with heating rate of 2 K/min under applied uniaxial pressure varied from 40 to 100 MPa. This study found that highly densified and transparent Cr-doped Al2O3 can be obtained by the PECS process with the high applied pressure at sintering temperature of 1200°C.

  14. Thermoelectric Properties of Hot-Pressed and PECS-Sintered Magnesium-Doped Copper Aluminum Oxide

    Science.gov (United States)

    Liu, Chang; Morelli, Donald T.

    2011-05-01

    Copper aluminum oxide (CuAlO2) is considered as a potential candidate for thermoelectric applications. Partially magnesium-doped CuAlO2 bulk pellets were fabricated using solid-state reactions, hot-pressing, and pulsed electric current sintering (PECS) techniques. X-ray diffraction and scanning electron microscopy were adopted for structural analysis. High-temperature transport property measurements were performed on hot-pressed samples. Electrical conductivity increased with Mg doping before secondary phases became significant, while the Seebeck coefficient displayed the opposite trend. Thermal conductivity was consistently reduced as the Mg concentration increased. Effects of Mg doping, preparation conditions, and future modification on this material's properties are discussed.

  15. Lanthanide (Nd, Gd) compounds with garnet and monazite structures. Powders synthesis by “wet” chemistry to sintering ceramics by Spark Plasma Sintering

    Energy Technology Data Exchange (ETDEWEB)

    Potanina, Ekaterina, E-mail: ekaterina.potanina@list.ru [Department of Solid State Chemistry, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 2, 603950 Nizhny Novgorod (Russian Federation); Golovkina, Ludmila, E-mail: golovkina_lyudmila@mail.ru [Department of Solid State Chemistry, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 2, 603950 Nizhny Novgorod (Russian Federation); Orlova, Albina, E-mail: albina.orlova@inbox.ru [Department of Solid State Chemistry, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 2, 603950 Nizhny Novgorod (Russian Federation); Nokhrin, Aleksey, E-mail: nokhrin@nifti.unn.ru [Research Institute of Physics and Technology, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 3, 603950 Nizhny Novgorod (Russian Federation); Boldin, Maksim, E-mail: boldin@nifti.unn.ru [Research Institute of Physics and Technology, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 3, 603950 Nizhny Novgorod (Russian Federation); Sakharov, Nikita, E-mail: nvsaharov@nifti.unn.ru [Research Institute of Physics and Technology, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 3, 603950 Nizhny Novgorod (Russian Federation)

    2016-05-15

    Complex oxide Y{sub 2.5}Nd{sub 0.5}Al{sub 5}O{sub 12} with garnet structure and phosphates NdPO{sub 4} and GdPO{sub 4} with monazite structure were obtained by using precipitation methods. Ceramics Y{sub 2.5}Nd{sub 0.5}Al{sub 5}O{sub 12} and NdPO{sub 4} were processed by Spark Plasma Sintering (SPS). Relative density more 98%, sintering time did not exceed 8 min, sintering temperature 1330–1390 °C. Leaching rates of elements from ceramics were 10{sup −6}–10{sup −7} g/(cm{sup 2} d). The process of ceramics sintering has two-stage character: the first step of sintering-compaction process is related to the plastic flow of the material, the second step–to the process of grain boundary diffusion and grain growth. - Highlights: • Powders were obtained by precipitation (sol–gel) method. • Ceramics were sintering by Spark Plasma Sintering method (ρ{sub rel} > 98%); shrinkage time does not exceed 8 min. • The process of ceramics sintering has two-stage character.

  16. In situ Raman Spectroscopy of Oxide Films on Zirconium Alloy in Simulated PWR Primary Water Condition

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Tae Ho; Choi, Kyoung Joon; Yoo, Seung Chang; Kim, Ji Hyun [UNIST, Ulsan (Korea, Republic of)

    2016-05-15

    The two layered oxide structure is formed in pre-transition oxide for the zirconium alloy in high temperature water environment. It is known that the corrosion rate is related to the volume fraction of zirconium oxide and the pores in the oxides; therefore, the aim of this paper is to investigate the oxidation behavior in the pretransition zirconium oxide in high-temperature water chemistry. In this work, Raman spectroscopy was used for in situ investigations for characterizing the phase of zirconium oxide. In situ Raman spectroscopy is a well-suited technique for investigating in detail the characteristics of oxide films in a high-temperature corrosion environment. In previous studies, an in situ Raman system was developed for investigating the oxides on nickel-based alloys and low alloy steels in high-temperature water environment. Also, the early stage oxidation behavior of zirconium alloy with different dissolved hydrogen concentration environments in high temperature water was treated in the authors' previous study. In this study, a specific zirconium alloy was oxidized and investigated with in situ Raman spectroscopy for 100 d oxidation, which is close to the first transition time of the zirconium alloy oxidation. The ex situ investigation methods such as transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS) were used to further characterize the zirconium oxide structure. As oxidation time increased, the Raman peaks of tetragonal zirconium oxide were merged or became weaker. However, the monoclinic zirconium oxide peaks became distinct. The tetragonal zirconium oxide was just found near the O/M interface and this could explain the Raman spectra difference between the 30 d result and others.

  17. The pressureless sintering and mechanical properties of AlON ceramic

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, N., E-mail: zhangning5832@163.com [Key Lab. of Advanced Materials and Manufacturing Technology of Liaoning Province, Shenyang University, Shenyang, Liaoning 110044 (China); Liang, B.; Wang, X.Y.; Kan, H.M.; Zhu, K.W. [Key Lab. of Advanced Materials and Manufacturing Technology of Liaoning Province, Shenyang University, Shenyang, Liaoning 110044 (China); Zhao, X.J. [Department of Materials Science and Engineering, School of Materials and Metallurgy, Northeastern University, Shenyang, Liaoning 110004 (China)

    2011-07-25

    Highlights: {yields} A one-step pressureless sintering process was proposed, which is simple and viable. {yields} Cheap and easily available {alpha}-Al{sub 2}O{sub 3} and aluminum powders were chosen as raw materials substituting for expensive AlN ultrafine powders. {yields} The sintering temperature of AlON ceramic was reduced by 50 deg. C and the flexural strength was enhanced by 29.4%. - Abstract: Aluminum oxynitride (AlON) ceramic was synthesized by one-step pressureless sintering technology using low cost and easily available {alpha}-Al{sub 2}O{sub 3} and aluminum powders as raw materials. The sintering temperature was reduced because aluminum powders were nitridized into high activity AlN under the flowing nitrogen atmosphere. The curves of thermal analysis, microstructure and atomic distribution were investigated. The influence of sintering temperatures on phase composition, sintering densification and flexural strength was also explored. The experimental results showed that {alpha}-Al{sub 2}O{sub 3} and aluminum powders were acceptable substitutes for more expensive AlN ultrafine powders. Under the optimum sintering process at 1750 deg. C for 2 h, the sintered density and flexural strength of AlON ceramic were higher, 3.62 g/cm{sup 3} and 321 MPa, respectively. The sintering temperature was decreased by 50 deg. C because newly formed high activity AlN in situ reacted with Al{sub 2}O{sub 3} into Al{sub 23}O{sub 27}N{sub 5}, enhancing flexural strength by 29.4%. However, the sintering temperature could not be too high because grain growth and displacement of oxygen atoms from AlON ceramics by nitrogen atoms caused a decline in sintering densification and flexural strength.

  18. Effect of rare earth oxide addition on microstructures of ultra-fine WC-Co particulate reinforced Cu matrix composites prepared by direct laser sintering

    International Nuclear Information System (INIS)

    Gu Dongdong; Shen Yifu; Zhao Long; Xiao Jun; Wu Peng; Zhu Yongbing

    2007-01-01

    This paper presents a detailed investigation into the influence of the rare earth (RE) oxide (La 2 O 3 ) addition upon the densification and the resultant microstructural characteristics of the submicron WC-Co particulate reinforced Cu matrix composites prepared by direct laser sintering. It is found that the relative density of the laser sintered sample with 1 wt.% La 2 O 3 addition increased by 11.5% as compared with the sample without RE addition. The addition of RE element favored the microstructural refinement and improved the particulate dispersion homogeneity and the particulate/matrix interfacial coherence. The metallurgical functions of the RE element in improving the sinterability were also addressed. It shows that due to the unique properties of RE element such as high surface activity and large atomic radius, the addition of trace RE element can decrease the surface tension of the melt, resist the grain growth coarsening and increase the heterogeneous nucleation rate during laser sintering

  19. Improved Modeling Approaches for Constrained Sintering of Bi-Layered Porous Structures

    DEFF Research Database (Denmark)

    Tadesse Molla, Tesfaye; Frandsen, Henrik Lund; Esposito, Vincenzo

    2012-01-01

    Shape instabilities during constrained sintering experiment of bi-layer porous and dense cerium gadolinium oxide (CGO) structures have been analyzed. An analytical and a numerical model based on the continuum theory of sintering has been implemented to describe the evolution of bow and densificat...

  20. Low-cost optical fabrication of flexible copper electrode via laser-induced reductive sintering and adhesive transfer

    Science.gov (United States)

    Back, Seunghyun; Kang, Bongchul

    2018-02-01

    Fabricating copper electrodes on heat-sensitive polymer films in air is highly challenging owing to the need of expensive copper nanoparticles, rapid oxidation of precursor during sintering, and limitation of sintering temperature to prevent the thermal damage of the polymer film. A laser-induced hybrid process of reductive sintering and adhesive transfer is demonstrated to cost-effectively fabricate copper electrode on a polyethylene film with a thermal resistance below 100 °C. A laser-induced reductive sintering process directly fabricates a high-conductive copper electrode onto a glass donor from copper oxide nanoparticle solution via photo-thermochemical reduction and agglomeration of copper oxide nanoparticles. The sintered copper patterns were transferred in parallel to a heat-sensitive polyethylene film through self-selective surface adhesion of the film, which was generated by the selective laser absorption of the copper pattern. The method reported here could become one of the most important manufacturing technologies for fabricating low-cost wearable and disposable electronics.

  1. Development of a Sinter/HIP process for the superalloy Udimet 700 with investigations of the influence of the sinteratmosphere

    International Nuclear Information System (INIS)

    Wenning, L.

    1991-03-01

    The oxidation free treatment of reactive metalpowders like the nickel base alloy Udimet 700 demands sufficient oxygen free sinteratmospheres in nowadays sinter-HIP plants are not reachable. The reported work deals with the development of a sinter-HIP process which enables a sufficient low partial pressure of oxygen by scavenging the Udimet 700 powder packings with argon during vacuum sintering. By this the sinter hindering oxidation is avoided. Intensive investigations of the sinteratmosphere with a mass spectrometer and a zirconium oxide probe verify the reduction of the oxygen content of the residual gas atmosphere reached with different processes. In a second part the applicability of the scavenging gas process during the capsule free sinter-HIP treatment of metall injection moulded (MIM) samples is shown. (orig.) [de

  2. Phenomenological model of sintering of oxide nuclear fuel with doping admixtures

    Science.gov (United States)

    Baranov, V. G.; Devyatko, Yu. N.; Tenishev, A. V.; Khomyakov, O. V.

    2015-12-01

    It is shown that a change in the linear dimension of compacted UO2 in the sintering process is associated with its plastic yielding under the action of the forces of residual stress and capillary forces. From the curves of sintering of a fuel with doping admixtures in various gaseous media, its rate of creep is reduced.

  3. Sintering and densification; new techniques: sinter forging

    International Nuclear Information System (INIS)

    Winnubst, A.J.A.

    1998-01-01

    In this chapter pressure assisted sintering methods will be described. Attention will mainly be paid to sinter forging as a die-wall free uniaxial pressure sintering technique, where large creep strains are possible. Sinter forging is an effective tool to reduce sintering temperature and time and to obtain a nearly theoretically dense ceramic. In this way grain size in tetragonal zirconia ceramics can be reduced down to 100 nm. Another important phenomenon is the reduction of the number density and size of cracks and flaws resulting in higher strength and improved reliability, which is of utmost importance for engineering ceramics. The creep deformation during sinter forging causes a rearrangement of the grains resulting in a reduction of interatomic spaces between grains, while grain boundary (glassy) phases can be removed. The toughness and in some cases the wear resistance is enhanced after sinter forging as a result of the grain-boundary-morphology improvement. (orig.)

  4. Disruption of an Alumina Layer During Sintering of Aluminium in Nitrogen

    Directory of Open Access Journals (Sweden)

    Pieczonka T.

    2017-06-01

    Full Text Available Aluminium oxide layer on aluminium particles cannot be avoided. However, to make the metal-metal contacts possible, this sintering barrier has to be overcome in some way, necessarily to form sintering necks and their development. It is postulated that the disruption of alumina layer under sintering conditions may originate physically and chemically. Additionally, to sinter successfully non alloyed aluminium powder in nitrogen, the operation of both types mechanism is required. It is to be noted that metallic aluminium surface has to be available to initiate reactions between aluminium and the sintering atmosphere, i.e. mechanical disruption of alumina film precedes the chemical reactions, and only then chemically induced mechanisms may develop. Dilatometry, gravimetric and differential thermal analyses, and microstructure investigations were used to study the sintering response of aluminium at 620°C in nitrogen, which is the only sintering atmosphere producing shrinkage.

  5. Solidification of high level liquid waste (HLLW) into ceramics by sintering process

    International Nuclear Information System (INIS)

    Masuda, Sumio; Oguino, Naohiko; Tsunoda, Naomi; O-oka, Kazuo; Ohta, Takao.

    1979-01-01

    One of the alternatives to vitrified solid which is acceptable and well characterized for storing radioactive HLLW with desirable long-term stability is ceramics. On the other hand, the solidification process of highly radioactive wastes should be simple and suitable for continuous production. On the above described basis, the authors have made preliminary study on the production of sintered ceramics by the addition of several oxides to HLLW. The simulated waste and additive oxides were pressed in a mold to make the preforms of 50 mm diameter and 10 to 15 mm thick. The preforms were then normally sintered at temperature from 1000 to 1400 deg C for 2 to 4 hours. The characterization of the sintered solids revealed the following facts. (1) X-ray diffraction analysis showed that the expected crystals were formed by normal-sintering as well as by hot-pressing. (2) The bulk density of the ceramics by normal-sintering was around 90 to 95% of the assumed theoretical values. (3) The leach-rate of the solids was affected by the bulk density. (4) Other properties of the solids, such as thermal expansion or thermal conductivity, are dominantly determined by those of main crystals in the solids. Sintering process is generally simple and productive as far as normal sintering is concerned. However, hot-pressing is an intermittent and time consuming process. From this fact, the authors intended to adopt the normal sintering process for the ceramic solidification of high level liquid wastes. (Wakatsuki, Y.)

  6. Effect of grain size on the hardness and reactivity of plasma-sintered beryllium

    International Nuclear Information System (INIS)

    Kim, Jae-Hwan; Nakamichi, Masaru

    2014-01-01

    Beryllium and its intermetallic compounds have attracted great attention as promising neutron multipliers in fusion reactors. In this study, mechanical and chemical properties of fabricated plasma-sintered beryllium (PS-Be) with different grain-sizes are investigated. Density and hardness analysis results of the fabricated PS-Be samples infer that a smaller grain size in the sintered Be indicates higher porosity and hardness. Sintered Be with a large grain size exhibits better resistance toward oxidation at 1273 K in dry air and at 1073 K in Ar/1% H 2 O, since oxidation at the grain boundaries of the determines the rate. In contrast, at 1273 K in Ar/1% H 2 O, a catastrophic oxidation is indicated by the increase of weight of the samples and the generation of H 2 from the bulk Be

  7. Spark plasma sintering of pure and doped tungsten as plasma facing material

    Science.gov (United States)

    Autissier, E.; Richou, M.; Minier, L.; Naimi, F.; Pintsuk, G.; Bernard, F.

    2014-04-01

    In the current water cooled divertor concept, tungsten is an armour material and CuCrZr is a structural material. In this work, a fabrication route via a powder metallurgy process such as spark plasma sintering is proposed to fully control the microstructure of W and W composites. The effect of chemical composition (additives) and the powder grain size was investigated. To reduce the sintering temperature, W powders doped with a nano-oxide dispersion of Y2O3 are used. Consequently, the sintering temperature for W-oxide dispersed strengthened (1800 °C) is lower than for pure W powder. Edge localized mode tests were performed on pure W and compared to other preparation techniques and showed promising results.

  8. Effect of boron oxide on the cubic-to-monoclinic phase transition in yttria-stabilized zirconia

    International Nuclear Information System (INIS)

    Florio, D.Z. de; Muccillo, R.

    2004-01-01

    Specimens of yttria fully stabilized zirconia with different amounts of boron oxide have been studied by X-ray diffraction at room temperature and at higher temperatures up to 1250 deg. C. A boron oxide-assisted cubic-to-monoclinic phase transformation was determined in the temperature range 800-1250 deg. C. In situ high temperature X-ray diffraction experiments gave evidences of the dependence of the phase transformation on the heating rate. The possibility of tuning the cubic-monoclinic phase ratio by suitable addition of boron oxide before pressing and sintering is proposed

  9. Sintering and Electrical Characterization of La and Nb Co‐doped SrTiO3 Electrode Materials for Solid Oxide Cell Applications

    DEFF Research Database (Denmark)

    Sudireddy, Bhaskar Reddy; Agersted, Karsten

    2014-01-01

    Single‐phase lanthanum and niobium co‐doped strontium titanate (Sr1–3x/2LaxTi0.9Nb0.1O3; x = 0–0.02) ceramics were prepared. Dilatometry in reducing atmosphere showed an increase in the sintering rate and sintered density with an increase in La amount. Microscopy of fractured surfaces of sintered...... samples showed that the average grain size increased drastically in reducing conditions with increasing La content (and associated A‐site vacancies). By incorporating 2 mol.% La, the electronic conductivity significantly improved from 80 to 135 S cm−1 at 1,000 °C, and even larger improvements were...... observed at lower temperatures. These observations demonstrate the flexibility in tailoring the microstructure and electronic transport properties by doping small amounts of La into the Nb‐doped SrTiO3 and show that Sr1–3x/2LaxTi0.9Nb0.1O3 is a potential electrode material for solid oxide cells....

  10. Surface phenomena during the early stages of sintering in steels modified with Fe–Mn–Si–C master alloys

    Energy Technology Data Exchange (ETDEWEB)

    Oro, Raquel, E-mail: raqueld@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden); Campos, Mónica, E-mail: campos@ing.uc3m.es [Department of Materials Science and Engineering, IAAB, Universidad Carlos III de Madrid, Av. Universidad 30, 28911 Leganés, Madrid (Spain); Hryha, Eduard, E-mail: hryha@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden); Torralba, José Manuel, E-mail: torralba@ing.uc3m.es [Department of Materials Science and Engineering, IAAB, Universidad Carlos III de Madrid, Av. Universidad 30, 28911 Leganés, Madrid (Spain); IMDEA Materials Institute, C/Eric Kandel, 2, 28906 Getafe, Madrid (Spain); Nyborg, Lars, E-mail: lars.nyborg@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden)

    2013-12-15

    The characteristics of the metallic powder surface play a critical role in the development of strong bonds between particles during sintering, especially when introducing elements with a high affinity for oxygen. In this study, Mn and Si have been combined in a Fe–Mn–Si–C master alloy powder in order to reduce their chemical activity and prevent oxidation during the heating stage of the sintering process. However, when this master alloy powder is mixed with an iron base powder, differences in chemical activity between both components can lead to an oxygen transfer from the iron base powder to the surface of the master alloy particles. The present research is focused on studying the evolution of the master alloy particle surface during the early stages of sintering. Surface characterization by X-ray Photoelectron Spectroscopy (XPS) shows that the master alloy powder surface is mostly covered by a thin easily reducible iron oxide layer (∼ 1 nm). Mn–Si particulate oxides are found as inclusions in specific areas of the surface. Evolution of oxides during sintering was studied on green compacts containing iron powder, graphite and Fe–Mn–Si–C master alloy powder that were heat treated in vacuum (10{sup −6} mbar) at different temperatures (from 400, 600, 800 to 1000 °C) and analyzed by means of XPS. Vacuum sintering provides the necessary conditions to remove manganese and silicon oxides from the powder surface in the range of temperatures between 600 °C and 1000 °C. When sintering in vacuum, since the gaseous products from reduction processes are continuously eliminated, oxidation of master alloy particles due to oxygen transfer through the atmosphere is minimized. - Highlights: • Mn and Si were introduced in sintered steels using a master alloy powder. • Surface of the master alloy is mainly covered by an easily reducible iron oxide. • Temperature ranges for oxidation/reduction are identified. • Vacuum conditions avoid oxygen transfer to

  11. Sintering Theory and Practice

    Science.gov (United States)

    German, Randall M.

    1996-01-01

    process all around us--in manufactured objects from metals, ceramics, polymers, and many compounds. From a vast professional literature, Sintering Theory and Practice emerges as the only comprehensive, systematic, and self-contained volume on the subject. Covering all aspects of sintering as a processing topic, including materials, processes, theories, and the overall state of the art, the book Offers numerous examples, illustrations, and tables that detail actual processing cycles, and that stress existing knowledge in the field Uses the specifics of various consolidation cycles to illustrate the basics Leads the reader from the fundamentals to advanced topics, without getting bogged down in various mathematical disputes over treatments and measurements Supports the discussion with critically selected references from thousands of sources Examines the sintering behavior of a wide variety of engineered materials--metals, alloys, oxide ceramics, composites, carbides, intermetallics, glasses, and polymers Guides the reader through the sintering processes for several important industrial materials and demonstrates how to control these processes effectively and improve present techniques Provides a helpful reference for specific information on materials, processing problems, and concepts For practitioners and researchers in ceramics, powder metallurgy, and other areas, and for students and faculty in materials science and engineering, this book provides the know-how and understanding crucial to many industrial operations, offers many ideas for further research, and suggests future applications of this important technology. This book offers an unprecedented opportunity to explore sintering in both practical and theoretical terms, whether at the lab or in real-world applications, and to acquire a broad, yet thorough, understanding of this important technology.

  12. Gas-phase advanced oxidation for effective, efficient in situ control of pollution

    DEFF Research Database (Denmark)

    Johnson, Matthew Stanley; Nilsson, Elna Johanna Kristina; Svensson, Erik Anders

    2014-01-01

    In this article, gas-phase advanced oxidation, a new method for pollution control building on the photo-oxidation and particle formation chemistry occurring in the atmosphere, is introduced and characterized. The process uses ozone and UV-C light to produce in situ radicals to oxidize pollution......, generating particles that are removed by a filter; ozone is removed using a MnO2 honeycomb catalyst. This combination of in situ processes removes a wide range of pollutants with a comparatively low specific energy input. Two proof-of-concept devices were built to test and optimize the process...... particulate mass. Secondary pollution including formaldehyde and ultrafine particles might be generated, depending on the composition of the primary pollution....

  13. Short Communication on “In-situ TEM ion irradiation investigations on U{sub 3}Si{sub 2} at LWR temperatures”

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Yinbin, E-mail: ymiao@anl.gov [Argonne National Laboratory, Lemont, IL 60439 (United States); Harp, Jason [Idaho National Laboratory, Idaho Fall, ID 83415 (United States); Mo, Kun [Argonne National Laboratory, Lemont, IL 60439 (United States); Bhattacharya, Sumit [Northwestern University, Evanston, IL 60208 (United States); Baldo, Peter; Yacout, Abdellatif M. [Argonne National Laboratory, Lemont, IL 60439 (United States)

    2017-02-15

    The radiation-induced amorphization of U{sub 3}Si{sub 2} was investigated by in-situ transmission electron microscopy using 1 MeV Kr ion irradiation. Both arc-melted and sintered U{sub 3}Si{sub 2} specimens were irradiated at room temperature to confirm the similarity in their responses to radiation. The sintered specimens were then irradiated at 350 °C and 550 °C up to 7.2 × 10{sup 15} ions/cm{sup 2} to examine their amorphization behavior under light water reactor (LWR) conditions. U{sub 3}Si{sub 2} remains crystalline under irradiation at LWR temperatures. Oxidation of the material was observed at high irradiation doses.

  14. Liquid phase sintered SiC. Processing and transformation controlled microstructure tailoring

    Directory of Open Access Journals (Sweden)

    V.A. Izhevskyi

    2000-10-01

    Full Text Available Microstructure development and phase formation processes during sintering of silicon carbide based materials with AlN-Y2O3, AlN-Yb2O3, and AlN-La2O3 sintering additives were investigated. Densification of the materials occurred by liquid-phase sintering mechanism. Proportion of alpha- and beta-SiC powders in the initial mixtures was a variable parameter, while the molar ratio of AlN/RE2O3, and the total amount of additives (10 vol. % were kept constant. Shrinkage behavior during sintering in interrelation with the starting composition of the material and the sintering atmosphere was investigated by high temperature dilatometry. Kinetics of b-SiC to a-SiC phase transformation during post-sintering heat treatment at temperatures 1900-1950 °C was studied, the degree of phase transformation being determined by quantitative x-ray analysis using internal standard technique. Evolution of microstructure resulting from beta-SiC to alpha-SiC transformation was followed up by scanning electron microscopy on polished and chemically etched samples. Transformation-controlled grain growth mechanism similar to the one observed for silicon nitride based ceramics was established. Possibility of in-situ platelet reinforced dense SiC-based ceramics fabrication with improved mechanical properties by means of sintering was shown.

  15. In-situ oxidation study of Pd(100) by surface x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Kilic, Volkan; Franz, Dirk; Stierle, Andreas [AG Grenzflaechen, Universitaet Siegen (Germany); Martin, Natalia; Lundgren, Edvin [Department of Synchrotron Radiation Research, Lund University (Sweden); Mantilla, Miguel [MPI fuer Metallforschung, Stuttgart (Germany)

    2011-07-01

    The oxidation of the Pd(100) surface at oxygen pressures in the 10{sup -6} mbar to 10{sup 3} mbar range and temperatures up to 1000 K has been studied in-situ by surface x-ray diffraction (SXRD). The SXRD experiments were performed at the MPI beamline at the Angstrom Quelle Karlsruhe (ANKA). We present the surface and crystal truncation rod (CTR) data from the ({radical}(5) x {radical}(5)) surface layer. We show that the transformation from the surface oxide to PdO bulk oxide can be observed in-situ under specific pressure and temperature conditions. We compare our results with previously proposed structure models based on low energy electron diffraction (LEED) I(V) curves and density functional theory calculations. Finally, we elucidate the question of commensurability of the surface oxide layer with respect to the Pd(100) substrate.

  16. Mechanisms and mechanics of shape loss during supersolidus liquid-phase sintering

    Science.gov (United States)

    Lal, Anand

    Rapid sinter densification of relatively coarse prealloyed powders is possible by exceeding the solidus temperature in an approach termed supersolidus liquid phase sintering (SLPS). However, narrow processing windows for densification without distortion often limit this process. The liquid films at the grain boundaries that are responsible for densification also reduce the structural rigidity of components. Hence, components tend to slump under their own weight. Thus, the present study investigates shape loss during SLPS and rationalizes the processing and material factors with regard to separating densification from distortion. Experiments are performed on various prealloyed powders, including bronze, 316L stainless steel, and T15 tool steel. Differential thermal analysis, dilatometry, and in situ video imaging of sintering compacts are used to follow melting, densification, and distortion, respectively. Further, density and dimensional measurements are performed on sintered compacts. Results indicate a dependence of distortion on the sintering temperature and time, compact size, and melting behavior of the alloy. It is shown that the sintering temperature window, where high-density, precise components are obtained, can be widened for 316L stainless steel by boron addition. For the first time, a beam bending technique is used to measure the macroscopic apparent viscosity of semisolid bronze. The viscosity drops with temperature above the solidus and lies in the range of 108 to 106 Pa-s. Additionally, the in situ transverse rupture strength of bronze is measured to demonstrate the softening above the solidus temperature. Further, microstructural measurements are performed to enable correlation with the slumping behavior and viscosity. A model combining the deformation mechanisms, driving forces, and microstructural characteristics is developed to predict the conditions for densification and distortion onset. The microstructure is also correlated with the magnitude

  17. Oxidation of triclosan by permanganate (Mn(VII)): importance of ligands and in situ formed manganese oxides.

    Science.gov (United States)

    Jiang, Jin; Pang, Su-Yan; Ma, Jun

    2009-11-01

    Experiments were conducted to examine permanganate (Mn(VII); KMnO(4)) oxidation of the widely used biocide triclosan (one phenolic derivative) in aqueous solution at pH values of 5-9. Under slightly acidic conditions, the reactions displayed autocatalysis, suggesting the catalytic role of in situ formed MnO(2). This was further supported by the promoting effects of the addition of preformed MnO(2) colloids on Mn(VII) oxidations of triclosan and two other selected phenolics (i.e., phenol and 2,4-dichlorophenol), as well as p-nitrophenol which otherwise showed negligible reactivity toward Mn(VII) and MnO(2) colloids, respectively. Surprisingly, phosphate buffer significantly enhanced Mn(VII) oxidation of triclosan, as well as phenol and 2,4-dichlorophenol over a wide pH range. Further, several other selected ligands (i.e., pyrophosphate, EDTA, and humic acid) also exerted oxidation enhancement, supporting a scenario where highly active aqueous manganese intermediates (Mn(INT)(aq)) formed in situ upon Mn(VII) reduction might be stabilized to a certain extent in the presence of ligands and subsequently involved in further oxidation of target phenolics, whereas without stabilizing agents Mn(INT)(aq) autodecomposes or disproportionates spontaneously. The effectiveness of Mn(VII) for the oxidative removal of triclosan in natural water and wastewater was confirmed. Their background matrices were also found to accelerate Mn(VII) oxidation of phenolics.

  18. Sintering Characteristics of Multilayered Thermal Barrier Coatings Under Thermal Gradient and Isothermal High Temperature Annealing Conditions

    Science.gov (United States)

    Rai, Amarendra K.; Schmitt, Michael P.; Bhattacharya, Rabi; Zhu, Dongming; Wolfe, Douglas E.

    2014-01-01

    Pyrochlore oxides have most of the relevant attributes for use as next generation thermal barrier coatings such as phase stability, low sintering kinetics and low thermal conductivity. One of the issues with the pyrochlore oxides is their lower toughness and therefore higher erosion rate compared to the current state-of-the-art TBC material, yttria (6 to 8 wt%) stabilized zirconia (YSZ). In this work, sintering characteristics were investigated for novel multilayered coating consisted of alternating layers of pyrochlore oxide viz Gd2Zr2O7 and t' low k (rare earth oxide doped YSZ). Thermal gradient and isothermal high temperature (1316 C) annealing conditions were used to investigate sintering and cracking in these coatings. The results are then compared with that of relevant monolayered coatings and a baseline YSZ coating.

  19. In situ Reduction and Oxidation of Nickel from Solid Oxide Fuel Cells in a Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Faes, Antonin; Jeangros, Quentin; Wagner, Jakob Birkedal

    2009-01-01

    Environmental transmission electron microscopy was used to characterize in situ the reduction and oxidation of nickel from a Ni/YSZ solid oxide fuel cell anode support between 300-500{degree sign}C. The reduction is done under low hydrogen pressure. The reduction initiates at the NiO/YSZ interface...

  20. Characterization and Electrical Response to Humidity of Sintered Polymeric Electrospun Fibers of Vanadium Oxide-({TiO}_{{2}} /{WO}_{{3}} )

    Science.gov (United States)

    Araújo, E. S.; Libardi, J.; Faia, P. M.; de Oliveira, H. P.

    2018-02-01

    Metal oxide composites have attracted much consideration due to their promising applications in humidity sensors in response to the physical and chemical property modifications of the resulting materials. This work focused on the preparation, microstructural characterization and analysis of humidity-dependent electrical properties of undoped and vanadium oxide (V2O5)-doped titanium oxide/tungsten oxide (TiO2/WO3) sintered ceramic films obtained by electrospinning. The electrical properties were investigated by impedance spectroscopy (400 Hz-40 MHz) as a function of relative humidity (RH). The results revealed a typical transition in the transport mechanisms controlled by the appropriated doping level of V2O5, which introduces important advantages to RH detection due to the atomic substitution of titanium by vanadium atoms in highly doped structures. These aspects are directly related to the microstructure modification and structure fabrication procedure.

  1. Sintering of nanoscale silver coated textiles, a new approach to attain conductive fabrics for electromagnetic shielding

    International Nuclear Information System (INIS)

    Kardarian, Kasra; Busani, Tito; Osório, Inês; Domingos, Helena; Igreja, Rui; Franco, Ricardo; Cortez, João

    2014-01-01

    The demand for conductive textiles is increasing, owing to the need for lightweight and flexible conductive materials for a variety of applications, including electromagnetic shielding of electronic equipment. Herein we propose a process that combines the in situ synthesis of silver nanoparticles at the textile fibre surface followed by sintering of the nanoparticles to obtain highly conductive fabrics. The formation of silver particles at the nanoscale allowed for sintering to be performed efficiently, at reduced temperature and time, bestowing fabrics with high conductivity and capability of shielding electromagnetic radiation. The nanoparticle synthesis method entailed the precipitation of 2.0 g L −1 silver nitrate and further reduction with citrate, with the formation of a deposit of silver nanoparticles at the fabric surface. The amount of silver deposited (up to 195 mg of silver per g of fabric) resulted in moderate electrical conductivity with sheet resistance of 803 Ω/sq. Upon sintering, this value decreased dramatically to 5.2 Ω/sq. The sintering process was monitored by SEM, which showed that sintering at 200 °C for 30 min resulted in maximal electrical conductivity with the lowest amount of silver deposited, while forming a homogenous surface. Fabrics submitted to these sintering conditions maintained their sheet resistance and shielding effectiveness values, even after eight washing cycles. - Highlights: • Assembly of highly conductive textiles capable of shielding electromagnetic radiation. • Procedure combines in situ synthesis of AgNPs at the textile surface and sintering. • AgNPs formed by precipitation of AgNO 3 and reduction with citrate, as observed by SEM. • Sintering increased dramatically conductivity and shielding effectiveness. • Treated fabrics maintained conductivity and shielding effectiveness after 8 washes

  2. Sintering of nanoscale silver coated textiles, a new approach to attain conductive fabrics for electromagnetic shielding

    Energy Technology Data Exchange (ETDEWEB)

    Kardarian, Kasra [REQUIMTE, Departamento de Química, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Busani, Tito [CENIMAT/I3N, Departamento de Ciência dos Materiais, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Osório, Inês [REQUIMTE, Departamento de Química, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Domingos, Helena; Igreja, Rui [CENIMAT/I3N, Departamento de Ciência dos Materiais, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Franco, Ricardo [REQUIMTE, Departamento de Química, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Cortez, João, E-mail: j.cortez@fct.unl.pt [REQUIMTE, Departamento de Química, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal)

    2014-10-15

    The demand for conductive textiles is increasing, owing to the need for lightweight and flexible conductive materials for a variety of applications, including electromagnetic shielding of electronic equipment. Herein we propose a process that combines the in situ synthesis of silver nanoparticles at the textile fibre surface followed by sintering of the nanoparticles to obtain highly conductive fabrics. The formation of silver particles at the nanoscale allowed for sintering to be performed efficiently, at reduced temperature and time, bestowing fabrics with high conductivity and capability of shielding electromagnetic radiation. The nanoparticle synthesis method entailed the precipitation of 2.0 g L{sup −1} silver nitrate and further reduction with citrate, with the formation of a deposit of silver nanoparticles at the fabric surface. The amount of silver deposited (up to 195 mg of silver per g of fabric) resulted in moderate electrical conductivity with sheet resistance of 803 Ω/sq. Upon sintering, this value decreased dramatically to 5.2 Ω/sq. The sintering process was monitored by SEM, which showed that sintering at 200 °C for 30 min resulted in maximal electrical conductivity with the lowest amount of silver deposited, while forming a homogenous surface. Fabrics submitted to these sintering conditions maintained their sheet resistance and shielding effectiveness values, even after eight washing cycles. - Highlights: • Assembly of highly conductive textiles capable of shielding electromagnetic radiation. • Procedure combines in situ synthesis of AgNPs at the textile surface and sintering. • AgNPs formed by precipitation of AgNO{sub 3} and reduction with citrate, as observed by SEM. • Sintering increased dramatically conductivity and shielding effectiveness. • Treated fabrics maintained conductivity and shielding effectiveness after 8 washes.

  3. Two-step flash light sintering of copper nanoparticle ink to remove substrate warping

    Energy Technology Data Exchange (ETDEWEB)

    Ryu, Chung-Hyeon; Joo, Sung-Jun [Department of Mechanical Convergence Engineering, Hanyang University, Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Kim, Hak-Sung, E-mail: kima@hanyang.ac.kr [Department of Mechanical Convergence Engineering, Hanyang University, Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Institute of Nano Science and Technology, Hanyang University, Seoul, 133-791 (Korea, Republic of)

    2016-10-30

    Highlights: • We performed the two-step flash light sintering for copper nanoparticle ink to remove substrate warping. • 12 J/cm{sup 2} of preheating and 7 J/cm{sup 2} of main sintering energies were determined as optimum conditions to sinter the copper nanoparticle ink. • The resistivity of two-step sintered copper nanoparticle ink was 3.81 μΩ cm with 5B adhesion level, 2.3 times greater than that of bulk copper. • The two-step sintered case showed a high conductivity without any substrate warping. - Abstract: A two-step flash light sintering process was devised to reduce the warping of polymer substrates during the sintering of copper nanoparticle ink. To determine the optimum sintering conditions of the copper nanoparticle ink, the flash light irradiation conditions (pulse power, pulse number, on-time, and off-time) were varied and optimized. In order to monitor the flash light sintering process, in situ resistance and temperature monitoring of copper nanoink were conducted during the flash light sintering process. Also, a transient heat transfer analysis was performed by using the finite-element program ABAQUS to predict the temperature changes of copper nanoink and polymer substrate. The microstructures of the sintered copper nanoink films were analyzed by scanning electron microscopy. Additionally, an X-ray diffraction and Fourier transform infrared spectroscopy were used to characterize the crystal phase change of the sintered copper nanoparticles. The resulting two-step flash light sintered copper nanoink films exhibited a low resistivity (3.81 μΩ cm, 2.3 times of that of bulk copper) and 5B level of adhesion strength without warping of the polymer substrate.

  4. Oxide-supported metal clusters: models for heterogeneous catalysts

    International Nuclear Information System (INIS)

    Santra, A K; Goodman, D W

    2003-01-01

    Understanding the size-dependent electronic, structural and chemical properties of metal clusters on oxide supports is an important aspect of heterogeneous catalysis. Recently model oxide-supported metal catalysts have been prepared by vapour deposition of catalytically relevant metals onto ultra-thin oxide films grown on a refractory metal substrate. Reactivity and spectroscopic/microscopic studies have shown that these ultra-thin oxide films are excellent models for the corresponding bulk oxides, yet are sufficiently electrically conductive for use with various modern surface probes including scanning tunnelling microscopy (STM). Measurements on metal clusters have revealed a metal to nonmetal transition as well as changes in the crystal and electronic structures (including lattice parameters, band width, band splitting and core-level binding energy shifts) as a function of cluster size. Size-dependent catalytic reactivity studies have been carried out for several important reactions, and time-dependent catalytic deactivation has been shown to arise from sintering of metal particles under elevated gas pressures and/or reactor temperatures. In situ STM methodologies have been developed to follow the growth and sintering kinetics on a cluster-by-cluster basis. Although several critical issues have been addressed by several groups worldwide, much more remains to be done. This article highlights some of these accomplishments and summarizes the challenges that lie ahead. (topical review)

  5. Heterojunction p-Cu2O/ZnO-n solar cell fabricated by spark plasma sintering

    Directory of Open Access Journals (Sweden)

    Christophe Tenailleau

    2017-09-01

    Full Text Available Abstract Cuprous oxide and zinc oxide nanoparticles were prepared at room temperature by inorganic polycondensation. X-ray diffraction (XRD analyses show that the oxide phases formed are pure and well crystallized. The spark plasma sintering (SPS technique was successfully used to prepare dense nanoceramics with superimposed layers of Cu2O and ZnO nanopowders. Sintering conditions were optimized to densify the ceramics without phase transformation or diffusion. These ceramics were also characterized by XRD and scanning electron microscopy (SEM, as well as X-ray computed tomography (XCT. SEM and XCT showed that nanograins are preserved after SPS throughout both oxide materials, while a smaller layer (~20 µm of pure oxide phase with larger grains is formed in between Cu2O and ZnO during the sintering process. The SPS technique results in high material density, with the absence of porosity and cracks, homogenous distribution, and a good phase separation. This is the first time that such as-prepared dense oxide-based heterojunction exhibits a photovoltaic effect under illumination opening a new route for preparing solar cells.

  6. Microbial dynamics during and after in situ chemical oxidation of chlorinated solvents

    NARCIS (Netherlands)

    Sutton, N.B.; Atashgahi, S.; Wal, van der J.; Wijn, G.; Grotenhuis, J.T.C.; Smidt, H.; Rijnaarts, H.

    2015-01-01

    In situ chemical oxidation (ISCO) followed by a bioremediation step is increasingly being considered as an effective biphasic technology. Information on the impact of chemical oxidants on organohalide respiring bacteria (OHRB), however, is largely lacking. Therefore, we used quantitative PCR (qPCR)

  7. Nd-Fe-B sintered magnets fabrication by using atomized powders

    International Nuclear Information System (INIS)

    Goto, R; Sugimoto, S; Matsuura, M; Tezuka, N; Une, Y; Sagawa, M

    2011-01-01

    Nd-Fe-B sintered magnets are required to achieve high coercivity for improvement of their thermal stability. Dy is added to increase coercivity, however, this element decrease magnetization and energy products. Therefore, Dy-lean Nd-Fe-B sintered magnets with high coercivity are strongly demanded. To increase coercivity, it is necessary that microstructure of sintered magnets is consisted of both fine main phase particles and homogeneously distributed Nd-rich phases around the main phase. To meet those requirements, Nd-Fe-B atomized powders were applied to the fabrication process of sintered magnets. Comparing with the case of using strip casting (SC) alloys, jet-milled powders from atomized powders show homogeneous distribution of Nd-rich phase. After optimized thermal treatment, coercivities of sintered magnets from atomized powders and SC alloys reach 1050 kA·m-1 and 1220 kA·m-1, respectively. This difference in coercivity was due to initial oxygen concentration of starting materials. Consequently, Nd-rich phases became oxides with high melting points, and did not melt and spread during sintering and annealing.

  8. Morphological analysis and modelling of sintering and of sintered materials

    International Nuclear Information System (INIS)

    Jernot, Jean-Paul

    1982-01-01

    This research thesis addresses the study of solid phase sintering of metallic powders, and aims at describing as precisely as possible the different involved matter transport mechanisms, first by using a thermodynamic approach to sintering. Sintering diagrams are also used to determine prevailing mechanisms. The microstructure of sintered materials has been studied by using image quantitative analysis, thus by using a morphological approach to sintering. Morphological parameters allow, on the one hand, the evolution of powders during sintering to be followed, and, on the other hand, sintered products to be correctly characterised. Moreover, the author reports the study of the evolution of some physical properties of sintered materials with respect to their microstructure parameters. This leads to the development of a modelling of the behaviour of these materials [fr

  9. Sintering of micro-trusses created by extrusion-3D-printing of lunar regolith inks

    Science.gov (United States)

    Taylor, Shannon L.; Jakus, Adam E.; Koube, Katie D.; Ibeh, Amaka J.; Geisendorfer, Nicholas R.; Shah, Ramille N.; Dunand, David C.

    2018-02-01

    The development of in situ fabrication methods for the infrastructure required to support human life on the Moon is necessary due to the prohibitive cost of transporting large quantities of materials from the Earth. Cellular structures, consisting of a regular network (truss) of micro-struts with ∼500 μm diameters, suitable for bricks, blocks, panels, and other load-bearing structural elements for habitats and other infrastructure are created by direct-extrusion 3D-printing of liquid inks containing JSC-1A lunar regolith simulant powders, followed by sintering. The effects of sintering time, temperature, and atmosphere (air or hydrogen) on the microstructures, mechanical properties, and magnetic properties of the sintered lunar regolith micro-trusses are investigated. The air-sintered micro-trusses have higher relative densities, linear shrinkages, and peak compressive strengths, due to the improved sintering of the struts within the micro-trusses achieved by a liquid or glassy phase. Whereas the hydrogen-sintered micro-trusses show no liquid-phase sintering or glassy phase, they contain metallic iron 0.1-2 μm particles from the reduction of ilmenite, which allows them to be lifted with magnets.

  10. In Situ Cleanable Alternative HEPA Filter Media

    International Nuclear Information System (INIS)

    Adamson, D. J.; Terry, M. T.

    2002-01-01

    The Westinghouse Savannah River Company, located at the Savannah River Site in Aiken, South Carolina, is currently testing two types of filter media for possible deployment as in situ regenerable/cleanable High Efficiency Particulate Air (HEPA) filters. The filters are being investigated to replace conventional, disposable, glass-fiber, HEPA filters that require frequent removal, replacement, and disposal. This is not only costly and subjects site personnel to radiation exposure, but adds to the ever-growing waste disposal problem. The types of filter media being tested, as part of a National Energy Technology Laboratory procurement, are sintered nickel metal and ceramic monolith membrane. These media were subjected to a hostile environment to simulate conditions that challenge the high-level waste tank ventilation systems. The environment promoted rapid filter plugging to maximize the number of filter loading/cleaning cycles that would occur in a specified period of time. The filters were challenged using nonradioactive simulated high-level waste materials and atmospheric dust; materials that cause filter pluggage in the field. The filters are cleaned in situ using an aqueous solution. The study found that both filter media were insensitive to high humidity or moisture conditions and were easily cleaned in situ. The filters regenerated to approximately clean filter status even after numerous plugging and in situ cleaning cycles. Air Techniques International is conducting particle retention testing on the filter media at the Oak Ridge Filter Test Facility. The filters are challenged using 0.3-mm di-octyl phthalate particles. Both the ceramic and sintered media have a particle retention efficiency > 99.97%. The sintered metal and ceramic filters not only can be cleaned in situ, but also hold great potential as a long life alternative to conventional HEPA filters. The Defense Nuclear Facility Safety Board Technical Report, ''HEPA Filters Used in the Department of

  11. In situ characterization of nanoscale catalysts during anodic redox processes

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Renu [National Institute of Standards and Technology; Crozier, Peter [Arizona State University; Adams, James [Arizona State University

    2013-09-19

    Controlling the structure and composition of the anode is critical to achieving high efficiency and good long-term performance. In addition to being a mixed electronic and ionic conductor, the ideal anode material should act as an efficient catalyst for oxidizing hydrogen, carbon monoxide and dry hydrocarbons without de-activating through either sintering or coking. It is also important to develop novel anode materials that can operate at lower temperatures to reduce costs and minimized materials failure associated with high temperature cycling. We proposed to synthesize and characterize novel anode cermets materials based on ceria doped with Pr and/or Gd together with either a Ni or Cu metallic components. Ceria is a good oxidation catalyst and is an ionic conductor at room temperature. Doping it with trivalent rare earths such as Pr or Gd retards sintering and makes it a mixed ion conductor (ionic and electronic). We have developed a fundamental scientific understanding of the behavior of the cermet material under reaction conditions by following the catalytic oxidation process at the atomic scale using a powerful Environmental Scanning Transmission Electron Microscope (ESTEM). The ESTEM allowed in situ monitoring of structural, chemical and morphological changes occurring at the cermet under conditions approximating that of typical fuel-cell operation. Density functional calculations were employed to determine the underlying mechanisms and reaction pathways during anode oxidation reactions. The dynamic behavior of nanoscale catalytic oxidation of hydrogen and methane were used to determine: ? Fundamental processes during anodic reactions in hydrogen and carbonaceous atmospheres ? Interfacial effects between metal particles and doped ceria ? Kinetics of redox reaction in the anode material

  12. A field-scale test of in situ chemical oxidation through recirculation

    International Nuclear Information System (INIS)

    West, O.R.; Cline, S.R.; Holden, W.L.; Gardner, F.G.; Schlosser, B.M.; Siegrist, R.L.; Houk, T.C.

    1998-01-01

    In situ chemical oxidation is a developing class of remediation technologies in which organic contaminants are degraded in place by powerful oxidants. Successful implementation of this technology requires an effective means for dispersing the oxidant to contaminated regions in the subsurface. An oxidant delivery technique has been developed wherein the treatment solution is made by adding an oxidant to extracted groundwater. The oxidant-laden groundwater is then injected and recirculated into a contaminated aquifer through multiple horizontal and/or vertical wells. This technique, referred to as in situ chemical oxidation through recirculation (ISCOR), can be applied to saturated and hydraulically conductive formations and used with relatively stable oxidants such as potassium permanganate (KMnO 4 ). A field-scale test of ISCOR was conducted at a site (Portsmouth Gaseous Diffusion Plant) where groundwater in a 5-ft thick silty gravel aquifer is contaminated with trichloroethylene (TCE) at levels that indicate the presence of residual dense non-aqueous phase liquids (DNAPLs). The field test was implemented using a pair of parallel horizontal wells with 200-ft screened sections. For approximately one month, groundwater was extracted from one horizontal well, dosed with crystalline KMnO 4 , and re-injected into the other horizontal well 90 ft away. Post-treatment characterization showed that ISCOR was effective at removing TCE in the saturated region. Lateral and vertical heterogeneities within the treatment zone impacted the uniform delivery of the oxidant solution. However, TCE was not detected in groundwater samples collected from monitoring wells and soil samples from borings in locations where the oxidant had permeated

  13. The application of in situ analytical transmission electron microscopy to the study of preferential intergranular oxidation in Alloy 600

    Energy Technology Data Exchange (ETDEWEB)

    Burke, M.G., E-mail: m.g.burke@manchester.ac.uk; Bertali, G.; Prestat, E.; Scenini, F.; Haigh, S.J.

    2017-05-15

    In situ analytical transmission electron microscopy (TEM) can provide a unique perspective on dynamic reactions in a variety of environments, including liquids and gases. In this study, in situ analytical TEM techniques have been applied to examine the localised oxidation reactions that occur in a Ni-Cr-Fe alloy, Alloy 600, using a gas environmental cell at elevated temperatures. The initial stages of preferential intergranular oxidation, shown to be an important precursor phenomenon for intergranular stress corrosion cracking in pressurized water reactors (PWRs), have been successfully identified using the in situ approach. Furthermore, the detailed observations correspond to the ex situ results obtained from bulk specimens tested in hydrogenated steam and in high temperature PWR primary water. The excellent agreement between the in situ and ex situ oxidation studies demonstrates that this approach can be used to investigate the initial stages of preferential intergranular oxidation relevant to nuclear power systems. - Highlights: • In situ analytical TEM has been performed in 1 bar H{sub 2}-H{sub 2}O vapor at 360–480 °C. • Nanoscale GB migration and solute partitioning correlate with ex situ data for Alloy 600 in H{sub 2}-steam. • This technique can provide new insights into localised reactions associated with localised oxidation.

  14. Two-step sintering of ultrafine-grained barium cerate proton conducting ceramics

    International Nuclear Information System (INIS)

    Wang, Siwei; Zhang, Lei; Zhang, Lingling; Brinkman, Kyle; Chen, Fanglin

    2013-01-01

    Ultra-fine grained dense BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3−δ (BZCYYb) ceramics have been successfully prepared via a two-step sintering method. Co-precipitation method has been adopted to prepare nano-sized BZCYYb precursors with an average particle size of 30 nm. By controlling the sintering profile, an average grain size of 184 nm was obtained for dense BZCYYb ceramics via the two-step sintering method, compared to 445 nm for the conventional sintered samples. The two-step sintered BZCYYb samples showed less impurity and an enhanced electrical conductivity compared with the conventional sintered ones. Further, the two-step sintering method was applied to fabricate anode supported solid oxide fuel cells (SOFCs) using BZCYYb as the electrolyte, resulting in dense ultrafine-grained electrolyte membranes and porous anode substrates with fine particles. Due to the reduced ohmic as well as polarization resistances, the maximum power output of the cells fabricated from the two-step sintering method reached 349 mW m −2 at 700 °C, significantly improved from 172 mW cm −2 for the conventional sintered cells, suggesting that two-step sintering method is very promising for optimizing the microstructure and thus enhancing the electrochemical performances for barium cerate based proton-conducting SOFCs.

  15. Study on the characteristics and sinterability of DUPIC powder by using simulated fuel

    International Nuclear Information System (INIS)

    Lee, Jae-Won; Lee, Jung-Won; Kim, Jong-Ho; Yim, Sung-Paal; Lee, Young-Woo; Yang, Myung-Seung

    2002-01-01

    The sinterability of the OREOX (oxidation and reduction of oxide fuels) powder was investigated in terms of the number of the OREOX cycles and milling time using simulated spent fuel of an equivalent burnup of 35,000 MWD/MTU. Wet milled powder was prepared and sintered to compare the morphology and sinterability with the dry milled powder. Powders having a medium particle size of less than 1μm were obtained by dry milling of OREOX powders regardless of the number of cycles. The specific surface area of the simulated DUPIC powder was governed by the number of OREOX cycles rather than by milling time. The sound pellets with a sintered density of higher than 95% TD and average grain size of larger than 8μm were obtained with the dry milled powder after 1 cycle of OREOX treatment. The powders prepared by dry milling for a short time and wet milling for a long time after 3 cycles of OREOX treatment also produced pellets with a sintered density of higher than 95% TD and average grain size of larger than 8μm. (author)

  16. Oxidation protection and behavior of in-situ zirconium diboride–silicon carbide coating for carbon/carbon composites

    International Nuclear Information System (INIS)

    Li, Lu; Li, Hejun; Yin, Xuemin; Chu, Yanhui; Chen, Xi; Fu, Qiangang

    2015-01-01

    Highlights: • ZrB 2 –SiC coating was prepared on C/C composite by in-situ reaction. • A two-layered structure was obtained when the coating was oxidized at 1500 °C. • The formation and collapse of bubbles influenced the coating oxidation greatly. • The morphology evolution of oxide scale during oxidation was illuminated. - Abstract: To protect carbon/carbon (C/C) composites against oxidation, zirconium diboride–silicon carbide (ZrB 2 –SiC) coating was prepared by in-situ reaction using ZrC, B 4 C and Si as raw materials. The in-situ ZrB 2 –SiC coated C/C presented good oxidation resistance, whose weight loss was only 0.15% after isothermal oxidation at 1500 °C for 216 h. Microstructure evolution of coating at 1500 °C was studied, revealing a two-layered structure: (1) ZrO 2 (ZrSiO 4 ) embedded in SiO 2 -rich glass, and (2) unaffected ZrB 2 –SiC. The formation and collapse of bubbles influenced the coating oxidation greatly. A model based on the evolution of oxide scale was proposed to explain the failure mechanism of coating

  17. Influence of sintering temperature on the properties of pulsed electric current sintered hybrid coreshell powders

    Czech Academy of Sciences Publication Activity Database

    Mahmed, N.; Larismaa, J.; Heczko, Oleg; Cura, M.E.; Hannula, S.-P.

    2013-01-01

    Roč. 33, č. 12 (2013), s. 2233-2239 ISSN 0955-2219 R&D Projects: GA ČR(CZ) GAP107/11/0391 Institutional support: RVO:68378271 Keywords : sintering * silver * iron oxide * SiO 2 * phase transformation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.307, year: 2013 http://dx.doi.org/10.1016/j.jeurceramsoc.2012.12.023

  18. In Situ Study of Noncatalytic Metal Oxide Nanowire Growth

    DEFF Research Database (Denmark)

    Rackauskas, Simas; Jiang, Hua; Wagner, Jakob Birkedal

    2014-01-01

    a catalyst is still widely disputed and unclear. Here, we show that the nanowire growth during metal oxidation is limited by a nucleation of a new layer. On the basis of in situ transmission electron microscope investigations we found that the growth occurs layer by layer at the lowest specific surface...

  19. Determination of oxygen to metal ratio for varying UO2 content in sintered (U,Th)O2 pellet by oxidation-reduction method using thermo-gravimetric analyser

    International Nuclear Information System (INIS)

    Mahanty, B.N.; Khan, F.A.; Karande, A.P.; Prakash, A.; Afzal, Md.; Panakkal, J.P.

    2009-01-01

    Experiments were carried out to determine oxygen to metal ratio in 4%, 6%, 10%, 20%, 50% and 80% UO 2 in sintered (U, Th) O 2 pellets by oxidation-reduction method using thermo gravimetric analyser. (author)

  20. Sintering process of Eu doped luminescent glass prepared from porous glass

    International Nuclear Information System (INIS)

    Akai, T; Murakami, M; Yamashita, M; Okajima, T; Umesaki, N

    2011-01-01

    Eu doped high silica glass prepared by sintering porous glass exhibits blue luminescence with high quantum efficiency. In this work, we studied effects of sintering temperature on valance state of europium ion. To investigate a change of valance state of Eu, X-ray absorption near edge structure (XANES) spectroscopy measurements were carried out. Intensity of blue emission at around 430nm drastically increases when the sintering temperature is above 1000 deg. C. From XANES spectra, it is found that almost all the Eu exist as Eu 3+ in a samples sintered below 900 deg. C, while more than 70% of Eu exist as Eu 2+ in the sample sintered at 1050 deg. C and 1100 deg. C. The drastic change of oxidation state of europium ion between 900 and 1050 deg. C is discussed in relation to the structural change probed by infrared (IR) spectroscopy.

  1. Sintering of MSW fly ash for reuse as a concrete aggregate.

    Science.gov (United States)

    Mangialardi, T

    2001-10-12

    The sintering process of municipal solid waste (MSW) fly ash was investigated in order to manufacture sintered products for reuse as concrete aggregates. Four types of fly ash resulting from different Italian MSW incineration plants were tested in this study. A modification of the chemical composition of MSW fly ash--through a preliminary four-stage washing treatment of this material with water--was attempted to improve the chemical and mechanical characteristics of sintered products.The sintering treatment of untreated or washed fly ash was performed on cylindrical compact specimens (15 mm in diameter and 20mm in height) at different compact pressures, sintering temperatures and times.The sintering process of untreated MSW fly ashes proved to be ineffective for manufacturing sintered products for reuse as a construction material, because of the adverse chemical characteristics of these fly ashes in terms of sulfate, chloride, and vitrifying oxide contents.A preliminary washing treatment of MSW fly ash with water greatly improved the chemical and mechanical characteristics of sintered products and, for all the types of fly ash tested, the sintered products satisfied the Italian requirements for normal weight aggregates for use in concretes having a specified strength not greater than 12 and 15N/mm(2), when measured on cylindrical and cubic specimens, respectively.A compact pressure of 28 N/mm(2), a sintering temperature of 1140 degrees C, and a sintering time of 60 min were the best operating conditions for manufacturing sintered products of washed MSW fly ash.

  2. Properties and Structure of In Situ Transformed PAN-Based Carbon Fibers

    Directory of Open Access Journals (Sweden)

    Jingjing Cao

    2018-06-01

    Full Text Available Carbon fibers in situ prepared during the hot-pressed sintering in a vacuum is termed in situ transformed polyacrylonitrile-based (PAN-based carbon fibers, and the fibrous precursors are the pre-oxidized PAN fibers. The properties and structure of in situ transformed PAN-based carbon fibers are investigated by Nano indenter, SEM, TEM, XRD, and Raman. The results showed that the microstructure of the fiber surface layer was compact, while the core was loose, with evenly-appearing microvoids. The elastic modulus and nanohardness of the fiber surface layer (303.87 GPa and 14.82 GPa were much higher than that of the core (16.57 GPa and 1.54 GPa, and its interlayer spacing d002 and crystallinity were about 0.347 nm and 0.97 respectively. It was found that the preferred orientation of the surface carbon layers with ordered carbon atomic arrangement tended to be parallel to the fiber axis, whereas the fiber core in the amorphous region exhibited a random texture and the carbon atomic arrangement was in a disordered state. It indicates that the in situ transformed PAN-based carbon fibers possess significantly turbostratic structure and anisotropy.

  3. Experimental investigation of in situ cleanable HEPA filter

    International Nuclear Information System (INIS)

    Adamson, D.J.

    1999-01-01

    The Westinghouse Savannah River Company located at the Savannah River Site (SRS) in Aiken, South Carolina is currently testing the feasibility of developing an in situ cleanable high efficiency particulate air (HEPA) filter system. Sintered metal filters are being tested for regenerability or cleanability in simulated conditions found in a high level waste (HLW) tank ventilation system. The filters are being challenged using materials found in HLW tanks. HLW simulated salt, HLW simulated sludge and South Carolina road dust. Various cleaning solutions have been used to clean the filters in situ. The tanks are equipped with a ventilation system to maintain the tank contents at negative pressure to prevent the release of radioactive material to the environment. This system is equipped with conventional disposable glass-fiber HEPA filter cartridges. Removal and disposal of these filters is not only costly, but subjects site personnel to radiation exposure and possible contamination. A test apparatus was designed to simulate the ventilation system of a HLW tank with an in situ cleaning system. Test results indicate that the Mott sintered metal HEPA filter is suitable as an in situ cleanable or regenerable HEPA filter. Data indicates that high humidity or water did not effect the filter performance and the sintered metal HEPA filter was easily cleaned numerous times back to new filter performance by an in situ spray system. The test apparatus allows the cleaning of the soiled HEPA filters to be accomplished without removing the filters from process. This innovative system would eliminate personnel radiation exposure associated with removal of contaminated filters and the high costs of filter replacement and disposal. The results of these investigations indicate that an in situ cleanable HEPA filter system for radioactive and commercial use could be developed and manufactured

  4. Sintering and electrical properties of strontium-doped lanthanum manganite

    Energy Technology Data Exchange (ETDEWEB)

    Tarrago, Diego Pereira; Sousa, Vania Caldas de [Universidade Federal do Rio Grande do Sul (LABIOMAT/PPGEM/UFRGS), Porto Alegre, RS (Brazil). Programa de Pos-Graduacao em Engenharia de Minas, Metalurgica e de Materiais. Lab. de Biomateriais], Email: dptarrago@gmail.com; Moreno Buriel, Berta; Chinarro Martini, Eva; Jurado Egea, Jose Ramon [Consejo Superior de Investigaciones Cientificas (ICV/CSIC), Madrid (Spain). Inst. de Ceramica y Vidrio; Malfatti, Celia de Fraga [Universidade Federal do Rio Grande do Sul (LAPEC/PPGEM/UFRGS), Porto Alegre, RS (Brazil). Programa de Pos-Graduacao em Engenharia de Minas, Metalurgica e de Materiais. Lab. de Pesquisa em Corrosao

    2010-07-01

    Lanthanum strontium manganites (LSM) are potential materials for cathode applications in solid oxide fuel cells (SOFC) due to their good catalytic activity, chemical stability and compatibility with electrolyte materials in high temperatures. The sinterability of single phase La{sub 1-x}Sr{sub x}Mn{sub O3} (x=0.18) perovskite powders and the electrical properties of the resulting samples are analyzed in this study. Using a heating microscope, the powders were pressed and sintered at different pressures and temperatures, resulting in an open porosity of 33.36% when compacted at 125 MPa and sintered at 1200 degree C. Top and cross-section s canning electron microscopy (SEM) micrographs revealed interconnected pores in the sintered body and, hence, a suitable microstructure for the application. The activation energy for conductance was 0.04 eV and the tested LSM bulk started to exhibit adequate electrical properties at about 500 degree C. (author)

  5. On bacteria oxidizing enlargement scale test for uranium in-situ leaching at. 381 mine

    International Nuclear Information System (INIS)

    Hu Kaiguang; Wang Qingliang; Liu Yingjiu; Shi Wenge; Hu Shihe; Hu Yincai; Fang Qiu

    1999-01-01

    The results of enlarged scale test of bacteria as oxidizer for uranium in-situ leaching at No 381 mine showed that redox potential of the oxidized absorbed tailing water by bacteria is more than 510 mV, without any effects on after treatments by using bacteria as oxidizer and reduce oxidizer costs 70% compared with H 2 O 2 as oxidizer

  6. Predicting sintering deformation of ceramic film constrained by rigid substrate using anisotropic constitutive law

    International Nuclear Information System (INIS)

    Li Fan; Pan Jingzhe; Guillon, Olivier; Cocks, Alan

    2010-01-01

    Sintering of ceramic films on a solid substrate is an important technology for fabricating a range of products, including solid oxide fuel cells, micro-electronic PZT films and protective coatings. There is clear evidence that the constrained sintering process is anisotropic in nature. This paper presents a study of the constrained sintering deformation using an anisotropic constitutive law. The state of the material is described using the sintering strains rather than the relative density. In the limiting case of free sintering, the constitutive law reduces to a conventional isotropic constitutive law. The anisotropic constitutive law is used to calculate sintering deformation of a constrained film bonded to a rigid substrate and the compressive stress required in a sinter-forging experiment to achieve zero lateral shrinkage. The results are compared with experimental data in the literature. It is shown that the anisotropic constitutive law can capture the behaviour of the materials observed in the sintering experiments.

  7. Microwave Sintering of Ceramic Materials for Industrial Application Final Report CRADA No. TC-1116-95

    Energy Technology Data Exchange (ETDEWEB)

    Caplan, M. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Tandon, R. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Callis, R. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2017-10-19

    The goal of this project was to develop the commercial capability in the US to sinter alumina oxide ceramic parts for the semiconductor manufacturing equipment industry. We planned to use the millimeter microwave (30 GHz) sintering system first developed by IAP in Russia.

  8. Co-sintering of CGO/NIO-CGO bilayers for solid oxide fuel cell

    International Nuclear Information System (INIS)

    Neto, P.P.B.; Grilo, J.P.F.; Souza, G.L.; Macedo, D.A.; Paskocimas, C.A.; Nascimento, R.M.

    2012-01-01

    Reducing the operating temperature of solid oxide fuel cells (SOFC) for the range between 500 and 700°C is one of the challenges which more has aroused the interest of research in SOFC in recent years. In this context, the bilayer anode/electrolyte composed of a porous support based on Ni-doped ceria (anode) and a ceria doped gadolinia (CGO) electrolyte, presents itself as one of the half-cell configurations of the most interest towards the production of electricity in the operating logic of a SOFC. In this work, CGO films were successfully prepared on NiO-CGO substrates using the resources of the screen-printing technique. The bi-layers were co-sintered between 1350 and 1450 ° C for 4 h and then characterized by scanning electron microscopy and energy dispersive X-ray spectroscopy (EDS). The results showed good adhesion at the film/substrate interface and no cracks in the films. (author)

  9. In Situ Chemical Oxidation Using Potassium Permanganate. Innovative Technology Summary Report

    International Nuclear Information System (INIS)

    1999-01-01

    The In Situ Chemical Oxidation Using Potassium Permanganate [KMnO4] treats soils or groundwater contaminated with a range of organic chemicals, including trichlorethylene. Potential application to metal and radionuclide contaminants, including oxidation/immobilization of uranium, is being investigated. This technology is designed for use with efficient delivery systems, such as the Multi-Point Injection System and Deep Soil Mixing, to treat contaminants in low permeability soils

  10. Role of Cu During Sintering of Fe0.96Cu0.04 Nanoparticles

    Science.gov (United States)

    Sivaprahasam, D.; Sriramamurthy, A. M.; Bysakh, S.; Sundararajan, G.; Chattopadhyay, K.

    2018-04-01

    Nanoparticle agglomerates of passivated Fe ( n-Fe) and Fe0.96Cu0.04 ( n-Fe0.96Cu0.04), synthesized through the levitational gas condensation (LGC) process, were compacted and sintered using the conventional powder metallurgy method. The n-Fe0.96Cu0.04 agglomerates produced lower green density than n-Fe, and when compacted under pressure beyond 200 MPa, they underwent lateral cracking during ejection attributed to the presence of a passive oxide layer. Sintering under dynamic hydrogen atmosphere can produce a higher density of compact in n-Fe0.96Cu0.04 in comparison to n-Fe. Both the results of dilatometry and thermogravimetric (TG) measurements of the samples under flowing hydrogen revealed enhancement of the sintering process as soon as the reduction of oxide layers could be accomplished. The shrinkage rate of n-Fe0.96Cu0.04 reached a value three times higher than n-Fe at a low temperature of 723 K (450 °C) during heating. This enhanced shrinkage rate was the manifestation of accumulation of Cu at the surface of the particles. The formation of a thin-surface melted layer enriched with copper during heating to isothermal holding facilitated as a medium of transport for diffusion of the elements. The compacts produced by sintering at 773 K (500 °C), with relative density 82 pct, were found to be unstable and oxidized instantly when exposed to ambient atmosphere. The stable compacts of density more than 92 pct with 300- to 450-nm grain size could only be produced when sintering was carried out at 973 K (700 °C) and beyond. The 0.22 wt pct residual oxygen obtained in the sintered compact is similar to what is used for conventional ferrous powder metallurgy products.

  11. Phase identification and morphology study of hematite (Fe2O3) with sintering time varitions

    Science.gov (United States)

    Yazirin, Cepi; Puspitasari, Poppy; Sasongko, Muhammad Ilman Nur; Tsamroh, Dewi Izzatus; Risdanareni, Puput

    2017-09-01

    Iron oxide has been the interest of many studies due to its applications in various scientific and industrial fields including in environment, corrosion, soil science, and exhaust emissions. Iron oxide (Fe2O3) has potential applications in catalytic reactions in electronic devices such as semiconductors, paint formulations, and lithium rechargeable batteries. Fe2O3 can be synthesized through the process of stirring, decomposition of organic iron, sol-gel, combustion, and evaporating solvents. Most of the methods used involve several steps and take a long time. The aim of this research was to investigate the phase and morphology characterization of iron oxide (Fe2O3) powder with solvent ethylene glycol after being sintered for 1 hour, 2 hours and 3 hours. The characterization tools utilized were XRD, SEM-EDX, and FTIR. The results of XRD analysis showed that the Fe2O3 sintered for 1 hour had the smallest crystallite size with a diameter of 21.05 nm. In the XRD test, the beam of X-ray was shot directly at the grain being tested. The results of SEM analysis showed thatthe Fe2O3 sintered for 1 hour produced the best result due to its crystallite size of 12.36 nm and hada shape of homogeneous nanosphere; the duration of sintering indeed had a great influence on the grain size of iron oxide (Fe2O3). In addition, the results of the elemental composition analysis indicate that the longer the sintering process, the higher the concentration of O but the lower the Fe.

  12. Polyacrylamide grafting of modified graphene oxides by in situ free radical polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Mingyi [Department of Applied Chemistry, School of Science, Tianjin University of Commerce, Tianjin 300134 (China); Xu, Xiaoyang, E-mail: xiaoyangxu2012@163.com [School of Science, Tianjin University, Tianjin 30072 (China); Wu, Tao [School of Science, Tianjin University, Tianjin 30072 (China); Zhang, Sai; Li, Xianxian [Department of Applied Chemistry, School of Science, Tianjin University of Commerce, Tianjin 300134 (China); Li, Yi, E-mail: liyi@tju.edu.cn [School of Science, Tianjin University, Tianjin 30072 (China)

    2014-12-15

    Highlights: • Graphene oxide (GO) was modified by chemical reactions to functionalized GO (FGO). • The FGOs and the GO were then subjected to in situ free radical polymerization. • Hydroxyl groups of GO were the most reactive grafting sites. - Abstract: Graphene oxide (GO) was modified using chemical reactions to obtain three types of functionalized GO sheets (FGO). The FGO sheets and the GO were then subjected to in situ free radical polymerization in order to study the grafting polymerization. The FGO and grafted-.FGO were analyzed with Fourier transform infrared spectroscopy, scanning electronic microscopy, thermo-gravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS). The grafting percentages in the materials were calculated using the TGA and XPS results. The FGO sheets with different functional groups exhibited different grafting abilities, and hydroxyl groups were proven to be the most reactive grafting sites for the in situ free radical grafting polymerization of polyacrylamide.

  13. Polyacrylamide grafting of modified graphene oxides by in situ free radical polymerization

    International Nuclear Information System (INIS)

    Tang, Mingyi; Xu, Xiaoyang; Wu, Tao; Zhang, Sai; Li, Xianxian; Li, Yi

    2014-01-01

    Highlights: • Graphene oxide (GO) was modified by chemical reactions to functionalized GO (FGO). • The FGOs and the GO were then subjected to in situ free radical polymerization. • Hydroxyl groups of GO were the most reactive grafting sites. - Abstract: Graphene oxide (GO) was modified using chemical reactions to obtain three types of functionalized GO sheets (FGO). The FGO sheets and the GO were then subjected to in situ free radical polymerization in order to study the grafting polymerization. The FGO and grafted-.FGO were analyzed with Fourier transform infrared spectroscopy, scanning electronic microscopy, thermo-gravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS). The grafting percentages in the materials were calculated using the TGA and XPS results. The FGO sheets with different functional groups exhibited different grafting abilities, and hydroxyl groups were proven to be the most reactive grafting sites for the in situ free radical grafting polymerization of polyacrylamide

  14. Ash chemistry and sintering, verification of the mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Hupa, M.; Skrifvars, B.J. [Aabo Akademi, Turku (Finland)

    1996-12-01

    In this project four sintering mechanisms have been studied, i.e., partial melting with a viscous liquid, partial melting with a non-viscous liquid, chemical reaction sintering and solid state sintering. The work has aimed at improving the understanding of ash sintering mechanisms and quantifying their role in combustion and gasification. The work has been oriented in particular on the understanding of biomass ash behavior. The work has not directly focused on any specific technical application. However, results can also be applied on other fuels such as brown coal, petroleum coke, black liquor and different types of wastes (PDF, RDF, MSW). In one part of study the melting behavior was calculated for ten biomass ashes and compared with lab measurements of sintering tendencies. The comparison showed that the T{sub 15} temperatures, i.e. those temperatures at which the ashes contained 15 % molten phase, correlated fairly well with the temperature at which the sintering measurements detected sintering. This suggests that partial melting can be predicted fairly accurate for some ashes already with the today existing thermodynamic calculation routines. In some cases, however the melting calculations did not correlate with the detected sintering temperatures. In a second part detailed measurements on ash behavior was conducted both in a semi full scale CFB and a lab scale FBC. Ashes and deposits were collected and analyzed in several different ways. These analyses show that the ash chemistry shifts radically when the fuel is shifted. Fuels with silicate based ashes behaved totally different than those with an oxide or salt based ash. The chemistry was also affected by fuel blending. The ultimate goal has been to be able to predict the ash thermal behavior during biomass thermal conversion, using the fuel and ash elemental analyses and a few operational key parameters as the only input data. This goal has not yet today been achieved. (author)

  15. Study on the isothermal oxidation behavior in air of Ti3AlC2 sintered by hot pressing

    Institute of Scientific and Technical Information of China (English)

    XU Xuewen; LI Yangxian; MEI Bingchu; ZHU Jiaoqun; LIU Heyan; QU Jingping

    2006-01-01

    The isothermal oxidation behavior at 900―1300℃ for 20 h in air of bulk Ti3AlC2 with 2.8 wt% TiC sintered by means of hot pressing was investigated in the work. The isothermal oxidation behavior generally followed a parabolic rate law. The parabolic rate constants increased from 1.39×10-10 kg2·m-4·s-1 at 900℃ to 5.56×10-9 kg2·m-4·s-1 at 1300℃. The calculated activation energy was 136.45 kJ/mol. It was demonstrated that Ti3AlC2 had excellent oxidation resistance due to the continuous, dense and adhesive protect scales consisted of a mass of α-Al2O3 and a little of TiO2 and/or Al2TiO5. In principle, the oxide scale was grown by the inward diffusion of O2- and the outward diffusion of Ti4+ and Al3+. The rapid outward diffusion of cations usually resulted in the formation of cracks, gaps, and holes.

  16. Microstructural evaluation of the NbC-20Ni cemented carbides during sintering

    International Nuclear Information System (INIS)

    Rodrigues, D.; Cannizza, E.

    2016-01-01

    Full text: Fine carbides in a metallic matrix (binder) form the microstructure of the cemented carbides. Grain size and binder content are the main variables to adjust hardness and toughness. These products are produced by Powder Metallurgy, and traditional route involves mixing carbides with binder by high energy milling, pressing and sintering. During sintering, a liquid phase promotes densification, and a final relative density higher than 99% is expected. Sintering is carried out at high temperatures, and dissolution of the carbides changes the chemical composition of the binder. To control grain growth of the main carbide, which reduces hardness, small quantities of secondary carbides are used. These additives limit dissolution and precipitation of the main carbides reducing the final grain size. This paper focused the structural and chemical evolution during sintering using NbC-20Ni cermets. Mixtures of very fine NbC carbides and carbonyl Ni powders were produce by intense milling. These mixtures were pressed using uniaxial pressures from 50 to 200MPa. Shrinkage was evaluated using dilatometric measurements under an atmosphere of dynamic argon. Samples were also sintered under vacuum in high temperature industrial furnace. The sintered samples were characterized in terms of density hardness, toughness and microstructure. DRX was the main tool used to evaluate the structural evolution of the binder. In situ chemical analysis helped to understand the dissolution mechanisms. (author)

  17. On the Role of the Electrical Field in Spark Plasma Sintering of UO2+x

    Science.gov (United States)

    Tyrpekl, Vaclav; Naji, Mohamed; Holzhäuser, Michael; Freis, Daniel; Prieur, Damien; Martin, Philippe; Cremer, Bert; Murray-Farthing, Mairead; Cologna, Marco

    2017-01-01

    The electric field has a large effect on the stoichiometry and grain growth of UO2+x during Spark Plasma Sintering. UO2+x is gradually reduced to UO2.00 as a function of sintering temperature and time. A gradient in the oxidation state within the pellets is observed in intermediate conditions. The shape of the gradient depends unequivocally on the direction of the electrical field. The positive surface of the pellet shows a higher oxidation state compared to the negative one. An area with larger grain size is found close to the positive electrode, but not in contact with it. We interpret these findings with the redistribution of defects under an electric field, which affect the stoichiometry of UO2+x and thus the cation diffusivity. The results bear implications for understanding the electric field assisted sintering of UO2 and non-stoichiometric oxides in general. PMID:28422164

  18. Real time nanoscale structural evaluation of gold structures on Si (100) surface using in-situ transmission electron microscopy

    International Nuclear Information System (INIS)

    Rath, A.; Juluri, R. R.; Satyam, P. V.

    2014-01-01

    Transport behavior of gold nanostructures on Si(100) substrate during annealing under high vacuum has been investigated using in-situ real time transmission electron microscopy (TEM). A comparative study has been done on the morphological changes due to annealing under different vacuum environments. Au thin films of thickness ∼2.0 nm were deposited on native oxide covered silicon substrate by using thermal evaporation system. In-situ real time TEM measurements at 850 °C showed the isotropic growth of rectangular/square shaped gold-silicon alloy structures. During the growth, it is observed that the alloying occurs in liquid phase followed by transformation into the rectangular shapes. For similar system, ex-situ annealing in low vacuum (10 −2 millibars) at 850 °C showed the spherical gold nanostructures with no Au-Si alloy formation. Under low vacuum annealing conditions, the rate of formation of the oxide layer dominates the oxide desorption rate, resulting in the creation of a barrier layer between Au and Si, which restricts the inter diffusion of Au in to Si. This work demonstrates the important role of interfacial oxide layer on the growth of nanoscale Au-Si alloy structures during the initial growth. The time dependent TEM images are presented to offer a direct insight into the fundamental dynamics of the sintering process at the nanoscale

  19. Assessment of consolidation of oxide dispersion strengthened ferritic steels by spark plasma sintering: from laboratory scale to industrial products

    International Nuclear Information System (INIS)

    Boulnat, X.; Fabregue, D.; Perez, M.; Urvoy, S.; Hamon, D.; Carlan, Y. de

    2014-01-01

    Oxide dispersion strengthened steels are new generation alloys that are usually processed by hot isostatic pressing (HIP). In this study, spark plasma sintering (SPS) was studied as an alternative consolidation technique. The influence of the processing parameters on the microstructure was quantified. The homogeneity of the SPSed materials was characterised by electron microprobe and microhardness. A combination of limited grain growth and minimised porosity can be achieved on semi-industrial compact. Excellent tensile properties were obtained compared to the literature. (authors)

  20. Uranium oxidation kinetics monitored by in-situ X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Zalkind, S., E-mail: shimonzl@nrcn.org.il; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

    2017-03-15

    The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90–150 °C was studied by means of in-situ X-ray diffraction (XRD). A “breakaway” in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO{sub 2}(111) is the prominent one. As the oxide thickens, the growth rate of UO{sub 2}(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Q{sub parabolic} = 17.5 kcal/mol and Q{sub linear} = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

  1. Pressureless sintering of dense Si3N4 and Si3N4/SiC composites with nitrate additives

    International Nuclear Information System (INIS)

    Kim, J.Y.; Iseki, Takayoshi; Yano, Toyohiko

    1996-01-01

    The effect of aluminum and yttrium nitrate additives on the densification of monolithic Si 3 N 4 and a Si 3 N 4 /SiC composite by pressureless sintering was compared with that of oxide additives. The surfaces of Si 3 N 4 particles milled with aluminum and yttrium nitrates, which were added as methanol solutions, were coated with a different layer containing Al and Y from that of Si 3 N 4 particles milled with oxide additives. Monolithic Si 3 N 4 could be sintered to 94% of theoretical density (TD) at 1,500 C with nitrate additives. The sintering temperature was about 100 C lower than the case with oxide additives. After pressureless sintering at 1,750 C for 2 h in N 2 , the bulk density of a Si 3 N 4 /20 wt% SiC composite reached 95% TD with nitrate additives

  2. Porous Fe21Cr7Al1Mo0.5Y metal supports for oxygen transport membranes: Thermo-mechanical properties, sintering and corrosion behaviour

    DEFF Research Database (Denmark)

    Glasscock, Julie; Mikkelsen, Lars; Persson, Åsa Helen

    2013-01-01

    and creep rates are sufficiently low. Ceramic interlayers with graded porosity and pore-size were applied and co-fired with the metal supports, producing substrates that were shown to be viable for a 3 μm dense Ce 0.8Gd0.2O1.9 - δ oxygen transport membrane deposited using sputtering. © 2013 Elsevier B.V....... are optimised simultaneously in-situ during sintering by controlling the growth rate of the oxide scale. Oxidation of metal supports with 20-40% porosity at 850 C and oxygen partial pressure of 10- 11 kPa showed sub-parabolic kinetics and stability over 3000 h. The FeCrAl steel shows vastly superior oxidation...... resistance compared with an FeCr steel of similar composition and porosity. Modelling of the alloy lifetime as a function of surface area and Al-content was performed, and lifetimes over 30 000 h are predicted for a metal support with 30% porosity operating at a temperature of 750 C, where the oxidation...

  3. On the Mechanism of Microwave Flash Sintering of Ceramics

    Directory of Open Access Journals (Sweden)

    Yury V. Bykov

    2016-08-01

    Full Text Available The results of a study of ultra-rapid (flash sintering of oxide ceramic materials under microwave heating with high absorbed power per unit volume of material (10–500 W/cm3 are presented. Ceramic samples of various compositions—Al2O3; Y2O3; MgAl2O4; and Yb(LaO2O3—were sintered using a 24 GHz gyrotron system to a density above 0.98–0.99 of the theoretical value in 0.5–5 min without isothermal hold. An analysis of the experimental data (microwave power; heating and cooling rates along with microstructure characterization provided an insight into the mechanism of flash sintering. Flash sintering occurs when the processing conditions—including the temperature of the sample; the properties of thermal insulation; and the intensity of microwave radiation—facilitate the development of thermal runaway due to an Arrhenius-type dependency of the material’s effective conductivity on temperature. The proper control over the thermal runaway effect is provided by fast regulation of the microwave power. The elevated concentration of defects and impurities in the boundary regions of the grains leads to localized preferential absorption of microwave radiation and results in grain boundary softening/pre-melting. The rapid densification of the granular medium with a reduced viscosity of the grain boundary phase occurs via rotation and sliding of the grains which accommodate their shape due to fast diffusion mass transport through the (quasi-liquid phase. The same mechanism based on a thermal runaway under volumetric heating can be relevant for the effect of flash sintering of various oxide ceramics under a dc/ac voltage applied to the sample.

  4. Geochemical and Microbiological Characteristics during in Situ Chemical Oxidation and in Situ Bioremediation at a Diesel Contaminated Site

    NARCIS (Netherlands)

    Sutton, N.B.; Kalisz, M.; Krupanek, J.; Marek, J.; Grotenhuis, J.T.C.; Smidt, H.; Weert, de J.; Rijnaarts, H.H.M.; Gaans, van P.; Keijzer, T.

    2014-01-01

    While in situ chemical oxidation with persulfate has seen wide commercial application, investigations into the impacts on groundwater characteristics, microbial communities and soil structure are limited. To better understand the interactions of persulfate with the subsurface and to determine the

  5. On the oxidation behaviour of a Cu-10 vol% Cr in situ composite

    International Nuclear Information System (INIS)

    Haugsrud, R.; Lee, K.L.

    2005-01-01

    The oxidation behaviour of copper and Cu-10 vol% Cr in situ composite was studied at 400-700 deg. C in air and in argon containing 10 ppm O 2 . Oxidation kinetics was investigated by means of isothermal thermogravimetry and the oxide scales were characterized by scanning electron microscopy (SEM). The presence of the chromium fibres increases the oxidation resistance compared to unalloyed copper up to 600 deg. C. The oxidation mechanism and the influence of the different oxidation phenomena on the creep characteristics of the alloy composite are discussed

  6. Preparation of a sinterable beryllium oxide through decomposition of beryllium hydroxide (1963); Preparation d'un oxyde de beryllium frittable par decomposition de l'hydiloxyde (1963)

    Energy Technology Data Exchange (ETDEWEB)

    Bernier, M [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1963-07-01

    In the course of the present study, we have attempted to precise the factors which among the ones effective in the course of the preparation of the beryllium hydroxide and oxide and during the sintering have an influence on the final result: the density and homogeneity of the sintered body. Of the several varieties of hydroxides precipitated from a sulfate solution the {beta}-hydroxide only is always contaminated with beryllium sulfate and cannot be purified even by thorough washing. We noticed that those varieties of the hydroxide (gel, {alpha}, {beta}) have different decomposition rates; this behaviour is used to identify and even to dose the different species in ({alpha}, {beta}) mixtures. The various hydroxides transmit to the resulting oxides the shape they had when precipitated. Accordingly the history of the oxide is revealed by its behaviour during its fabrication and sintering. By comparing the results of the sintering operation with the various measurements performed on the oxide powders we are led to the conclusion that an oxide obtained from beryllium hydroxide is sinterable under vacuum if the following conditions are fulfilled: the particle size must lie between 0.1 and 0.2 {mu} and the BeSO{sub 4} content of the powder must be less than 0.25 per cent wt (expressed as SO{sub 3}/BeO). The best fitting is obtained with the oxide issued from an {alpha}-hydroxide precipitated as very small aggregates and with a low sulfur-content. We have observed that this is also the case for the oxide obtained by direct calcination of beryllium sulfate. (author) [French] Au cours de cette etude, nous avons cherche a preciser les facteurs qui, intervenant tout au long de la preparation de l'hydroxyde, puis de l'oxyde de beryllium et enfin du frittage, peuvent avoir une influence sur le resultat final: la densite et l'homogeneite du fritte. Parmi tous les hydroxydes precipites d'une solution de sulfate, seul l'hydroxyde {beta} est toujours fortement pollue par le sulfate

  7. Enhanced In Situ Chemical Oxidation Using Surfactants and Shear Thinning Fluids

    Science.gov (United States)

    Hauswirth, S.; Sadeghi, S.; Cerda, C. C.; Espinoza, I.; Schultz, P. B.; Miller, C. T.

    2017-12-01

    In situ chemical oxidation (ISCO) is an attractive approach for the remediation of recalcitrant contaminants, due to the fact that target compounds are degraded in place, precluding the need for ex situ treatment or disposal. However, field applications of ISCO approaches have been plagued by "rebound" of contaminant concentrations in groundwater weeks to months after treatment. The cause of rebound at a given site may vary, but is typically associated with back-diffusion from finer grained, low permeability units or the presence of non-aqueous phase liquids (NAPLs) that are incompletely degraded during treatment. Modifications to traditional ISCO methods have been proposed to overcome these challenges, including the use of shear-thinning polymers to improve delivery of oxidants to low permeability units and the addition of surfactants to improve dissolution of contaminants from NAPLs. In this work, we investigate the application of these approaches to the oxidation of manufactured gas plant (MGP) tars—NAPLs composed primarily of polycyclic aromatic hydrocarbons (PAHs). We conducted experiments to determine the mutual impact of each chemical component on the physical and chemical properties of the overall system. Specifically, experiments were designed to: determine the kinetics and overall effectiveness of contaminant-oxidant reactions for multiple oxidant-activator combinations; screen several common surfactants in terms of their ability to increase MGP tar solubility and their compatibility with oxidant systems; measure the impact of oxidants and surfactants on the rheology of several common polymer additives; and assess the effect of surfactants and polymers on the consumption of oxidants/activators and on the kinetics of contaminant-oxidant reactions. The results of this work provide insight into the chemical and physical mechanisms associated with enhanced ISCO approaches and an improved basis with which to model and design ISCO applications at both the lab

  8. Sinterability and conductivity of barium doped aluminium lanthanum oxyapatite La{sub 9.5}Ba{sub 0.5}Si{sub 5.5}Al{sub 0.5}O{sub 26.5} electrolyte of solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Cao Xiaoguo [Faculty of Materials and Energy, Guangdong University of Technology, Guangzhou 510006, Guangdong (China); Jiang Sanping, E-mail: s.jiang@curtin.edu.au [Fuels and Energy Technology Institute and Department of Chemical Engineering, Curtin University, Perth, WA 6102 (Australia)

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer Ba doping enhances the sintering and densification properties of aluminium lanthanum apatite. Black-Right-Pointing-Pointer Ba doping improves the oxide conductivity of aluminium lanthanum apatite. Black-Right-Pointing-Pointer The enhancement of Ba doping is mainly due to the significantly reduced grain boundary resistance of the aluminium lanthanum apatite. - Abstract: Apatite ceramics are interesting alternative solid oxide fuel cells (SOFCs) electrolytes because of their open structure for the transportation of oxide ions and their good chemical stability. This study reports the influence of barium doping on the microstructure, sinterability and oxide conductivity properties of the aluminium lanthanum oxyapatite La{sub 9.5}Ba{sub 0.5}Si{sub 5.5}Al{sub 0.5}O{sub 26.5}. SEM results show that lanthanum substitution with barium improves the sinterability of apatite ceramics. The barium doping also enhances the conductivity of the aluminium lanthanum silicates. The oxygen ion conductivity of La{sub 9.5}Ba{sub 0.5}Si{sub 5.5}Al{sub 0.5}O{sub 26.5} sintered at 1600 Degree-Sign C is 2.21 Multiplication-Sign 10{sup -2} S cm{sup -1} at 800 Degree-Sign C, higher than 9.81 Multiplication-Sign 10{sup -3} S cm{sup -1} of La{sub 10}Si{sub 5}AlO{sub 26.5} sample prepared under the same conditions. The results in the present study demonstrate that doping Ba on the La site for aluminium lanthanum oxyapatite reduces the sintering temperature and improves the ion conductivity. The enhancement of Ba dopant is mainly on the improvement of the densification and thus substantially reduced grain boundary resistance of aluminium lanthanum oxyapatite particularly at low temperatures.

  9. The state of permanganate with relation to in situ chemical oxidation

    International Nuclear Information System (INIS)

    Veronda, Brenda; Dingens, Matthew

    2007-01-01

    In Situ Chemical Oxidation (ISCO) with permanganate had its beginnings over 10 years ago. Since that time, many sites have been successfully treated for organic compounds including chlorinated ethenes (perchloroethylene, trichloroethylene, etc.) phenols, explosives such as RDX, and many other organics. The successful application of ISCO with permanganate requires the integration of many site-specific factors into the remedial design. ISCO with permanganate is an effective technology, not only for its oxidative properties and persistence, but also for its application flexibility to remediate soil and groundwater. The merits of any type of treatment technology can be assessed in terms of effectiveness, ease of use, reaction rate, and cost. The use of permanganate for in situ chemical oxidation results in the complete mineralization of TCE and PCE and can result in treatment levels below detection limits. Permanganate is a single component oxidizer, which is easily handled, mixed and distributed to the subsurface. Permanganate is also inexpensive to design and implement as compared to other technologies. This presentation will provide a general overview of the application and safety aspects of ISCO with permanganate. This paper will discuss the advantages and limitations of this technology, typical cost ranges, site evaluation and application technologies. (authors)

  10. In-Situ Growth and Characterization of Indium Tin Oxide Nanocrystal Rods

    Directory of Open Access Journals (Sweden)

    Yan Shen

    2017-11-01

    Full Text Available Indium tin oxide (ITO nanocrystal rods were synthesized in-situ by a vapor-liquid-solid (VLS method and electron beam evaporation technique. When the electron-beam gun bombarded indium oxide (In2O3 and tin oxide (SnO2 mixed sources, indium and tin droplets appeared and acted as catalysts. The nanocrystal rods were in-situ grown on the basis of the metal catalyst point. The nanorods have a single crystal structure. Its structure was confirmed by X-ray diffraction (XRD and transmission electron microscopy (TEM. The surface morphology was analyzed by scanning electron microscopy (SEM. During the evaporation, a chemical process was happened and an In2O3 and SnO2 solid solution was formed. The percentage of doped tin oxide was calculated by Vegard’s law to be 3.18%, which was in agreement with the mixture ratio of the experimental data. The single crystal rod had good semiconductor switch property and its threshold voltage of single rod was approximately 2.5 V which can be used as a micro switch device. The transmission rate of crystalline nanorods ITO film was over 90% in visible band and it was up to 95% in the blue green band as a result of the oxygen vacancy recombination luminescence.

  11. Special metallurgy - the electrical butt-welding by flashing of sintered magnesium-magnesium oxide composites (1963)

    International Nuclear Information System (INIS)

    Charleux, J.

    1963-01-01

    Electrical resistance welding has become quite important since World War II because of the need of a high yield in aeronautical production. Progress has been due in particular to the improvements made in electronically controlled apparatus making possible the automatic control of welding. For the butt-welding of sections requiring either a high production rate or a high quality weld, the flash butt-welding system has been very much developed these last few years. The use of this welding method is of great importance in the field of the bonding of oxidisable metals such as magnesium or aluminium and its alloys, because the welded joint is free from oxides. This study consists of general considerations on the flash-welding process with regard to temperature distribution in the parts during welding, and to electrical phenomena connected with flashing. Besides this general or theoretical section, we have applied the welding process to the bonding of sintered magnesium, a magnesium-magnesium oxide composite, whose use as a structural element in nuclear reactors is considered. (author) [fr

  12. SnO2*CoO ceramic obtained by microwave sintering

    International Nuclear Information System (INIS)

    Bordignon, M.A.N; Moura, F.; Zaghete, M.A.; Varela, J.A.; Perazolli, L.

    2009-01-01

    This work consists in the sintering study of CoO doped SnO 2 using microwave sintering oven and silicon carbide as a susceptor. The powders were obtained by dry oxides mixture and conformed in cylindrical shapes with 6mmx8mm and green density to 60%. Then the compacts were sintering up to 1.050 deg C, using heating rate of 50 deg C/min and isotherm up to 30min. The densities obtained were above 95% for both techniques. It was observed that occurred a temperature reducing of 400 deg C and time reducing of 210min to obtain the same densities, when was used the microwave oven without the phenomena of thermal runaway. So the sintered compacts were accomplished using DRX and SEM. It was made the electrical characterization (current x voltage) and it was found to have great potential in the production of dense ceramic-based SnO 2 with low resistivity to obtain electro-ceramic devices. (author)

  13. In situ chemical synthesis of ruthenium oxide/reduced graphene oxide nanocomposites for electrochemical capacitor applications.

    Science.gov (United States)

    Kim, Ji-Young; Kim, Kwang-Heon; Yoon, Seung-Beom; Kim, Hyun-Kyung; Park, Sang-Hoon; Kim, Kwang-Bum

    2013-08-07

    An in situ chemical synthesis approach has been developed to prepare ruthenium oxide/reduced graphene oxide (RGO) nanocomposites. It is found that as the C/O ratio increases, the number density of RuO2 nanoparticles decreases, because the chemical interaction between the Ru ions and the oxygen-containing functional groups provides anchoring sites where the nucleation of particles takes place. For electrochemical capacitor applications, the microwave-hydrothermal process was carried out to improve the conductivity of RGO in RuO2/RGO nanocomposites. The significant improvement in capacitance and high rate capability might result from the RuO2 nanoparticles used as spacers that make the interior layers of the reduced graphene oxide electrode available for electrolyte access.

  14. Effort to improve coupled in situ chemical oxidation with bioremediation: a review of optimization strategies

    NARCIS (Netherlands)

    Sutton, N.B.; Grotenhuis, J.T.C.; Langenhoff, A.A.M.; Rijnaarts, H.H.M.

    2011-01-01

    Purpose - In order to provide highly effective yet relatively inexpensive strategies for the remediation of recalcitrant organic contaminants, research has focused on in situ treatment technologies. Recent investigation has shown that coupling two common treatments-in situ chemical oxidation (ISCO)

  15. Effects of sintering temperature on the mechanical properties of sintered NdFeB permanent magnets prepared by spark plasma sintering

    International Nuclear Information System (INIS)

    Wang, G.P.; Liu, W.Q.; Huang, Y.L.; Ma, S.C.; Zhong, Z.C.

    2014-01-01

    Sintered NdFeB-based permanent magnets were fabricated by spark plasma sintering (SPS) and a conventional method to investigate the mechanical and magnetic properties. The experimental results showed that sintered NdFeB magnet prepared by the spark plasma sintering (SPS NdFeB) possesses a better mechanical properties compared to the conventionally sintered one, of which the maximum value of bending strength and Vickers hardness was 402.3 MPa and 778.1 MPa, respectively. The effects of sintering temperature on bending strength and Vickers hardness were investigated. It was shown that the bending strength firstly increases to the maximum value and then decreases with the increase of sintering temperature in a certain range. The investigations of microstructures and mechanical properties indicated that the unique sintering mechanism in the SPS process is responsible for the improvement of mechanical properties of SPS NdFeB. Furthermore, the relations between the mechanical properties and relevant microstructure have been analyzed based on the experimental fact. - Highlights: • Studied the sintering temperature effect on strengthening mechanism of NdFeB magnet firstly. • It showed that sintering temperature may effectively affect the mechanical properties. • The maximum bending strength and Vickers hardness was 402.3 MPa and 778.1 MPa, respectively

  16. Effects of sintering temperature on the mechanical properties of sintered NdFeB permanent magnets prepared by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Wang, G.P., E-mail: wgp@jxnu.edu.cn [College of Physics and Communication Electronics, Jiangxi Normal University, Nanchang 330022 (China); Liu, W.Q. [Key Laboratory of Advanced Functional Materials Science and Engineering, Ministry of Education, Beijing University of Technology, Beijing 100022 (China); Huang, Y.L.; Ma, S.C.; Zhong, Z.C. [School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063 (China)

    2014-01-15

    Sintered NdFeB-based permanent magnets were fabricated by spark plasma sintering (SPS) and a conventional method to investigate the mechanical and magnetic properties. The experimental results showed that sintered NdFeB magnet prepared by the spark plasma sintering (SPS NdFeB) possesses a better mechanical properties compared to the conventionally sintered one, of which the maximum value of bending strength and Vickers hardness was 402.3 MPa and 778.1 MPa, respectively. The effects of sintering temperature on bending strength and Vickers hardness were investigated. It was shown that the bending strength firstly increases to the maximum value and then decreases with the increase of sintering temperature in a certain range. The investigations of microstructures and mechanical properties indicated that the unique sintering mechanism in the SPS process is responsible for the improvement of mechanical properties of SPS NdFeB. Furthermore, the relations between the mechanical properties and relevant microstructure have been analyzed based on the experimental fact. - Highlights: • Studied the sintering temperature effect on strengthening mechanism of NdFeB magnet firstly. • It showed that sintering temperature may effectively affect the mechanical properties. • The maximum bending strength and Vickers hardness was 402.3 MPa and 778.1 MPa, respectively.

  17. Lanthana-bearing nanostructured ferritic steels via spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Pasebani, Somayeh [Department of Chemical and Materials Engineering, University of Idaho, Moscow, ID 83844 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States); Charit, Indrajit, E-mail: icharit@uidaho.edu [Department of Chemical and Materials Engineering, University of Idaho, Moscow, ID 83844 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States); Wu, Yaqiao; Burns, Jatuporn; Allahar, Kerry N.; Butt, Darryl P. [Department of Materials Science and Engineering, Boise State University, Boise, ID 83725 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States); Cole, James I. [Idaho National Laboratory, Idaho Falls, ID 83401 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States); Alsagabi, Sultan F. [Department of Chemical and Materials Engineering, University of Idaho, Moscow, ID 83844 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States)

    2016-03-15

    A lanthana-containing nanostructured ferritic steel (NFS) was processed via mechanical alloying (MA) of Fe-14Cr-1Ti-0.3Mo-0.5La{sub 2}O{sub 3} (wt.%) and consolidated via spark plasma sintering (SPS). In order to study the consolidation behavior via SPS, sintering temperature and dwell time were correlated with microstructure, density, microhardness and shear yield strength of the sintered specimens. A bimodal grain size distribution including both micron-sized and nano-sized grains was observed in the microstructure of specimens sintered at 850, 950 and1050 °C for 45 min. Significant densification occurred at temperatures greater than 950 °C with a relative density higher than 98%. A variety of nanoparticles, some enriched in Fe and Cr oxides and copious nanoparticles smaller than 10 nm with faceted morphology and enriched in La and Ti oxides were observed. After SPS at 950 °C, the number density of Cr–Ti–La–O-enriched nanoclusters with an average radius of 1.5 nm was estimated to be 1.2 × 10{sup 24} m{sup −3}. The La + Ti:O ratio was close to 1 after SPS at 950 and 1050 °C; however, the number density of nanoclusters decreased at 1050 °C. With SPS above 950 °C, the density improved but the microhardness and shear yield strength decreased due to partial coarsening of the grains and nanoparticles.

  18. Thulium oxide fuel characterization study: Part 3, Procedures

    International Nuclear Information System (INIS)

    Nelson, C.A.; Anderson, R.W.; Talbot, M.; Bierds, W.

    1970-06-01

    Procedures are presented for the following: Tm 2 O 3 -Yb 2 O 3 pseudo - binary phase diagram tests; compatibility tests; thulium-170 oxide dose rate measurements; preparation of Tm 2 O 3 wafers; SRL thulium and/or ytterbium oxide powder reprocessing for sintering; cold pressing and sintering thulium oxide wafers; preparation of thulium and/or ytterbium oxide powder via precipitation with oxalic acid, ammonium oxalate, urea and methyl oxalate; determination of the total surface area of rare earth oxide powders; determining oxygen in thulia - thulia/ytterbia for the purpose of determining metal-to-oxygen ratios; and determination of the impact resistance to fines generation of sintered rare earth oxide

  19. Laser Surface Treatment of Sintered Alumina

    Science.gov (United States)

    Hagemann, R.; Noelke, C.; Kaierle, S.; Wesling, V.

    Sintered alumina ceramics are used as refractory materials for industrial aluminum furnaces. In this environment the ceramic surface is in permanent contact with molten aluminum resulting in deposition of oxidic material on its surface. Consequently, a lower volume capacity as well as thermal efficiency of the furnaces follows. To reduce oxidic adherence of the ceramic material, two laser-based surface treatment processes were investigated: a powder- based single-step laser cladding and a laser surface remelting. Main objective is to achieve an improved surface quality of the ceramic material considering the industrial requirements as a high process speed.

  20. Evidence against the nuclear in situ binding of arsenicals-oxidative stress theory of arsenic carcinogenesis

    International Nuclear Information System (INIS)

    Kitchin, Kirk T.; Wallace, Kathleen

    2008-01-01

    A large amount of evidence suggests that arsenicals act via oxidative stress in causing cancer in humans and experimental animals. It is possible that arsenicals could bind in situ close to nuclear DNA followed by Haber-Weiss type oxidative DNA damage. Therefore, we tested this hypothesis by using radioactive 73 As labeled arsenite and vacuum filtration methodology to determine the binding affinity and capacity of 73 As arsenite to calf thymus DNA and Type 2A unfractionated histones, histone H3, H4 and horse spleen ferritin. Arsenicals are known to release redox active Fe from ferritin. At concentrations up to about 1 mM, neither DNA nor any of the three proteins studied, Type II-A histones, histone H3, H4 or ferritin, bound radioactive arsenite in a specific manner. Therefore, it appears highly unlikely that initial in situ binding of trivalent arsenicals, followed by in situ oxidative DNA damage, can account for arsenic's carcinogenicity. This experimental evidence (lack of arsenite binding to DNA, histone Type II-A and histone H3, H4) does not rule out other possible oxidative stress modes of action for arsenic such as (a) diffusion of longer lived oxidative stress molecules, such as H 2 O 2 into the nucleus and ensuing oxidative damage, (b) redox chemistry by unbound arsenicals in the nucleus, or (c) arsenical-induced perturbations in Fe, Cu or other metals which are already known to oxidize DNA in vitro and in vivo

  1. Ex-Situ and In-Situ Ellipsometric Studies of the Thermal Oxide on InP

    Science.gov (United States)

    1990-12-06

    ion---- Distribution/ Availabilit ? Codes£v l llt Codes Avail and/or Dist| Special Abstract The thermally grown InP oxide as etched by an aqueous...aqueous NH4OH/NH4F, and Law(17) has reported observations of orientational ordering of water and organic solvents on pyrex surfaces by in-situ...minutes, followed by a sequence of acetone, deionized water (d. i. water ) rinse. After being dipped in a concentrated aqueous HF solution for 15 seconds

  2. In-situ electrochemical impedance spectroscopy measurements of zirconium alloy oxide conductivity: Relationship to hydrogen pickup

    International Nuclear Information System (INIS)

    Couet, Adrien; Motta, Arthur T.; Ambard, Antoine; Livigni, Didier

    2017-01-01

    Highlights: • In-situ electrochemistry on zirconium alloys in 360 °C pure water show oxide layer resistivity changes during corrosion. • A linear relationship is observed between oxide resistivity and instantaneous hydrogen pickup fraction. • The resistivity of the oxide layer formed on Zircaloy-4 (and thus its hydrogen pickup fraction) is higher than on Zr-2.5Nb. - Abstract: Hydrogen pickup during nuclear fuel cladding corrosion is a critical life-limiting degradation mechanism for nuclear fuel. Following a program dedicated to zirconium alloys, corrosion, it has been hypothesized that oxide electronic resistivity determines hydrogen pickup. In-situ electrochemical impedance spectroscopy experiments were performed on Zircaloy-4 and Zr-2.5Nb alloys in 360 °C water. The oxide resistivity was measured as function of time. The results show that as the oxide resistivity increases so does the hydrogen pickup fraction. The resistivity of the oxide layer formed on Zircaloy-4 is higher than on Zr-2.5Nb, resulting in a higher hydrogen pickup fraction of Zircaloy-4, compared to Zr-2.5Nb.

  3. Optimization of the sintering atmosphere for high-density hydroxyapatite–carbon nanotube composites

    Science.gov (United States)

    White, Ashley A.; Kinloch, Ian A.; Windle, Alan H.; Best, Serena M.

    2010-01-01

    Hydroxyapatite–carbon nanotube (HA–CNT) composites have the potential for improved mechanical properties over HA for use in bone graft applications. Finding an appropriate sintering atmosphere for this composite presents a dilemma, as HA requires water in the sintering atmosphere to remain phase pure and well hydroxylated, yet CNTs oxidize at the high temperatures required for sintering. The purpose of this study was to optimize the atmosphere for sintering these composites. While the reaction between carbon and water to form carbon monoxide and hydrogen at high temperatures (known as the ‘water–gas reaction’) would seem to present a problem for sintering these composites, Le Chatelier's principle suggests this reaction can be suppressed by increasing the concentration of carbon monoxide and hydrogen relative to the concentration of carbon and water, so as to retain the CNTs and keep the HA's structure intact. Eight sintering atmospheres were investigated, including standard atmospheres (such as air and wet Ar), as well as atmospheres based on the water–gas reaction. It was found that sintering in an atmosphere of carbon monoxide and hydrogen, with a small amount of water added, resulted in an optimal combination of phase purity, hydroxylation, CNT retention and density. PMID:20573629

  4. Shape distortion and thermo-mechanical properties of dense SOFC components from green tape to sintered body

    DEFF Research Database (Denmark)

    Teocoli, Francesca; Esposito, Vincenzo; Ni, De Wei

    stresses, which develop a camber in the final sintered body. To analyze the phenomena, shrinkage of SOFC components single layers and camber development of bi-layers were measured in-situ by optical dilatometry. In addition, a thoughtful investigation of the viscoelastic properties of individual layers......Sintering of ceramic materials is a critical process, especially when the components are shaped as multilayer. Microstructural changes and stresses take place in ceramics as single layer from the green stage to the densification stage, leading to shape distortion, delamination and cracks...

  5. Superior sinterability of nano-crystalline gadolinium doped ceria powders synthesized by co-precipitation method

    International Nuclear Information System (INIS)

    Hari Prasad, D.; Kim, H.-R.; Park, J.-S.; Son, J.-W.; Kim, B.-K.; Lee, H.-W.; Lee, J.-H.

    2010-01-01

    Reduced sintering temperature of doped ceria can greatly simplify the fabrication process of solid oxide fuel cells (SOFCs) by utilizing the co-firing of all cell components with a single step. In the present study, nano-crystalline gadolinium doped ceria (GDC) powders of high sinterability at lower sintering temperature has been synthesized by co-precipitation at room temperature. The successful synthesis of nano-crystalline GDC was confirmed by XRD, TEM and Raman spectroscopy analysis. Dilatometry studies showed that GDC prepared by this method can be fully densified (97% relative density) at a sintering temperature of 950 o C which is fairly lower than ever before. It has also been found that the sintered samples have a higher ionic conductivity of 1.64 x 10 -2 S cm -1 at 600 o C which is suitable for the intermediate temperature SOFC application.

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

    Directory of Open Access Journals (Sweden)

    Kétner Bendo Demétrio

    2013-01-01

    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.

  7. In situ Oxidation of Ultrathin Silver Films on Ni(111)

    International Nuclear Information System (INIS)

    Meyer, A.; Flege, I.; Senanayake, S.; Kaemena, B.; Rettew, R.; Alamgir, F.; Falta, J.

    2011-01-01

    Oxidation of silver films of one- and two-monolayer thicknesses on the Ni(111) surface was investigated by low-energy electron microscopy at temperatures of 500 and 600 K. Additionally, intensity-voltage curves were measured in situ during oxidation to reveal the local film structure on a nanometer scale. At both temperatures, we find that exposure to molecular oxygen leads to the destabilization of the Ag film with subsequent relocation of the silver atoms to small few-layer-thick silver patches and concurrent evolution of NiO(111) regions. Subsequent exposure of the oxidized surface to ethylene initiates the transformation of bilayer islands back into monolayer islands, demonstrating at least partial reversibility of the silver relocation process at 600 K.

  8. Sintering and annealing effects on undoped yttria transparent ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Letue, Laetitia; Petit, Johan, E-mail: johan.petit@onera.fr; Ritti, Marie-Hélène; Lalanne, Sylvie; Landais, Stéphane

    2017-06-15

    Transparent yttrium oxide (Y{sub 2}O{sub 3}) ceramics were processed by several densifications steps without any doping species. The green bodies were obtained by the aqueous way and sintered at high temperature under vacuum and then under high pressure. We studied the effects of different sintering cycles and air annealing at different steps of the process on the density and the grain growth. We also focused on the reaction between yttria ceramics and BN-coated graphite crucible which occurs during HIP. We noted that a low heating rate and two annealing steps are necessary to improve our samples’ transparency. - Highlights: • The quality of transparent ceramics is compared with the tested process parameters. • Air annealing is critical when using a carbon environment in the process. • Intra-granular pores, and so the final transparency, are directly linked to the sintering heating rates.

  9. Gaining electricity from in situ oxidation of hydrogen produced by fermentative cellulose degradation.

    Science.gov (United States)

    Niessen, J; Schröder, U; Harnisch, F; Scholz, F

    2005-01-01

    To exploit the fermentative hydrogen generation and direct hydrogen oxidation for the generation of electric current from the degradation of cellulose. Utilizing the metabolic activity of the mesophilic anaerobe Clostridium cellulolyticum and the thermophilic Clostridium thermocellum we show that electricity generation is possible from cellulose fermentation. The current generation is based on an in situ oxidation of microbially synthesized hydrogen at platinum-poly(tetrafluoroaniline) (Pt-PTFA) composite electrodes. Current densities of 130 mA l(-1) (with 3 g cellulose per litre medium) were achieved in poised potential experiments under batch and semi-batch conditions. The presented results show that electricity generation is possible by the in situ oxidation of hydrogen, product of the anaerobic degradation of cellulose by cellulolytic bacteria. For the first time, it is shown that an insoluble complex carbohydrate like cellulose can be used for electricity generation in a microbial fuel cell. The concept represents a first step to the utilization of macromolecular biomass components for microbial electricity generation.

  10. Sintering of nonstoichiometric UO2

    International Nuclear Information System (INIS)

    Susnik, D.; Holc, J.

    1983-01-01

    Activated sintering of UO 2 pellets at 1100 deg C is described. In CO 2 atmosphere is UO 2 is nonstoichiometric and pellets from active UO 2 powders sinter at 900 deg C to high density. At 1100 deg C the final sintered density is practically achieved at heating on sintering temperature. After reduction and cooling in H 2 atmosphere which is followed sintering in CO 2 the structure is identical to the structured UO 2 pellets sintered at high temperature in H 2 . Density of activated sintered UO 2 pellets is stable, even after additional sintering at 1800 deg C. (author)

  11. Titanium Powder Sintering in a Graphite Furnace and Mechanical Properties of Sintered Parts

    Directory of Open Access Journals (Sweden)

    Changzhou Yu

    2017-02-01

    Full Text Available Recent accreditation of titanium powder products for commercial aircraft applications marks a milestone in titanium powder metallurgy. Currently, powder metallurgical titanium production primarily relies on vacuum sintering. This work reported on the feasibility of powder sintering in a non-vacuum furnace and the tensile properties of the as-sintered Ti. Specifically, we investigated atmospheric sintering of commercially pure (C.P. titanium in a graphite furnace backfilled with argon and studied the effects of common contaminants (C, O, N on sintering densification of titanium. It is found that on the surface of the as-sintered titanium, a severely contaminated porous scale was formed and identified as titanium oxycarbonitride. Despite the porous surface, the sintered density in the sample interiors increased with increasing sintering temperature and holding time. Tensile specimens cut from different positions within a large sintered cylinder reveal different tensile properties, strongly dependent on the impurity level mainly carbon and oxygen. Depending on where the specimen is taken from the sintered compact, ultimate tensile strength varied from 300 to 580 MPa. An average tensile elongation of 5% to 7% was observed. Largely depending on the interstitial contents, the fracture modes from typical brittle intergranular fracture to typical ductile fracture.

  12. Cr2O3-doped MOX fuel: doping and sintering atmosphere optimization

    International Nuclear Information System (INIS)

    Thomas, R.

    2013-01-01

    Optimal use of the Mixed Oxide (U,Pu)O 2 nuclear fuel in pressurized water reactors is mainly limited by the behavior of gaseous fission produced during irradiation. Within the MOX microstructure, the probability of fission gas release is increased by the presence of rich localized plutonium areas exhibiting a higher local burn-up. A solution consists in optimizing plutonium distribution within the industrial product and promoting the crystalline growth of the fuel grains. For this purpose, addition of chromium sesquioxide during the manufacturing process is currently considered. A previous thesis has shown that the best results are obtained for a Cr addition slightly greater than the solubility limit of Cr in (U,Pu)O 2 . In order to explain the enhanced plutonium homogeneity, the author highlighted the formation of PuCrO 3 precipitates at grain boundaries. A sintering model under reducing atmosphere, with chromium addition, was proposed. However, several points have to be more thoroughly investigated, especially regarding the solubility limit of chromium, as well as the optimal conditions of PuCrO 3 precipitates formation. In a first part, speciation of solubilized and precipitated chromium in the mixed oxide (U,Pu)O 2 is studied using electron probe microanalysis (EPMA) and X-ray absorption spectroscopy (XAS). It was shown that the oxidation state and the environment of soluble chromium within the (U,Pu)O 2 matrix do not depend on the oxygen partial pressure during sintering, neither on the plutonium content of the mixed oxide. However, both chemical nature of the precipitates and chromium solubility depend on the thermodynamic variable and on the plutonium content.Based on these results, a chromium solubility model in the mixed oxide (U,Pu)O 2-x was built using the law of mass action governing solubility equilibrium. This model is described as a function of the plutonium content (y) of the solid solution (U 1-y Pu y )O 2-x (y = 0,11; 0,275 et 1) and in the

  13. Preparation and sintering of Zr(C,N,O) phases

    International Nuclear Information System (INIS)

    Tamborenea, S.; Mazzoni, A.D.; Aglietti, E.F.

    2003-01-01

    The Zr(C,O,N) compounds form a great mono-phase zone belonging to the pseudoternary ZrO-ZrN-ZrC system.Theses phases have cubic crystalline structure with a o parameter depending on the C, O 2 and N 2 content.These phases have many potential applications in the manufacture of ceramic pieces utilizable as electronic conductors.The Zr (C,O,N) phases can be obtained from ZrO 2 by carbonitriding reactions: that is carbothermal reduction and simultaneous nitriding.In this work a series of experiences of carbonitriding of zirconia under different conditions (temperatures between 1400 and 1600degC, times of 120 min, carbon content between 20 and 40%) in order to obtain suitable powders to be sintered.The XRD analysis shows the Zr(C,O,N) as the main products and β -ZrON as the only secondary product in proportions depending on the obtaining conditions.The variables employed were the C content and the reaction temperature.The Zr(C,O,N) content varies between 40 and 90% and tends to increase with the temperature and the carbon content whereas the β -ZrON phase varies between the 40 and 10 % decreasing its proportion with temperature and the carbon content.The oxidation resistance of these phases was studied by DTA-TG tests in air.Results show complete oxidation reaction at ∼500degC in air.The sintering of these materials was made on disks obtained by pressing of powders of Zr(C,N,O) contents higher than 90%.Sintering was performed in nitrogen atmosphere and temperatures between 1450 and 1620degC.Disks were characterized by pycnometry and Hg volumeter.The densities obtained were between 5 and 6,6g/cm 3 with a tendency to increase with the Zr(C,N,O) phase content, the temperature and the sintering time.Sintered disks were characterized by dilatometry in N 2

  14. Transparent Lu 2 O 3 :Eu ceramics by sinter and HIP optimization

    Science.gov (United States)

    Seeley, Z. M.; Kuntz, J. D.; Cherepy, N. J.; Payne, S. A.

    2011-09-01

    Evolution of porosity and microstructure was observed during densification of lutetium oxide ceramics doped with europium (Lu 2O 3:Eu) fabricated via vacuum sintering and hot isostatic pressing (HIP'ing). Nano-scale starting powder was uniaxially pressed and sintered under high vacuum at temperatures between 1575 and 1850 °C to obtain densities ranging between 94% and 99%, respectively. Sintered compacts were then subjected to 200 MPa argon gas at 1850 °C to reach full density. Vacuum sintering above 1650 °C led to rapid grain growth prior to densification, rendering the pores immobile. Sintering between 1600 and 1650 °C resulted in closed porosity yet a fine grain size to allow the pores to remain mobile during the subsequent HIP'ing step, resulting in a fully-dense highly transparent ceramic without the need for subsequent air anneal. Light yield performance was measured and Lu 2O 3:Eu showed ˜4 times higher light yield than commercially used scintillating glass indicating that this material has the potential to improve the performance of high energy radiography devices.

  15. The Influence of Sintering Temperature of Reactive Sintered (Ti, MoC-Ni Cermets

    Directory of Open Access Journals (Sweden)

    Marek Jõeleht

    2015-09-01

    Full Text Available Titanium-molybdenum carbide nickel cermets ((Ti, MoC-Ni were produced using high energy milling and reactive sintering process. Compared to conventional TiC-NiMo cermet sintering the parameters for reactive sintered cermets vary since additional processes are present such as carbide synthesis. Therefore, it is essential to acquire information about the suitable sintering regime for reactive sintered cermets. One of the key parameters is the final sintering temperature when the liquid binder Ni forms the final matrix and vacancies inside the material are removed. The influence of the final sintering temperature is analyzed by scanning electron microscopy. Mechanical properties of the material are characterized by transverse rupture strength, hardness and fracture toughness.DOI: http://dx.doi.org/10.5755/j01.ms.21.3.7179

  16. Evaluation of dilatometric techniques for studies of sintering kinetics

    International Nuclear Information System (INIS)

    El-Sayed Ali, M.; Toft Soerensen, O.

    1985-04-01

    The kinetics of the initial sintering stage of CeO 2 is evaluated by three different techniques: constant heating rate dilatometry, constant shrinkage rate dilatometry and a new technique recently introduced by the authors called Stepwise Isothermal Dilatometry (SID). Comparative measurements with these techniques showed that too high activation energies were obtained with the two first techniques, both of which can be termed as nonisothermal, whereas activation energies comparable to those reported for cation diffusion in other fluorite oxides were obtained with the latter technique. Of the three techniques SID is thus considered to be the most accurate for studies of the sintering kinetics. In contrast to the two nonisothermal techniques SID has the further advantage that both the controlling mechanism and its activation energy can be determined in a single experiment. From the SID-measurement it was concluded that the initial sintering stage of CeO 2 is controlled by grain-boundary diffusion. (author)

  17. Stability study of cermet-supported solid oxide fuel cells with bi-layered electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xinge; Gazzarri, Javier; Robertson, Mark; Deces-Petit, Cyrille [National Research Council, Institute for Fuel Cell Innovation, 4250 Wesbrook Mall, Vancouver, BC (Canada); Kesler, Olivera [Department of Mechanical and Industrial Engineering, University of Toronto, 5 King' s College Road, Toronto, ON (Canada)

    2008-12-01

    Performance and stability of five cermet-supported button-type solid oxide fuel cells featuring a bi-layered electrolyte (SSZ/SDC), an SSC cathode, and a Ni-SSZ anode, were analyzed using polarization curves, impedance spectroscopy, and post-mortem SEM observation. The cell performance degradation at 650 C in H{sub 2}/air both with and without DC bias conditions was manifested primarily as an increase in polarization resistance, approximately at a rate of 2.3 m{omega} cm{sup 2} h{sup -1} at OCV, suggesting a decrease in electrochemical kinetics as the main phenomenon responsible for the performance decay. In addition, the initial series resistance was about ten times higher than the calculated resistance corresponding to the electrolyte, reflecting a possible inter-reaction between the electrolyte layers that occurred during the sintering stage. In situ and ex situ sintered cathodes showed no obvious difference in cell performance or decay rate. The stability of the cells with and without electrical load was also investigated and no significant influence of DC bias was recorded. Based on the experimental results presented, we preliminarily attribute the performance degradation to electrochemical and microstructural degradation of the cathode. (author)

  18. Stability study of cermet-supported solid oxide fuel cells with bi-layered electrolyte

    Science.gov (United States)

    Zhang, Xinge; Gazzarri, Javier; Robertson, Mark; Decès-Petit, Cyrille; Kesler, Olivera

    Performance and stability of five cermet-supported button-type solid oxide fuel cells featuring a bi-layered electrolyte (SSZ/SDC), an SSC cathode, and a Ni-SSZ anode, were analyzed using polarization curves, impedance spectroscopy, and post-mortem SEM observation. The cell performance degradation at 650 °C in H 2/air both with and without DC bias conditions was manifested primarily as an increase in polarization resistance, approximately at a rate of 2.3 mΩ cm 2 h -1 at OCV, suggesting a decrease in electrochemical kinetics as the main phenomenon responsible for the performance decay. In addition, the initial series resistance was about ten times higher than the calculated resistance corresponding to the electrolyte, reflecting a possible inter-reaction between the electrolyte layers that occurred during the sintering stage. In situ and ex situ sintered cathodes showed no obvious difference in cell performance or decay rate. The stability of the cells with and without electrical load was also investigated and no significant influence of DC bias was recorded. Based on the experimental results presented, we preliminarily attribute the performance degradation to electrochemical and microstructural degradation of the cathode.

  19. Computer Modeling of Direct Metal Laser Sintering

    Science.gov (United States)

    Cross, Matthew

    2014-01-01

    A computational approach to modeling direct metal laser sintering (DMLS) additive manufacturing process is presented. The primary application of the model is for determining the temperature history of parts fabricated using DMLS to evaluate residual stresses found in finished pieces and to assess manufacturing process strategies to reduce part slumping. The model utilizes MSC SINDA as a heat transfer solver with imbedded FORTRAN computer code to direct laser motion, apply laser heating as a boundary condition, and simulate the addition of metal powder layers during part fabrication. Model results are compared to available data collected during in situ DMLS part manufacture.

  20. In situ growth of capping-free magnetic iron oxide nanoparticles on liquid-phase exfoliated graphene

    NARCIS (Netherlands)

    Tsoufis, T.; Syrgiannis, Z.; Akhtar, N.; Prato, M.; Katsaros, F.; Sideratou, Z.; Kouloumpis, A.; Gournis, D.; Rudolf, P.

    2015-01-01

    We report a facile approach for the in situ synthesis of very small iron oxide nanoparticles on the surface of high-quality graphene sheets. Our synthetic strategy involved the direct, liquid-phase exfoliation of highly crystalline graphite (avoiding any oxidation treatment) and the subsequent

  1. Oxidation kinetics of Si and SiGe by dry rapid thermal oxidation, in-situ steam generation oxidation and dry furnace oxidation

    Science.gov (United States)

    Rozé, Fabien; Gourhant, Olivier; Blanquet, Elisabeth; Bertin, François; Juhel, Marc; Abbate, Francesco; Pribat, Clément; Duru, Romain

    2017-06-01

    The fabrication of ultrathin compressively strained SiGe-On-Insulator layers by the condensation technique is likely a key milestone towards low-power and high performances FD-SOI logic devices. However, the SiGe condensation technique still requires challenges to be solved for an optimized use in an industrial environment. SiGe oxidation kinetics, upon which the condensation technique is founded, has still not reached a consensus in spite of various studies which gave insights into the matter. This paper aims to bridge the gaps between these studies by covering various oxidation processes relevant to today's technological needs with a new and quantitative analysis methodology. We thus address oxidation kinetics of SiGe with three Ge concentrations (0%, 10%, and 30%) by means of dry rapid thermal oxidation, in-situ steam generation oxidation, and dry furnace oxidation. Oxide thicknesses in the 50 Å to 150 Å range grown with oxidation temperatures between 850 and 1100 °C were targeted. The present work shows first that for all investigated processes, oxidation follows a parabolic regime even for thin oxides, which indicates a diffusion-limited oxidation regime. We also observe that, for all investigated processes, the SiGe oxidation rate is systematically higher than that of Si. The amplitude of the variation of oxidation kinetics of SiGe with respect to Si is found to be strongly dependent on the process type. Second, a new quantitative analysis methodology of oxidation kinetics is introduced. This methodology allows us to highlight the dependence of oxidation kinetics on the Ge concentration at the oxidation interface, which is modulated by the pile-up mechanism. Our results show that the oxidation rate increases with the Ge concentration at the oxidation interface.

  2. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    International Nuclear Information System (INIS)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2016-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  3. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

    2016-08-15

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  4. Quantification of the effect of in-situ generated uranium metal on the experimentally determined O/U ratio of a sintered uranium dioxide fuel pellet

    International Nuclear Information System (INIS)

    Narasimha Murty, B.; Bharati Misra, U.; Yadav, R.B.; Srivastava, R.K.

    2005-01-01

    This paper describes quantitatively the effect of in-situ generated uranium metal (that could be formed due to the conducive manufacturing conditions) in a sintered uranium dioxide fuel pellet on the experimentally determined O/U ratio using analytical methods involving dissolution of the pellet material. To quantify the effect of in-situ generated uranium metal in the fuel pellet, a mathematical expression is derived for the actual O/U ratio in terms of the O/U ratio as determined by an experiment involving dissolution of the material and the quantity of uranium metal present in the uranium dioxide pellet. The utility of this derived mathematical expression is demonstrated by tabulating the calculated actual O/U ratios for varying amounts of uranium metal (from 5 to 95% in 5% intervals) and different O/U ratio values (from 2.001 to 2.015 in 0.001 intervals). This paper brings out the necessity of care to be exercised while interpreting the experimentally determined O/U ratio and emphasizes the fact that it is always safer to produce the nuclear fuel with oxygen to uranium ratios well below the specified maximum limit of 2.015. (author)

  5. In situ reduction of as-prepared γ-Iron Oxide Nanoparticles

    DEFF Research Database (Denmark)

    Garbus, Pelle Gorm; Ahlburg, Jakob; Christensen, Mogens

    -ray diffraction measurement. The as-prepared maghemite nanoparticles were synthesized by the continuous decomposition of solutes in supercritical hydrothermal flow synthesis [3, 4]. The reagent used was ferric ammonium citrate (C6H8O7•xFe(III)•yNH3) that under hydrothermal flow synthesis decomposes into the γ......-iron oxide Fe2O3. The reduction of maghemite to body centered cubic (BCC) iron does not go through a detectable intermediate state.1.Jensen, K.M., et al., Mechanisms for iron oxide formation under hydrothermal conditions: an in situ total scattering study. ACS nano, 2014. 8(10): p. 10704-10714.2.Andersen, H...

  6. Manufacture of nano graphite oxides derived from aqueous glucose solutions and in-situ synthesis of magnetite–graphite oxide composites

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xiang, E-mail: liuxiang@ahut.edu.cn; Zhao, Tiantian; Liu, Pengpeng; Cui, Ping, E-mail: cokecp@sohu.com; Hu, Peng

    2015-03-01

    A “bottom up” approach of manufacturing graphite oxides (GOs) derived from aqueous glucose solutions by virtue of an environmentally-friendly process and the way of in-situ synthesizing magnetite–GOs composites are described in this work in detail. The dehydrations among glucose molecules under hydrothermal condition result in the initial carbon quantum dots and ultimate GOs. The structural information of the GOs is obtained by the infrared, ultraviolet–visible and X-ray photoelectron spectra. The magnetite–GOs composites were obtained by a one-pot method under the same hydrothermal conditions as the one of preparing GOs. The composites perform high activities in catalytic degradation of Rhodamine B in the presence of hydrogen peroxides without extra heating or pH adjusting. Both the GOs and the magnetite–GOs composites are also assured by measurements of transmission electron microscope and X-ray powder diffraction. - Highlights: • Graphite oxides are made from aqueous glucose solutions by hydrothermal reaction. • A way of in-situ synthesizing composites of magnetite–graphite oxides is depicted. • The composites perform high activities in catalytic degradation of Rhodamine B.

  7. Characterization of subcritical water oxidation with in situ monitoring and self-modeling curve resolution

    International Nuclear Information System (INIS)

    Gemperline, Paul J.; Yang Yu; Bian Zhihui

    2003-01-01

    In this paper, a subcritical water oxidation (SBWO) process was monitored using self-modeling curve resolution (SMCR) of in situ UV-Vis measurements to estimate time-dependant composition profiles of reactants, intermediates and products. A small laboratory scale reactor with UV-Vis fiber-optic probes and a flow cell was used to demonstrate the usefulness of SMCR for monitoring the destruction of model compounds phenol, benzoic acid, and aniline in a dilute aqueous solutions. Hydrogen peroxide was used as the oxidizing reagent at moderate temperature (150-250 deg. C) and pressure (60-90 atm) in a single phase. By use of in situ monitoring, reaction times were easily determined and conditions for efficient oxidations were easily diagnosed without the need for time consuming off-line reference measurements. For selected runs, the destruction of the model compound was confirmed by gas chromatography and chemical oxygen demand (COD) measurements. Suspected intermediate oxidation products were easily detected by the use of UV-Vis spectrometry and self-modeling curve resolution, but could not be detected by gas chromatography

  8. Low-temperature sintering and electrical properties of strontium- and magnesium-doped lanthanum gallate with V2O5 additive

    Science.gov (United States)

    Ha, Sang Bu; Cho, Yoon Ho; Ji, Ho-Il; Lee, Jong-Ho; Kang, Yun Chan; Lee, Jong-Heun

    2011-03-01

    The effects of a V2O5 additive on the low-temperature sintering and ionic conductivity of strontium- and magnesium-doped lanthanum gallate (LSGM: La0.8Sr0.2Ga0.8Mg0.2O2.8) are studied. The LSGM powders prepared by the glycine nitrate method are mixed with 0.5-2 at.% of VO5/2 and then sintered at 1100-1400 °C in air for 4 h. The apparent density and phase purity of the LSGM specimens are increased with increasing sintering temperature and VO5/2 concentration due to the enhanced sintering and mass transfer via the intergranular liquid phase. The 1 at.% VO5/2-doped LSGM specimen sintered at 1300 °C exhibits a high oxide ion conductivity of ∼0.027 S cm-1 at 700 °C over a wide range of oxygen partial pressure (PO2 =10-27 - 1 atm), thereby demonstrating its potential as a useful electrolyte for anode-supported solid oxide fuel cells (SOFCs) without the requirement for any buffer layer between the electrolyte and anode.

  9. Evaluation of growth of calcium phosphate ceramics on sintered Ti-Ca-P composites

    Energy Technology Data Exchange (ETDEWEB)

    Karanjai, Malobika [Centre for Nano Materials, International Advanced Research Centre for Powder Metallurgy and New Materials, Balapur P.O, Hyderabad - 500 005, Andhra Pradesh (India)], E-mail: malobika_k@rediffmail.com; Sundaresan, Ranganathan [Centre for Nano Materials, International Advanced Research Centre for Powder Metallurgy and New Materials, Balapur P.O, Hyderabad - 500 005, Andhra Pradesh (India); Mohan, Tallapragada Raja Rama; Kashyap, Bhagwati Prasad [Department of Metallurgical Engineering and Materials Science, Indian Institute of Technology Bombay, Mumbai - 400 076, Maharashtra (India)

    2008-12-01

    Sintered Ti-Ca-P composites having in situ formed calcium phosphate phases developed by powder metallurgy processing were soaked for 28 days in simulated body fluid (SBF) with a pH of 7.4 at 37 deg. C and evaluated for the growth of calcium phosphate ceramics onto its surface. The composites were taken out once every 7 days and characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) for evaluating the Ca-P growth. Based on the change in chemistry of the SBF and phase contents, a model has been proposed for mechanism of growth of calcium phosphate compounds on sintered Ti-Ca-P composites immersed in SBF.

  10. In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Lee, J. H.; Freeland, J. W.; Hong, Hawoong, E-mail: hhong@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Tung, I. C. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Department of Materials Science and Engineering, Northwestern University, Evanston, Illinois 60208 (United States); Chang, S.-H.; Bhattacharya, A.; Fong, D. D. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2016-01-15

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

  11. In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

    International Nuclear Information System (INIS)

    Lee, J. H.; Freeland, J. W.; Hong, Hawoong; Tung, I. C.; Chang, S.-H.; Bhattacharya, A.; Fong, D. D.

    2016-01-01

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques

  12. Discussion on Microwave-Matter Interaction Mechanisms by In Situ Observation of "Core-Shell" Microstructure during Microwave Sintering.

    Science.gov (United States)

    Liu, Wenchao; Xu, Feng; Li, Yongcun; Hu, Xiaofang; Dong, Bo; Xiao, Yu

    2016-02-23

    This research aims to deepen the understanding of the interaction mechanisms between microwave and matter in a metal-ceramic system based on in situ synchrotron radiation computed tomography. A special internal "core-shell" microstructure was discovered for the first time and used as an indicator for the interaction mechanisms between microwave and matter. Firstly, it was proved that the microwave magnetic field acted on metal particles by way of inducing an eddy current in the surface of the metal particles, which led to the formation of a "core-shell" microstructure in the metal particles. On this basis, it was proposed that the ceramic particles could change the microwave field and open a way for the microwave, thereby leading to selective heating in the region around the ceramic particles, which was verified by the fact that all the "core-shell" microstructure was located around ceramic particles. Furthermore, it was indicated that the ceramic particles would gather the microwaves, and might lead to local heating in the metal-ceramic contact region. The focusing of the microwave was proved by the quantitative analysis of the evolution rate of the "core-shell" microstructure in a different region. This study will help to reveal the microwave-matter interaction mechanisms during microwave sintering.

  13. Thermal diffusivity of alumina-zirconia sintered with niobium additions

    International Nuclear Information System (INIS)

    Santos, W.N. dos; Paulin Filho, P.I.; Taylor, R.

    1994-01-01

    The effect of niobium oxide addition on the alumina-zirconia thermal diffusivity was investigated from 100 0 C to 1000 0 C by the laser flash method. It was observed that 4 to 6% addition of niobium oxide increases the thermal diffusivity when samples were sintered at 1450 0 C. This effect was due to elimination of porosity by formation of liquid please above 1420 0 C in the Al 2 O 3 - Nb 2 O 5 system. (author). 7 refs., 3 figs

  14. Microscopy of Alloy Formation on Arc Plasma Sintered Oxide Dispersion Strengthen (ODS) Steel

    Science.gov (United States)

    Bandriyana, B.; Sujatno, A.; Salam, R.; Dimyati, A.; Untoro, P.

    2017-07-01

    The oxide dispersed strengthened (ODS) alloys steel developed as structure material for nuclear power plants (NPP) has good resistant against creep due to their unique microstructure. Microscopy investigation on the microstructure formation during alloying process especially at the early stages was carried out to study the correlation between structure and property of ODS alloys. This was possible thanks to the arc plasma sintering (APS) device which can simulate the time dependent alloying processes. The ODS sample with composition of 88 wt.% Fe and 12 wt.% Cr powder dispersed with 1 wt.% ZrO2 nano powder was mixed in a high energy milling, isostatic compressed to form sample coins and then alloyed in APS. The Scanning Electron Microscope (SEM) with X-ray Diffraction Spectroscopy (EDX) line scan and mapping was used to characterize the microstructure and elemental composition distribution of the samples. The alloying process with unification of each Fe and Cr phase continued by the alloying formation of Fe-Cr by inter-diffusion of both Fe and Cr and followed by the improvement of the mechanical properties of hardness.

  15. Effects of sintering atmosphere and initial particle size on sintering of gadolinia-doped ceria; Efeitos da atmosfera de sinterizacao e do tamanho de particula na sinterizacao da ceria-gadolinia

    Energy Technology Data Exchange (ETDEWEB)

    Batista, Rafael Morgado

    2014-07-01

    The effects of the sintering atmosphere and initial particle size on the sintering of ceria containing 10 mol% gadolinia (GdO{sub 1.5}) were systematically investigated. The main physical parameter was the specific surface area of the initial powders. Nanometric powders with three different specific surface areas were utilized, 210 m{sup 2}/g, 36,2 m{sup 2}/g e 7,4 m{sup 2}/g. The influence on the densification, and micro structural evolution were evaluated. The starting sintering temperature was verified to decrease with increasing on the specific surface area of raw powders. The densification was accelerated for the materials with smaller particle size. Sintering paths for crystallite growth were obtained. Master sintering curves for gadolinium-doped ceria were constructed for all initial powders. A computational program was developed for this purpose. The results for apparent activation energy showed noticeable dependence with specific surface area. In this work, the apparent activation energy for densification increased with the initial particle size of powders. The evolution of the particle size distributions on non isothermal sintering was investigated by WPPM method. It was verified that the grain growth controlling mechanism on gadolinia doped ceria is the pore drag for initial stage and beginning of intermediate stage. The effects of the sintering atmosphere on the stoichiometry deviation of ceria, densification, microstructure evolution, and electrical conductivity were analyzed. Inert, oxidizing, and reducing atmospheres were utilized on this work. Deviations on ceria stoichiometry were verified on the bulk materials. The deviation verified was dependent of the specific surface area and sintering atmosphere. Higher reduction potential atmospheres increase Ce{sup 3+} bulk concentration after sintering. Accelerated grain growth and lower electrical conductivities were verified when reduction reactions are significantly present on sintering. (author)

  16. Break‐down of Losses in High Performing Metal‐Supported Solid Oxide Fuel Cells

    DEFF Research Database (Denmark)

    Kromp, A.; Nielsen, Jimmi; Blennow Tullmar, Peter

    2013-01-01

    in the metal support, the electrochemical fuel oxidation at the anode and the oxygen reduction in the mixed ionic electronic conducting cathode. An additional process with a rather high relaxation frequency was attributed to the formation of insulating interlayers at the cathode/electrolyte‐interface. Based...... on these results, selective measures to improve performance and stability, such as (i) PVD‐deposited CGO buffer layer preventing solid state reaction between cathode and the zirconia‐based electrolyte, (ii) LSC‐CGO based in‐situ sintered cathodes and (iii) reduced corrosion of the metal support, were adopted...

  17. High-level radioactive waste fixation in sintered vitreous matrix

    International Nuclear Information System (INIS)

    Russo, D.O.; Messi de Bernasconi, N.; Audero, M.A.

    1987-01-01

    The safe storage of high-level wastes from fuel elements reprocessing includes, as a first step, the fixation of the same in materials having a good resistance to the leaching in aqueous medium, such as borosilicate glass. As an alternative to the usual method of the molten glasses, a procedure for the sintering of a powdered glass and waste mixture at lower temperatures (600-700 deg C) has been developed, which minimizes the volatilization of active compounds during the process. Two glasses matrices of different composition and characteristics were used, to which the simulated wastes were added in the ratio of a 10% in weight of oxides. Two sintering techniques were employed 1: cold pressing and further sintering; 2: hot pressing and sintering under pressure. The densities were measured, the microstructure of the samples was analyzed and leaching essays were made in distilled water. The pellet's microstructure was observed by means of optical microscopy, by reflection in polished samples and by transparency in thin slices. The presence of crystalline compounds was analyzed by means of x rays and electron microprobe. The results have shown the convenience to continue with hot pressing essays, because a denser product with a higher resistance to the leaching is thus obtained. (M.E.L.) [es

  18. Experimental measurements of the thermal conductivity of ash deposits: Part 2. Effects of sintering and deposit microstructure

    Energy Technology Data Exchange (ETDEWEB)

    A. L. Robinson; S. G. Buckley; N. Yang; L. L. Baxter

    2000-04-01

    The authors report results from an experimental study that examines the influence of sintering and microstructure on ash deposit thermal conductivity. The measurements are made using a technique developed to make in situ, time-resolved measurements of the effective thermal conductivity of ash deposits formed under conditions that closely replicate those found in the convective pass of a commercial boiler. The technique is designed to minimize the disturbance of the natural deposit microstructure. The initial stages of sintering and densification are accompanied by an increase in deposit thermal conductivity. Subsequent sintering continues to densify the deposit, but has little effect on deposit thermal conductivity. SEM analyses indicates that sintering creates a layered deposit structure with a relatively unsintered innermost layer. They hypothesize that this unsintered layer largely determines the overall deposit thermal conductivity. A theoretical model that treats a deposit as a two-layered material predicts the observed trends in thermal conductivity.

  19. CRITIC-I: Instrumented lithium oxide irradiation: Part 1, Lithium oxide fabrication and characteristics

    International Nuclear Information System (INIS)

    Applegate, D.S.; Poeppel, R.B.

    1987-06-01

    Fine-grained, sinterable lithium oxide powder was prepared by high-temperature vacuum calcination of molten lithium carbonate. The product was ball milled, cold pressed, and fired in an oxygen atmosphere. The fired density, grain size, and surface roughness varied widely with firing schedule. Most variations were attributed to moisture content. Rings of high-density, sintered lithium oxide will be used in an in-reactor experiment to measure tritium release. 2 refs., 8 figs., 1 tab

  20. Vacuum-sintered body of a novel apatite for artificial bone

    Science.gov (United States)

    Tamura, Kenichi; Fujita, Tatsushi; Morisaki, Yuriko

    2013-12-01

    We produced regenerative artificial bone material and bone parts using vacuum-sintered bodies of a novel apatite called "Titanium medical apatite (TMA®)" for biomedical applications. TMA was formed by chemically connecting a Ti oxide molecule with the reactive [Ca10(PO4)6] group of Hydroxyapatite (HAp). The TMA powders were kneaded with distilled water, and solid cylinders of compacted TMA were made by compression molding at 10 MPa using a stainless-steel vessel. The TMA compacts were dried and then sintered in vacuum (about 10-3 Pa) or in air using a resistance heating furnace in the temperature range 1073-1773 K. TMA compacts were sintered at temperatures greater than 1073 K, thus resulting in recrystallization. The TMA compact bodies sintered in the range 1273-1773 K were converted into mixtures composed of three crystalline materials: α-TCP (tricalcium phosphate), β-TCP, and Perovskite-CaTiO3. The Perovskite crystals were stable and hard. In vacuum-sintering, the Perovskite crystals were transformed into fibers (approximately 1 µm in diameter × 8 µm in length), and the fiber distribution was uniform in various directions. We refer to the TMA vacuum-sintered bodies as a "reinforced composite material with Perovskite crystal fibers." However, in atmospheric sintering, the Perovskite crystals were of various sizes and were irregularly distributed as a result of the effect of oxygen. After sintering temperature at 1573 K, the following results were obtained: the obtained TMA vacuum-sintered bodies (1) were white, (2) had a density of approximately 2300 kg/m3 (corresponding to that of a compact bone or a tooth), and had a thermal conductivity of approximately 31.3 W/(m·K) (corresponding to those of metal or ceramic implants). Further, it was possible to cut the TMA bodies into various forms with a cutting machine. An implant made of TMA and inserted into a rabbit jaw bone was covered by new bone tissues after just one month because of the high

  1. Structure and characteristics of functional powder composite materials obtained by spark plasma sintering

    Science.gov (United States)

    Oglezneva, S. A.; Kachenyuk, M. N.; Kulmeteva, V. B.; Ogleznev, N. B.

    2017-07-01

    The article describes the results of spark plasma sintering of ceramic materials based on titanium carbide, titanium carbosilicide, ceramic composite materials based on zirconium oxide, strengthened by carbon nanostructures and composite materials of electrotechnical purpose based on copper with addition of carbon structures and titanium carbosilicide. The research shows that the spark plasma sintering can achieve relative density of the material up to 98%. The effect of sintering temperature on the phase composition, density and porosity of the final product has been studied. It was found that with addition of carbon nanostructures the relative density and hardness decrease, but the fracture strength of ZrO2 increases up to times 2. The relative erosion resistance of the electrodes made of composite copper-based powder materials, obtained by spark plasma sintering during electroerosion treatment of tool steel exceeds that parameter of pure copper up to times 15.

  2. Compactibility of Al/Al2O3 Isotropic Composite with Variation of Holding Time Sintering.

    Directory of Open Access Journals (Sweden)

    Eddy S Siradj

    2008-11-01

    Full Text Available The requirement of component with structural ability, light weight and also strength is increasing base on Metal Matrix Composites (MMCs by aluminum as matrix (AMCs. A structural ability is connected to composites compactibility which is depend on quality of interfacial bounding. Powder metallurgy is one of method to produce composite with powder mixing, compacting and sintering. Volume fractions reinforced and sintering time can influence composites compactibility. Volume fractions reinforced variable can produce different reinforcement effect. Beside that, on sintering enables the formation of new phase during sintering time. In this research, Al/Al2O3 isotropic composites are made with aluminum as matrix and alumina (Al2O3 as reinforced. Volume fraction reinforced used 10%. 20%. 30% and 40%. Sintering temperature and compaction pressure are each 600oC and 15 kN. The tests that applied are compression and metallographic test. The result that obtained is optimum compactibility of Al/Al2O3 composite reached at holding time 2 hour. During sintering, new phase can occur that is aluminum oxides (alumina, with unstable properties. The best volume fraction reinforced and holding time sintering are 40% and 2 hours.

  3. Science of sintering

    International Nuclear Information System (INIS)

    Kuczynski, G.

    1977-01-01

    Although the methods of integration of materials by sintering, have been used since the early history of humanity, the actual understanding of the process involved came only in the last three decades. As in the most human endeavors, the art preceded theory. The comprehension of the elementary processes occuring during sintering comes from the studies of model system. Although the elementary processes occuring during sintering are today quite well understood, the problem of shrinkage of a powder compact which was at the origin of Sintering Science is still far from solved. This is due to the complexity of the internal geometry of the compacts. The recent attempts to apply statistics to this problem, seem to offer some promise

  4. Effect of the sintering temperature and time on phase assemblage and electrical conductivity of zirconia-scandia-ceria

    International Nuclear Information System (INIS)

    Grosso, R.L.; Muccillo, E.N.S.

    2012-01-01

    ZrO 2 -based solid electrolytes have been extensively studied over the last decades for application in solid oxide fuel cells (SOFCs). Zirconia containing scandia and ceria solid electrolyte is a potential candidate in SOFCs operating at intermediate temperatures (600 - 800 deg C). In this work, commercial ZrO 2 containing 10 mol% Sc 2 O 3 and 1 mol% CeO 2 was sintered by the conventional and two-step methods. Several sintering conditions were evaluated by varying the temperature as well as the residence time. High values of sintered density (> 98%) were obtained. A careful selection of the sintering conditions is necessary in order to obtain a single cubic phase, as revealed by X-ray diffraction results. The grain growth can be controlled in specimens sintered by the two-step method. The electrical conductivity show similar behavior for the grain component independent on the sintering method. (author)

  5. A study on some properties of sintered stainless steel powder compacts with sintering conditions

    International Nuclear Information System (INIS)

    Lee, Bang Sik; Kim, Kwan Hyu; Lee, Doh Jae; Choi, Dap Chun

    1986-01-01

    Sintered specimens for the mechanical and corrosion tests were prepared from 316L, 410L and 434L stainless steel powder compacts with green densities in the range of 6.2∼7.0g/cm 3 . The experimental variables studied were green density, sintering atmosphere, temperature and time, type of lubricant used and cooling rate after sintering operation. Mechanical properties of green compacts and sintered specimens were evaluated. The corrosion tests were performed by potentiodynamic anodic polarization technique. Mechanical properties were very sensitive to the sintering atmosphere; sintering in dissociated ammonia resulted in the strengthing but embrittlement of sintered 316L, 410L and 434L strainless steel powder compacts. Their corrosion resistance was also decreased. The tensile strength was increased with increases in sintering time and temperature while the decreases in the yield strength were observed. The tensile properties of green compacts were shown to closely related to the green density. Addition of 1% acrawax as a lubricant was appeared to be most effective for the improvement of green strength. (Author)

  6. In situ oxidation and reduction of triangular nickel nanoplates via environmental transmission electron microscopy

    KAUST Repository

    LAGROW, A.P.

    2017-08-29

    Understanding the oxidation and reduction mechanisms of transition metals, such as nickel (Ni), is important for their use in industrial applications of catalysis. A powerful technique for investigating the redox reactive species is in situ environmental transmission electron microscopy (ETEM), where oxidation and reduction can be tracked in real time. One particular difficulty in understanding the underlying reactions is understanding the underlying morphology of the starting structure in a reaction, in particular the defects contained in the material, and the exposed surface facets. Here-in, we use a colloidal nanoparticle synthesis in a continuous flow reactor to form nanoplates of nickel coated with oleylamine as a capping agent. We utilise an in situ heating procedure at 300 °C in vacuum to remove the oleylamine ligands, and then oxidise the Ni nanoparticles at 25 °C with 2 Pa oxygen, and follow the nanoparticles initial oxidation. After that, the nanoparticles are oxidised at 200 and 300 °C, making the size of the oxide shell increase to ∼4 nm. The oxide shell could be reduced under 2 Pa hydrogen at 500 °C to its initial size of ∼1 nm. High temperature oxidation encouraged the nanoparticles to form pure NiO nanoparticles, which occurred via the Kirkendall effect leading to hollowing and void formation.

  7. In situ oxidation and reduction of triangular nickel nanoplates via environmental transmission electron microscopy

    KAUST Repository

    LAGROW, A.P.; AlYami, Noktan; LLOYD, D.C.; Bakr, Osman; BOYES, E.D.; GAI, P.L.

    2017-01-01

    Understanding the oxidation and reduction mechanisms of transition metals, such as nickel (Ni), is important for their use in industrial applications of catalysis. A powerful technique for investigating the redox reactive species is in situ environmental transmission electron microscopy (ETEM), where oxidation and reduction can be tracked in real time. One particular difficulty in understanding the underlying reactions is understanding the underlying morphology of the starting structure in a reaction, in particular the defects contained in the material, and the exposed surface facets. Here-in, we use a colloidal nanoparticle synthesis in a continuous flow reactor to form nanoplates of nickel coated with oleylamine as a capping agent. We utilise an in situ heating procedure at 300 °C in vacuum to remove the oleylamine ligands, and then oxidise the Ni nanoparticles at 25 °C with 2 Pa oxygen, and follow the nanoparticles initial oxidation. After that, the nanoparticles are oxidised at 200 and 300 °C, making the size of the oxide shell increase to ∼4 nm. The oxide shell could be reduced under 2 Pa hydrogen at 500 °C to its initial size of ∼1 nm. High temperature oxidation encouraged the nanoparticles to form pure NiO nanoparticles, which occurred via the Kirkendall effect leading to hollowing and void formation.

  8. In situ measurement of methane oxidation in groundwater by using natural-gradient tracer tests

    International Nuclear Information System (INIS)

    Smith, R.L.; Howes, B.L.; Garabedian, S.P.

    1991-01-01

    Methane oxidation was measured in an unconfined sand and gravel aquifer (Cape Cod, Mass.) by using in situ natural-gradient tracer tests at both a pristine, oxygenated site and an anoxic, sewage-contaminated site. The tracer sites were equipped with multilevel sampling devices to create target grids of sampling points; the injectate was prepared with groundwater from the tracer site to maintain the same geochemical conditions. Methane oxidation was calculated from breakthrough curves of methane relative to halide and inert gas (hexafluoroethane) tracers and was confirmed by the appearance of 13 C-enriched carbon dioxide in experiments in which 13 C-enriched methane was used as the tracer. A V max for methane oxidation could be calculated when the methane concentration was sufficiently high to result in zero-order kinetics throughout the entire transport interval. Methane breakthrough curves could be simulated by modifying a one-dimensional advection-dispersion transport model to include a Michaelis-Menten-based consumption term for methane oxidation. The K m values for methane oxidation that gave the best match for the breakthrough curve peaks were 6.0 and 9.0 μM for the uncontaminated and contaminated sites, respectively. Natural-gradient tracer tests are a promising approach for assessing microbial processes and for testing in situ bioremediation potential in groundwater systems

  9. In Situ Raman Spectroscopy of Supported Chromium Oxide Catalysts: Reactivity Studies with Methanol and Butane

    NARCIS (Netherlands)

    Weckhuysen, B.M.; Wachs, I.E.

    1996-01-01

    The interactions of methanol and butane with supported chromium oxide catalysts under oxidizing and reducing conditions were studied by in situ Raman spectroscopy as a function of the specific oxide support (Al2O3, ZrO2, TiO2, SiO2, Nb2O5, 3% SiO2/TiO2, 3% TiO2/SiO2, and a physical mixture of SiO2

  10. Iron oxide/cassava starch-supported Ziegler-Natta catalysts for in situ ethylene polymerization.

    Science.gov (United States)

    Chancharoenrith, Sittikorn; Kamonsatikul, Choavarit; Namkajorn, Montree; Kiatisevi, Supavadee; Somsook, Ekasith

    2015-03-06

    Iron oxide nanoparticles were used as supporters for in situ polymerization to produce polymer nanocomposites with well-dispersed fillers in polymer matrix. Iron oxide could be sustained as colloidal solutions by cassava starch to produce a good dispersion of iron oxide in the matrix. New supports based on iron oxide/cassava starch or cassava starch for Ziegler-Natta catalysts were utilized as heterogeneous supporters for partially hydrolyzed triethylaluminum. Then, TiCl4 was immobilized on the supports as catalysts for polymerization of ethylene. High-density polyethylene (HDPE) composites were obtained by the synthesized catalysts. A good dispersion of iron oxide/cassava starch particles was observed in the synthesized polymer matrix promoting to good mechanical properties of HDPE. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Guidelines for active spreading during in situ chemical oxidation to remediate contaminated groundwater

    Science.gov (United States)

    The effectiveness of in situ chemical oxidation to remediate contaminated aquifers depends on the extent and duration of contact between the injected treatment chemical and the groundwater contaminant (the reactants). Techniques that inject and extract in the aquifer to ‘ac...

  12. Manufacture of sintered bricks of high density from beryllium oxide; Fabrication de frittes de forte densite a base d'oxyde de beryllium

    Energy Technology Data Exchange (ETDEWEB)

    Pointud, R; Rispal, Ch; Le Garec, M [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1959-07-01

    Beryllium oxide bricks of nuclear purity 100 x 100 x 50 and 100 x 100 x 100 mm of very high density (between 2.85 and 3.00) are manufactured by sintering under pressure in graphite moulds at temperatures between 1,750 and 1,850 deg. C, and under a pressure of 150 kg/cm{sup 2}. The physico-chemical state of the saw material is of considerable importance with regard to the success of the sintering operation. In addition, a study of the sintering of a BeO mixture with 3 to 5 per cent of boron introduced in the form of boric acid, boron carbide or elementary boron shows that high densities can only be obtained by sintering under pressure. For technical reasons of manufacture, only the mixture based on boron carbide is used. The sintering is carried out in graphite moulds at 1500 deg. C under 150 kg/cm{sup 2} pressure, and bricks can be obtained with density between 2,85 and 2,90. Laboratory studies and the industrial manufacture of various sinters are described in detail. (author) [French] La fabrication de briques d'oxyde de beryllium de purete nucleaire de 100 x 100 x 50 et de 100 x 100 x 100 mm de densite tres elevee (comprise entre 2.85 et 3.00) est realisee par frittage sous charge dans des moules en graphite entre 1750 et 1850 deg. C, sous 150 kg/cm{sup 2} de pression. L'etat physico-chimique de la matiere premiere a une importance considerable quant au succes de l'operation de frittage. Par ailleurs, l'etude du frittage du mixte BeO a 3 et 5 pour cent de bore element introduit sous forme d'anhydride borique, soit de carbure de bore ou de bore element, montre que seul le frittage sous charge permet d'obtenir des densites elevees. Pour des raisons techniques de fabrication seul le mixte a base de carbure de bore est retenu. Le frittage s'opere dans des moules de graphite a 1500 deg. C sous 150 kg/cm{sup 2} de pression et permet d'obtenir des briques de densite comprise entre 2.85 et 2.90. Les etudes de laboratoire et la fabrication industrielle des differents

  13. The dimensional accuracy of the sintered billets

    Directory of Open Access Journals (Sweden)

    Чингиз Ариф оглы Алиев

    2016-01-01

    Full Text Available The article presents the results of assessing the impact of the behaviour stability of the components included in the compositions and process parameters of their production, on the dimensional accuracy of workpieces. It was found that by increasing the amount of oxide in the composition is greater compaction of the sintered billet in the process of heat treatment. This also increases the density of all components of the composition

  14. Mineral Phases and Release Behaviors of As in the Process of Sintering Residues Containing As at High Temperature

    Directory of Open Access Journals (Sweden)

    Xingrun Wang

    2014-01-01

    Full Text Available To investigate the effect of sintering temperature and sintering time on arsenic volatility and arsenic leaching in the sinter, we carried out experimental works and studied the structural changes of mineral phases and microstructure observation of the sinter at different sintering temperatures. Raw materials were shaped under the pressure of 10 MPa and sintered at 1000~1350°C for 45 min with air flow rate of 2000 mL/min. The results showed that different sintering temperatures and different sintering times had little impact on the volatilization of arsenic, and the arsenic fixed rate remained above 90%; however, both factors greatly influenced the leaching concentration of arsenic. Considering the product’s environmental safety, the best sintering temperature was 1200°C and the best sintering time was 45 min. When sintering temperature was lower than 1000°C, FeAsS was oxidized into calcium, aluminum, and iron arsenide, mainly Ca3(AsO42 and AlAsO4, and the arsenic leaching was high. When it increased to 1200°C, arsenic was surrounded by a glass matrix and became chemically bonded inside the matrix, which lead to significantly lower arsenic leaching.

  15. Geometrical and electrical properties of NTC polycrystalline thermistors vs. Changes of sintering parameters

    Directory of Open Access Journals (Sweden)

    Savić S.M.

    2006-01-01

    Full Text Available NTC thermistor powder was made of a Mn, Ni, Fe and Co oxide mixture calcinated at 1050°C / 60 min. The powder was milled in a ball mill down to an average particle diameter of 0.9 μm. Small disc shaped pills of the powder obtained were made by pressing with a pressure of 2.5 MPa. The pills were sintered in the temperature range of 900-1400 °C for 30-240 min. The volume and specific volume resistivity change were measured as a function of sintering conditions. Microstructure development was observed using a SEM microscope. Using the results obtained, optimization of sintering parameters was performed in order to determine optimal electrical properties of the selected thermistor composition.

  16. In situ studies of oxide nucleation, growth, and transformation using slow electrons

    Science.gov (United States)

    Flege, Jan Ingo; Grinter, David C.

    2018-05-01

    Surface processes such as metal oxidation and metal oxide growth invariably influence the physical and chemical properties of materials and determine their interaction with their surroundings and hence their functionality in many technical applications. On a fundamental level, these processes are found to be governed by a complex interplay of thermodynamic variables and kinetic constraints, resulting in a rich variety of material-specific phenomena. In this review article, we discuss recent results and insights on transition metal oxidation and rare-earth oxide growth acquired by low-energy electron microscopy and related techniques. We demonstrate that the use of in situ surface sensitive methods is a prerequisite to gaining a deeper understanding of the underlying concepts and the mechanisms responsible for the emerging oxide structure and morphology. Furthermore, examples will be provided on how structural and chemical modifications of the oxide films and nanostructures can be followed in real-time and analyzed in terms of local reactivity and cooperative effects relevant for heterogeneous model catalysis.

  17. Bioactive glass-reinforced bioceramic ink writing scaffolds: sintering, microstructure and mechanical behavior.

    Science.gov (United States)

    Shao, Huifeng; Yang, Xianyan; He, Yong; Fu, Jianzhong; Liu, Limin; Ma, Liang; Zhang, Lei; Yang, Guojing; Gao, Changyou; Gou, Zhongru

    2015-09-10

    The densification of pore struts in bioceramic scaffolds is important for structure stability and strength reliability. An advantage of ceramic ink writing is the precise control over the microstructure and macroarchitecture. However, the use of organic binder in such ink writing process would heavily affect the densification of ceramic struts and sacrifice the mechanical strength of porous scaffolds after sintering. This study presents a low-melt-point bioactive glass (BG)-assisted sintering strategy to overcome the main limitations of direct ink writing (extrusion-based three-dimensional printing) and to produce high-strength calcium silicate (CSi) bioceramic scaffolds. The 1% BG-added CSi (CSi-BG1) scaffolds with rectangular pore morphology sintered at 1080 °C have a very small BG content, readily induce apatite formation, and show appreciable linear shrinkage (∼21%), which is consistent with the composite scaffolds with less or more BG contents sintered at either the same or a higher temperature. These CSi-BG1 scaffolds also possess a high elastic modulus (∼350 MPa) and appreciable compressive strength (∼48 MPa), and show significant strength enhancement after exposure to simulated body fluid-a performance markedly superior to those of pure CSi scaffolds. Particularly, the honeycomb-pore CSi-BG1 scaffolds show markedly higher compressive strength (∼88 MPa) than the scaffolds with rectangular, parallelogram, and Archimedean chord pore structures. It is suggested that this approach can potentially facilitate the translation of ceramic ink writing and BG-assisted sintering of bioceramic scaffold technologies to the in situ bone repair.

  18. In-situ XRD and EDS method study on the oxidation behaviour of Ni-Cu sulphide ore.

    Science.gov (United States)

    Li, Guangshi; Cheng, Hongwei; Xiong, Xiaolu; Lu, Xionggang; Xu, Cong; Lu, Changyuan; Zou, Xingli; Xu, Qian

    2017-06-12

    The oxidation mechanism of sulfides is the key issue during the sulphide-metallurgy process. In this study, the phase transformation and element migration were clearly demonstrated by in-situ laboratory-based X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS), respectively. The reaction sequence and a four-step oxidation mechanism were proposed and identified. The elemental distribution demonstrated that at a low temperature, the Fe atoms diffused outward and the Ni/Cu atoms migrated toward the inner core, whereas the opposite diffusion processes were observed at a higher temperature. Importantly, the unique visual presentation of the oxidation behaviour provided by the combination of in-situ XRD and EDS might be useful for optimising the process parameters to improve the Ni/Cu extraction efficiency during Ni-Cu sulphide metallurgy.

  19. Technological parameter effect on properties of sintered hard-magnetic type Nd-Fe-B materials

    International Nuclear Information System (INIS)

    Rastegaev, V.S.; Stepanova, G.I.; Gudim, Z.Yu.

    1989-01-01

    The effect of each technological operation on manufacturing hard magnets from Nd-Fe-B alloys on properties of sintered permanent magnets is studied. It is noted that violation of the metting regime can result in burn-up of boron and rare earths, and violation of the grinding mode-formation of nonmagnetic powder fractions, etc. Special attention is paid to material protection against oxidation by introducing passivating additions and creating of particular conditions for alloy sintering and heat treatment

  20. Kinetics of UO2 sintering

    International Nuclear Information System (INIS)

    Ristic, M.M.

    1962-01-01

    Detailed conclusions related to the UO 2 sintering can be drawn from investigating the kinetics of the sintering process. This report gives an thorough analysis of the the data concerned with sintering available in the literature taking into account the Jander and Arrhenius laws. This analysis completes the study of influence of the O/U ratio and the atmosphere on the sintering. Results presented are fundamentals of future theoretical and experimental work related to characterisation of the UO 2 sintering process

  1. Influences of chemical packing and the chemical composition in porcelain sintering: from theory to practice

    International Nuclear Information System (INIS)

    Conceicao, E.S.; Gouvea, D.; Romano, R.C.O.; Pileggi, R.G.

    2011-01-01

    Studies have been conducted using the size distribution particles as a tool to obtain maximum packing in porcelain bodies. However, little attention has been given for the maximum size of particles and its effect in the sintering. While some particles are relatively large (63 μ m) for some oxides in the porcelain composition, they could compromise the sintering if a liquid phase is formed during heat processing. In this work, a comparative analysis showed that compositions with a maximum green packing density does not always lead to a maximum final densification in sintering if there is no control of the maximum size of the particles. (author)

  2. In situ polymerization of highly dispersed polypyrrole on reduced graphite oxide for dopamine detection.

    Science.gov (United States)

    Qian, Tao; Yu, Chenfei; Wu, Shishan; Shen, Jian

    2013-12-15

    A composite consisting of reduced graphite oxide and highly dispersed polypyrrole nanospheres was synthesized by a straightforward technique, by in situ chemical oxidative polymerization. The novel polypyrrole nanospheres can prevent the aggregation of reduced graphite oxide sheets by electrostatic repulsive interaction, and enhance their electrochemical properties in the nano-molar measurement of dopamine in biological systems with a linear range of 1-8000 nM and a detection limit as low as 0.3 nM. © 2013 Elsevier B.V. All rights reserved.

  3. Consolidation of W–Ta composites: Hot isostatic pressing and spark and pulse plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Dias, M., E-mail: marta.dias@itn.pt [Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Guerreiro, F. [Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Correia, J.B. [LNEG, Laboratório Nacional de Energia e Geologia, Estrada do Paço do Lumiar, 1649-038 Lisboa (Portugal); Galatanu, A. [National Institute of Materials Physics, Atomistilor 105 bis Bucharest-Magurele, 077125 Ilfov (Romania); Rosiński, M. [Warsaw University of Technology, Faculty of Materials Science and Engineering, Warsaw (Poland); Monge, M.A.; Munoz, A. [Departamento de Física, Univerdidad Carlos III de Madrid, Avd. de la Universidad 30, 28911 Madrid (Spain); Alves, E. [Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Carvalho, P.A. [Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); CeFEMA, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal)

    2015-10-15

    Highlights: • Consolidation of W–Ta composites using three techniques: HIP, SPS and PPS. • Comparison of consolidation methods in terms of W–Ta interdiffusion and densification. • Microstructure analysis in terms of oxides formation. - Abstract: Composites consisting of tantalum fiber/powder dispersed in a nanostructured W matrix have been consolidated by spark and pulse plasma sintering as well as by hot isostatic pressing. The microstructural observations revealed that the tungsten–tantalum fiber composites consolidated by hot isostatic pressing and pulse plasma sintering presented a continuous layer of Ta{sub 2}O{sub 5} phase at the W/Ta interfaces, while the samples consolidated by spark plasma sintering evidenced a Ta + Ta{sub 2}O{sub 5} eutectic mixture due to the higher temperature of this consolidation process. Similar results have been obtained for the tungsten–tantalum powder composites. A (W, Ta) solid solution was detected around the prior nanostructured W particles in tungsten–tantalum powder composites consolidated by spark and pulse plasma sintering. Higher densifications were obtained for composites consolidated by hot isostatic pressing and pulse plasma sintering.

  4. Multi-metallic anodes for solid oxide fuel cell applications

    International Nuclear Information System (INIS)

    Restivo, T.A. Guisard; Mello-Castanho, S.R.H.; Leite, D. Will

    2009-01-01

    A new method for direct preparation of materials for solid oxide fuel cell anode - Ni- YSZ cermets - based on mechanical alloying (MA) of the original powders is developed, allowing to admix homogeneously any component. Additive metals are selected from thermodynamic criteria, leading to compacts consolidation through sintering by activated surface (SAS). The combined process MA-SSA can reduce the sintering temperature by 300 deg C, yielding porous anodes. Densification mechanisms are discussed from quasi-isothermal sintering kinetics results. Doping with Ag, W, Cu, Mo, Nb, Ta, in descending order, promotes the densification of pellets through liquid phase sintering and evaporation of metals and oxides, which allow reducing the sintering temperature. Powders and pellets characterization by electronic microscopy and X-ray diffraction completes the result analyses. (author)

  5. Study of the sintering process and the formation of a (Th, U) O2 solid solution

    International Nuclear Information System (INIS)

    Tomasi, Roberto

    1979-01-01

    The effect of some variables in the (Th, U) O 2 sintering process and solid solution formation was studied. ThO 2 , U 3 O 8 and UO 2 powder were prepared. The ThO 2 powders were obtained by calcination of thorium at 500 and 750 deg C; the U 3 O 8 powders were derived from the calcination of ADU at 660 and 750 deg C; the UO 2 powder were prepared from ADU and from ATCU. The different characteristics of these materials were determined by measurements of surface area, by scanning electron microscopy, tap density tests, X-ray diffractometry and by measurements of the O/U ratios. The oxide mixtures were chosen in order to produce a final composition with 10 w/o of UO 2 . A mixture of thorium oxalate and ADU was also prepared by calcining these salts in air at 700 deg C, in order to obtain certain amount of solid solution prior to sintering. The sintering operations were developed in an argon atmosphere at temperatures between 1400 and 1700 deg C, during interval varying from 1 to 4 hours. The effect of the mixture characteristics on the sintering process and solid solution formation were studied considering the results of densification, microstructure development and X-ray diffractometry. The ThO 2 powder characteristics have a main effect on the mixtures compactability and sinterability, the higher calcining temperatures increasing the green density, but decreasing the final density of the sintered pellets. In the sintering of mixtures containing U 3 O 3 , this oxide is reduced to UO 2 and it is possible to obtain pellets with density and microstructures similar to those produced from mixtures containing UO 2 . But if oxygen in excess is present during sintering, the process is affected, occurring exaggerated grain growth. The densification results were related to the Coble's kinetics equation for second stage of sintering, valid for bulk diffusion, grain boundary acting as vacancy sinks. The sintering activation energy is independent from the powder starting

  6. Combined in situ zymography, immunofluorescence, and staining of iron oxide particles in paraffin-embedded, zinc-fixed tissue sections.

    Science.gov (United States)

    Haeckel, Akvile; Schoenzart, Lena; Appler, Franziska; Schnorr, Joerg; Taupitz, Matthias; Hamm, Bernd; Schellenberger, Eyk

    2012-01-01

    Superparamagnetic iron oxide particles are used as potent contrast agents in magnetic resonance imaging. In histology, these particles are frequently visualized by Prussian blue iron staining of aldehyde-fixed, paraffin-embedded tissues. Recently, zinc salt-based fixative was shown to preserve enzyme activity in paraffin-embedded tissues. In this study, we demonstrate that zinc fixation allows combining in situ zymography with fluorescence immunohistochemistry (IHC) and iron staining for advanced biologic investigation of iron oxide particle accumulation. Very small iron oxide particles, developed for magnetic resonance angiography, were applied intravenously to BALB/c nude mice. After 3 hours, spleens were explanted and subjected to zinc fixation and paraffin embedding. Cut tissue sections were further processed to in situ zymography, IHC, and Prussian blue staining procedures. The combination of in situ zymography as well as IHC with subsequent Prussian blue iron staining on zinc-fixed paraffin-embedded tissues resulted in excellent histologic images of enzyme activity, protease distribution, and iron oxide particle accumulation. The combination of all three stains on a single section allowed direct comparison with only moderate degradation of fluorescein isothiocyanate-labeled substrate. This protocol is useful for investigating the biologic environment of accumulating iron oxide particles, with excellent preservation of morphology.

  7. Processing and microstructure characterisation of oxide dispersion strengthened Fe–14Cr–0.4Ti–0.25Y2O3 ferritic steels fabricated by spark plasma sintering

    International Nuclear Information System (INIS)

    Zhang, Hongtao; Huang, Yina; Ning, Huanpo; Williams, Ceri A.; London, Andrew J.; Dawson, Karl; Hong, Zuliang; Gorley, Michael J.; Grovenor, Chris R.M.; Tatlock, Gordon J.; Roberts, Steve G.; Reece, Michael J.; Yan, Haixue; Grant, Patrick S.

    2015-01-01

    Highlights: • Nanostructured ODS steels were successfully produced by SPS. • Presence of Y 2 Ti 2 O 7 nanoclusters was confirmed by synchrotron XRD and microscopy. • The chemistry of nanoclusters tested by ATP indicated they are Y–Ti–O oxides. - Abstract: Ferritic steels strengthened with Ti–Y–O nanoclusters are leading candidates for fission and fusion reactor components. A Fe–14Cr–0.4Ti + 0.25Y 2 O 3 (14YT) alloy was fabricated by mechanical alloying and subsequently consolidated by spark plasma sintering (SPS). The densification of the 14YT alloys significantly improved with an increase in the sintering temperature. Scanning electron microscopy and electron backscatter diffraction revealed that 14YT SPS-sintered at 1150 °C under 50 MPa for 5 min had a high density (99.6%), a random grain orientation and a bimodal grain size distribution (<500 nm and 1–20 μm). Synchrotron X-ray diffraction patterns showed bcc ferrite, Y 2 Ti 2 O 7 , FeO, and chromium carbides, while transmission electron microscopy and atom probe tomography showed uniformly dispersed Y 2 Ti 2 O 7 nanoclusters of <5 nm diameter and number density of 1.04 × 10 23 m −3 . Due to the very much shorter consolidation times and lower pressures used in SPS compared with the more usual hot isostatic pressing routes, SPS is shown to be a cost-effective technique for oxide dispersion strengthened (ODS) alloy manufacturing with microstructural features consistent with the best-performing ODS alloys

  8. Effect of zinc oxide and boron oxide addition on the properties of yttrium-doped barium zirconate

    International Nuclear Information System (INIS)

    Andrade, Tiago Felipe

    2011-01-01

    BaZr 0.8 Y 0.2 O 3- δ protonic conductors, prepared by the ceramic route, were pressed and sintered with ZnO and B 2 O 3 sinter ing aids. The sintered pellets were analyzed by X-ray diffraction and impedance spectroscopy. Polished and thermally etched surfaces of the pellets were observed in a scanning probe microscope. The highest values of apparent density, 95%T.D., were obtained with 2 and 5 wt.% ZnO. The lowest value of electrical resistivity was obtained in BaZr 0.8 Y 0.2 O 3- δ compounds with 5 wt.% ZnO. Boron oxide and zinc oxide sinter ing aids were efficient to improve the apparent density as well as the electrical conductivity of BaZr 0.8 Y 0.2 O 3- δ protonic conductors. (author)

  9. In situ X-ray Rietveld analysis of Ni-YSZ solid oxide fuel cell anodes during NiO reduction in H2

    International Nuclear Information System (INIS)

    Reyes Rojas, A; Esparza-Ponce, H E; Fuentes, L; Lopez-Ortiz, A; Keer, A; Reyes-Gasga, J

    2005-01-01

    A synthesis and characterization of solid oxide fuel cell (SOFC) anodes of nickel with 8%mol yttrium stabilized zirconia (Ni-YSZ) is presented. Attention was focused on the kinetics and phase composition associated with the transformation of NiO-YSZ to Ni-YSZ. The anodes were prepared with an alternative synthesis method that includes the use of nickel acetylacetonate as an inorganic precursor to obtain a highly porous material after sintering at 1400 deg. C and oxide reduction (NiO-YSZ → Ni-YSZ) at 800 deg. C for 8 h in a tubular reactor furnace using 10% H 2 /N 2 . The obtained material was compressed by unidirectional axial pressing into 1 cm-diameter discs with 15-66 wt% Ni and calcinated from room temperature to 800 deg. C. A heating rate of 1 deg. C min -1 showed the best results to avoid any anode cracking. Their structural and chemical characterization during the isothermal reduction were carried out by in situ time-resolved X-ray diffraction, refined with the Rietveld method (which allowed knowing the kinetic process of the reduction), scanning electron microscopy and X-ray energy dispersive spectroscopy. The results showed the formation of tetragonal YSZ 8%mol in the presence of nickel, a decrement in the unit cell volume of Ni and an increment of Ni in the Ni-YSZ anodes during the temperature reduction. The analysis indicated that the Johnson-Mehl-Avrami equation is unable to provide a good fit to the kinetics of the phase transformation. Instead, an alternative equation is presented

  10. Master Sintering Surface: A practical approach to its construction and utilization for Spark Plasma Sintering prediction

    Directory of Open Access Journals (Sweden)

    Pouchly V.

    2012-01-01

    Full Text Available The sintering is a complex thermally activated process, thus any prediction of sintering behaviour is very welcome not only for industrial purposes. Presented paper shows the possibility of densification prediction based on concept of Master Sintering Surface (MSS for pressure assisted Spark Plasma Sintering (SPS. User friendly software for evaluation of the MSS is presented. The concept was used for densification prediction of alumina ceramics sintered by SPS.

  11. A comparison between different oxide dispersion strengthened ferritic steel ongoing in situ oxide dissolution in High Voltage Electron Microscope

    International Nuclear Information System (INIS)

    Monnet, I.; Van den Berghe, T.; Dubuisson, Ph.

    2012-01-01

    ODS materials are considered for nuclear applications but previous experimental studies have shown a partial dissolution of some oxides under neutron irradiation. In this work, electron irradiations were used to evaluate the stability of the oxides depending on the chemical composition of the oxide dispersion. Four ferritic steels based on EM10 (Fe–9Cr–1Mo) and reinforced respectively by Al 2 O 3 , MgO, MgAl 2 O 4 and Y 2 O 3 , were studied. These materials were irradiated with 1 MeV or 1.2 MeV electrons in a High Voltage Electron Microscope. This technique allows to follow one single oxide and to determine the evolution of its size during the irradiation. In situ HVEM observations indicate that the dissolution rate depends on the chemical composition of the oxide, on the temperature and on the irradiation dose.

  12. In-situ reduced graphene oxide-polyvinyl alcohol composite coatings as protective layers on magnesium substrates

    Directory of Open Access Journals (Sweden)

    Xingkai Zhang

    2017-06-01

    Full Text Available A simple and feasible method was developed to fabricate in-situ reduced graphene oxide-polyvinyl alcohol composite (GO-PVA coatings as protective layers on magnesium substrates. Polyvinyl alcohol was used as an in-situ reductant to transform GO into reduced GO. Contiguous and uniform GO-PVA coatings were prepared on magnesium substrates by dip-coating method, and were further thermally treated at 120 °C under ambient condition to obtain in-situ reduced GO-PVA coatings. Owing to the reducing effect of PVA, thermal treatment at low temperature led to effective in-situ reduction of GO as confirmed by XRD, Raman, FTIR and XPS tests. The corrosion current density of magnesium substrates in 3.5 wt% NaCl solution could be lowered to its 1/25 when using in-situ reduced GO-PVA coatings as protective layers.

  13. Alternative sintering methods compared to conventional thermal sintering for inkjet printed silver nanoparticle ink

    NARCIS (Netherlands)

    Niittynen, J.; Abbel, R.; Mäntysalo, M.; Perelaer, J.; Schubert, U.S.; Lupo, D.

    2014-01-01

    In this contribution several alternative sintering methods are compared to traditional thermal sintering as high temperature and long process time of thermal sintering are increasing the costs of inkjet-printing and preventing the use of this technology in large scale manufacturing. Alternative

  14. Method to produce sintered carriers for electrodes of galvanic elements

    Energy Technology Data Exchange (ETDEWEB)

    Jost, E M

    1978-03-24

    Carrier plates of precisely uniform thickness can be produced according to the invention by firstly thickening a solution of polyethylene oxide and (preferably) methanol by adding water and then, by adding nickel powder, obtaining an essentially homogeneous suspension of considerable viscosity. This slurry is coated on both sides of a nickel grid, dried and sintered.

  15. Sol-gel synthesis of lithium metatitanate as tritium breeding material under different sintering conditions

    Science.gov (United States)

    Lu, Wei; Wang, Jing; Pu, Wenjing; Li, Kaiping; Ma, Shubing; Wang, Weihua

    2018-04-01

    Lithium metatitanate (Li2TiO3) is a promising tritium breeding material candidate for solid blanket of D-T fusion reactors, due to its high mechanical strength, chemical stability, and tritium release rate. In this paper, Li2TiO3 powder with homogeneous crystal structure is synthesized by sol-gel method. The chemical reactions in gel thermal cracking and sintering process are studied by thermo gravimetric/differential scanning calorimetry (TG-DSC). The relationship between the sintering condition and the particle/grain size is characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Results show that below 673 K the gel precursor is completely decomposed and Li2TiO3 phase initially forms. The LiTiO2 by-product formed under the reductive atmosphere in muffle furnace, could be oxidized continually to Li2TiO3 at higher sintering temperature (≥1273 K) for longer sintering time (≥10 h). Both grain and particle sizes rely on a linear growth with the increase of sintering time at 1273 K. Over 1473 K, significant agglomerations exist among particles. The optimal sintering condition is selected as 1273 K for 10 h, for the purer Li2TiO3 phase (>99%), smaller grain and particle size.

  16. Effect of two-stage sintering process on microstructure and mechanical properties of ODS tungsten heavy alloy

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Kyong H. [Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology, 373-1 Kusong-dong, Yusong-gu, Taejon 305-701 (Korea, Republic of); Cha, Seung I. [International Center for Young Scientists, National Institute for Materials Science 1-1, Namiki, Tsukuba 305-0044 (Japan); Ryu, Ho J. [DUPIC, Korea Atomic Energy Research Institute, 150 Deokjin-dong, Yusong-gu, Taejon 305-353 (Korea, Republic of); Hong, Soon H. [Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology, 373-1 Kusong-dong, Yusong-gu, Taejon 305-701 (Korea, Republic of)], E-mail: shhong@kaist.ac.kr

    2007-06-15

    Oxide dispersion strengthened (ODS) tungsten heavy alloys have been considered as promising candidates for advanced kinetic energy penetrator due to their characteristic fracture mode compared to conventional tungsten heavy alloy. In order to obtain high relative density, the ODS tungsten heavy alloy needs to be sintered at higher temperature for longer time, however, induces growth of tungsten grains. Therefore, it is very difficult to obtain controlled microstructure of ODS tungsten heavy alloy having fine tungsten grains with full densification. In this study, two-stage sintering process, consisted of primary solid-state sintering and followed by secondary liquid phase sintering, was introduced for ODS tungsten heavy alloys. The mechanically alloyed 94W-4.56Ni-1.14Fe-0.3Y{sub 2}O{sub 3} powders are solid-state sintered at 1300-1450 deg. C for 1 h in hydrogen atmosphere, and followed by liquid phase sintering temperature at 1465-1485 deg. C for 0-60 min. The microstructure of ODS tungsten heavy alloys showed high relative density above 97%, with contiguous tungsten grains after primary solid-state sintering. The microstructure of solid-state sintered ODS tungsten heavy alloy was changed into spherical tungsten grains embedded in W-Ni-Fe matrix during secondary liquid phase sintering. The two-stage sintered ODS tungsten heavy alloy from mechanically alloyed powders showed finer microstructure and higher mechanical properties than conventional liquid phase sintered alloy. The mechanical properties of ODS tungsten heavy alloys are dependent on the microstructural parameters such as tungsten grain size, matrix volume fraction and tungsten/tungsten contiguity, which can be controlled through the two-stage sintering process.

  17. In-situ measurement of the electrical conductivity of aluminum oxide in HFIR

    Energy Technology Data Exchange (ETDEWEB)

    Zinkle, S.J.; White, D.P.; Snead, L.L. [Oak Ridge National Lab., TN (United States)] [and others

    1996-10-01

    A collaborative DOE/Monbusho irradiation experiment has been completed which measured the in-situ electrical resistivity of 12 different grades of aluminum oxide during HFIR neutron irradiation at 450{degrees}C. No evidence for bulk RIED was observed following irradiation to a maximum dose of 3 dpa with an applied dc electric field of 200 V/mm.

  18. In situ oxidation of zirconium binary alloys by environmental SEM and analysis by AFM, FIB, and TEM

    International Nuclear Information System (INIS)

    Proff, C.; Abolhassani, S.; Dadras, M.M.; Lemaignan, C.

    2010-01-01

    Binary Zr-alloys containing 1%Fe and 1% Ni (large precipitates) and 1% Cr and 0.6% Nb (small precipitates), as well as a pure Zr sample were exposed in situ at 130 Pa water vapour pressure at 415 o C in an environmental SEM. The surface topography and composition of each sample was characterised before in situ experiments, during and after oxidation. After oxidation the surface was characterised by SEM and EDS, AFM and TEM combined with EDS. Focused ion beam was used to prepare cross sections of the metal-oxide interface and for the preparation of TEM thin foils. The oxidation behaviour of precipitates for these alloying elements can be characterised into two large families, those which show a rapid oxidation and those which induce a delayed oxidation in comparison with the Zr-matrix. At 415 o C after 1 h of oxidation for Zr1%Fe and Zr1%Ni, the formation of protrusions could be detected at the surface, being related to underlying SPP in the oxide. On Zr1%Cr and Zr0.6%Nb unoxidised SPPs were observed in the oxide, close to the metal-oxide interface. These SPPs were, however, oxidised close to the outer surface of the oxide. The surface roughness was increased for all materials after in situ oxidation, however, only for Zr1%Fe and Zr1%Ni protrusions appeared on the surface during oxidation. It was subsequently demonstrated that these latter correspond to the position of SPPs. For Zr1%Fe the surface roughness increased more than in the other materials and on these protrusions small iron oxide crystals have been observed at the surface. These observations confirm that Fe has a different behaviour compared to the other SPP forming elements, and it diffuses out to the free surface of the material. These alloying elements being the constituents of the commercial alloys (Fe and Cr for Zircaloy-4; Fe, Cr and Ni for Zircaloy-2 and Nb for all Nb-containing alloys), this study allows to separate their individual influence and can allow a subsequent comparison to the behaviour

  19. Structure and Properties of Nanocomposites based on PTT-block-PTMO Copolymer and Graphene Oxide prepared by in Situ Polymerization

    OpenAIRE

    Paszkiewicz, Sandra; Szymczyk, Anna; Špitalský, Zdenko; Mosnáček, Jaroslav; Kwiatkowski, Konrad; Rosłaniec, Zbigniew

    2014-01-01

    Poly(trimethylene terephthalate-block-tetramethylene oxide) (PTT-PTMO) copolymer/graphene oxide nanocomposites were prepared by in situ polymerization. From the SEM and TEM images of PTT-PTMO/GO nanocomposite, it can be seen that GO sheets are clearly well-dispersed in the PTT-PTMO matrix. TEM images also showed that graphene was well exfoliated into individual sheets, suggesting that in situ polymerization is a highly efficient method for preparing nanocomposites. The influence of GO on the ...

  20. The influence of green microstructure and sintering parameters on precipitation process during copper-nickel-zinc ferrites sintering

    Directory of Open Access Journals (Sweden)

    Barba, Antonio

    2014-04-01

    Full Text Available Microstructural changes that occur during heat treatment of copper-nickel-zinc ferrites have been studied. The process of precipitation of the two types of crystals that occur during the sintering process has been analyzed. It is found that this process depends on dry relative density of the press specimens and on the following sintering parameters: sintering temperature, sintering time and cooling rate of the thermal cycle. Crystal precipitates characterization have been done by scanning electron microscopy (SEM, energy-dispersive X-ray (EDX analysis, X-ray diffraction (XRD, and X-ray photoelectron spectroscopy (XPS. These techniques have allowed to determine the nature of these crystals, which in this case correspond to zinc and copper oxides. It has been used two chemical reactions to explain the bulk precipitation and subsequent re-dissolution of these crystal precipitates during sintering.En este trabajo se han estudiado los cambios microestructurales que se producen durante el tratamiento térmico de las ferritas de cobre-níquel-cinc y se ha analizado el proceso de precipitación de los dos tipos de cristales que aparecen durante el proceso de sinterización. Se ha encontrado que este proceso depende de la densidad relativa en seco de las muestras compactadas y de las siguientes variables de la etapa de sinterización: temperatura y tiempo de sinterización y velocidad de enfriamiento. La caracterización de los cristales precipitados se ha realizado por microscopía electrónica de barrido (MEB, microanálisis por dispersión de energía de rayos X (EDX, difracción de rayos X (DRX, y espectroscopía de fotoelectrones de rayos X (XPS. Estas técnicas han permitido determinar la naturaleza de estos cristales, que en este caso corresponden a los óxidos de cinc y de cobre. Se han propuesto dos reacciones químicas que permiten explicar el proceso de precipitación y la posterior re-disolución de estos cristales precipitados durante la

  1. Production of pure sintered alumina

    International Nuclear Information System (INIS)

    Rocha, J.C. da; Huebner, H.W.

    1982-01-01

    With the aim of optimizing the sintering parameters, the strength of a large number of alumina samples was determined which were produced under widely varying sintering conditions and with different amounts of MgO content. The strength as a function of sintering time or temperature was found to go through a maximum. With increasing time, this maximum is shifted to lower temperatures, and with decreasing temperature to longer times. Data pairs of sintering times and temperatures which yeld the strength maximum were determined. The value of the strength at the maximum remains unchanged. The strength is high (= 400 MN/m 2 , at a grain size of 3 um and a porosity of 2 per cent) and comparable to foreign aluminas produced for commercial purposes, or even higher. The increase in the sintering time from 1 h to 16 h permits a reduction of the sintering temperature from 1600 to 1450 0 C without losing strength. The practical importance of this fact for a production of sintered alumina on a large scale is emphasized. (Author) [pt

  2. Trace metal chemistry and silicification of microorganisms in geothermal sinter, Taupo Volcanic Zone, New Zealand

    Energy Technology Data Exchange (ETDEWEB)

    McKenzie, E.J.; Brown, K.L.; Campbell, K.A. [University of Auckland (New Zealand). Dept. of Geology; Cady, S.L. [Portland State University, Portland, OR (United States). Dept. of Geology

    2001-08-01

    As part of a pilot study investigating the role of microorganisms in the immobilisation ol As, Sb, B, Tl and Ug, the inorganic geochemistry of seven different active sinter deposits and their contact fluids were characterised. A comprehensive series of sequential extractions for a suite of trace elements was carried out on siliceous sinter and a mixed silica-carbonate sinter. The extractions showed whether metals were loosely exchangeable or bound to carbonate, oxide, organic or crystalline fractions. Hyperthermophilic microbial communities associated with sinters deposited from high temperature (92-94{sup o}C) fluids at a variety of geothermal sources were investigated using SEM. The rapidity and style of silicification of the hyperthermophiles can be correlated with the dissolved silica content of the fluid. Although high concentrations of Hg and TI were found associated with the organic fraction of the sinters, there was no evidence to suggest that any of the heavy metals were associated preferentially with the hyperthermophiles at the high temperature (92-94{sup o}C) ends of the terrestrial thermal spring ecosystems studied. (author)

  3. Kinetics of sintering of uranium dioxide

    International Nuclear Information System (INIS)

    Soni, N.C.; Moorthy, V.K.

    1978-01-01

    The kinetics of sintering of UO 2 powders derived from ADU route and calcined at different temperatures was studied. The activation energy for sintering was found to depend on the calcination temperature, the density chosen and the sintering temperature range. The motive force for sintering is the excess free energy in the particle system. This exists in the powder compact in the form of surface energy and the excess lattice energy due to defects. The defects which can be eliminated at the operating temperature are responsible for the mobility and hence sintering. This concept of the motive force for sintering has been used to explain the difference in the activation energies observed in the present study. This would also explain phenomena such as attainment of limiting density, presence of optimum sintering temperature and the influence of calcination treatments on the sintering behaviour of powders. (author)

  4. Cost and Performance Assessment of In-situ Chemical Oxidation for Intermittent and Continuous Oxidant Injection

    Science.gov (United States)

    Kim, U.; Parker, J.; Borden, R. C.

    2015-12-01

    In situ chemical oxidation (ISCO) is a popular remediation technology that involves injection of chemical oxidant into groundwater to destroy dissolved and non-aqueous liquid phase contaminants. Depending on site conditions, oxidant can be injected into the contaminated subsurface periodically (intermittently) or continuously. A common approach is to intermittently inject oxidant into a network of wells over a period long enough to emplace oxidant over a target treatment volume (referred to ISCO-int). The injection phase is followed by a passive phase when the oxidant is allowed to react with contaminants and natural oxygen demand (NOD) and to migrate under natural hydraulic gradients. This process may be repeated multiple times until termination criteria are met. Recently, some practitioners have adopted an alternative approach in which oxidant is injected continuously with extraction wells recovering unreacted oxidant to recycle with additional makeup oxidant to maintain its constant concentration (referred to ISCO-cont). Each method has certain advantages and disadvantages. This study numerically evaluates those two ISCO practices in terms of remediation costs and performance based on multiple equi-probable parameter sets. Stochastic cost optimization toolbox (SCOToolkit) is used for this purpose. SCOToolkit is an integrated semi-analytical model for contaminant transport and remediation (e.g., thermal source treatment, ISCO, electron donor injections, permeable reactive barriers) enabling inverse solution and Monte Carlo simulations. Four different aquifer settings, slow and fast Darcy velocities combined with low and high NOD conditions, are used for the evaluation. Preliminary results showed that ISCO-cont is effective for a full scale application without large investment while ISCO-int is more efficient to utilize oxidant in well-characterized sites. Pros and cons of each approach are discussed for the practical use of ISCO for various site conditions.

  5. Low-Cost Manufacturing of Bioresorbable Conductors by Evaporation-Condensation-Mediated Laser Printing and Sintering of Zn Nanoparticles.

    Science.gov (United States)

    Shou, Wan; Mahajan, Bikram K; Ludwig, Brandon; Yu, Xiaowei; Staggs, Joshua; Huang, Xian; Pan, Heng

    2017-07-01

    Currently, bioresorbable electronic devices are predominantly fabricated by complex and expensive vacuum-based integrated circuit (IC) processes. Here, a low-cost manufacturing approach for bioresorbable conductors on bioresorbable polymer substrates by evaporation-condensation-mediated laser printing and sintering of Zn nanoparticle is reported. Laser sintering of Zn nanoparticles has been technically difficult due to the surface oxide on nanoparticles. To circumvent the surface oxide, a novel approach is discovered to print and sinter Zn nanoparticle facilitated by evaporation-condensation in confined domains. The printing process can be performed on low-temperature substrates in ambient environment allowing easy integration on a roll-to-roll platform for economical manufacturing of bioresorbable electronics. The fabricated Zn conductors show excellent electrical conductivity (≈1.124 × 10 6 S m -1 ), mechanical durability, and water dissolvability. Successful demonstration of strain gauges confirms the potential application in various environmentally friendly sensors and circuits. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. In Situ Bioremediation of 1,4-Dioxane by Methane Oxidizing Bacteria in Coupled Anaerobic-Aerobic Zones

    Science.gov (United States)

    2016-02-11

    FINAL REPORT In Situ Bioremediation of 1,4-Dioxane by Methane Oxidizing Bacteria in Coupled Anaerobic-Aerobic Zones SERDP Project ER-2306...volatile organic compound (CVOCs), ethene and ethane in groundwater at Raritan Arsenal Area 18C after in situ bioremediation . 4 List of...aquifers, the bioremediation approach most commonly used for chlorinated solvents. The ability of methanotrophs to biodegrade 1,4-dioxane was

  7. Study of pore closure during pressure-less sintering of advanced oxide ceramics

    Czech Academy of Sciences Publication Activity Database

    Spusta, T.; Svoboda, Jiří; Maca, K.

    2016-01-01

    Roč. 115, AUG (2016), s. 347-353 ISSN 1359-6454 R&D Projects: GA ČR(CZ) GA15-06390S Institutional support: RVO:68081723 Keywords : Ceramic material * Sintering * Porosity * Modelling * Hot isostatic pressing Subject RIV: BJ - Thermodynamics Impact factor: 5.301, year: 2016

  8. Sintering and thermal ageing studies of zirconia - yttria ceramics by impedance spectroscopy

    International Nuclear Information System (INIS)

    Florio, Daniel Zanetti de

    1998-01-01

    ZrO 2 :8 mol %Y 2 O 3 solid electrolyte ceramic pellets have been prepared with powders of three different origins: a Nissan (Japan) commercial powder, a powder obtained by the coprecipitation technique at IPEN, and the mixing of powder oxides (ZrO 2 produced at a Pilot Plant at IPEN and 99.9% pure Y 2 O 3 of USA origin). These starting powders have been analysed by the following techniques: X-ray fluorescence for yttrium content, X-ray diffraction for structural phase content, sedimentation for particle size distribution, gas adsorption (BET) for surface area determination, and transmission electron microscopy for average particle size determination. Pressed ceramic pellets have been analysed by dilatometry to evaluate the sintering stages. Sintered pellets have been characterized by X-ray diffraction for phase analysis and scanning electron microscopy for grain morphology analysis. Impedance spectroscopy analysis have been carried out to follow thermal ageing of zirconia-yttria solid electrolyte at 600 deg C, the working temperature of permanent oxygen sensor, and to study sintering kinetics. The main results show that ageing at 600 deg C decreases the emf sensor response in the first 100 h to a steady value. Moreover, sintering studies by impedance spectroscopy allowed for finding correlations between electrical parameters, sintering kinetics and grain growth mechanisms. (author)

  9. In situ observations of oxide fracture on austenitic stainless steels relevant to IASCC

    International Nuclear Information System (INIS)

    Duff, J.; Burke, M.G.; Scenini, F.

    2015-01-01

    Stress Corrosion Cracking (SCC) and Irradiation-Assisted Stress Corrosion Cracking (IASCC) are important failure modes in the nuclear industry, yet the exact mechanism(s) responsible for these complex failure phenomena are not fully understood. In particular, considerable attention is being focused on SCC and IASCC initiation and the behaviour of the oxidised metal surface during straining in a relevant environment. Experimental observations and data for oxide fracture at the grain boundary are limited, but are also required for the development of crack growth models. In this work, the role of strain localization on surface oxide fracture has been examined via: 1) in situ straining experiments using a state-of-the-art imaging autoclave; and 2) ex situ studies using pre-oxidised samples in a FEG-SEM with a micro-tensile stage. The work was conducted using three materials: 1) a non-irradiated archive Type 316 Stainless Steel, 2) a 1 dpa proton-irradiated Type 316 Stainless Steel, and 3) a model alloy designed to simulate the grain boundary composition resulting from radiation induced segregation. The observations were performed on samples pre-oxidized at 320 C. degrees in high purity, water containing 30 cm 3 /kg of dissolved H 2 and 2 ppm Li additions. The samples were strained in tension and the surface deformation measured via Digital Image Correlation. This technique provided quantitative data regarding the intergranular strains associated with oxide fracture. Oxide fracture and strain development were also related to the local irradiation-induced microstructure and grain boundary character. The results from this work contribute to the mechanistic information on the role of strain localization and composition on the incubation stages of IASCC. (authors)

  10. Nickel and Copper-Free Sintered Structural Steels Containing Mn, Cr, Si, and Mo Developed for High Performance Applications

    Directory of Open Access Journals (Sweden)

    Cias A.

    2017-03-01

    Full Text Available In an attempt to study the sinterability of potential high-strength nickel-free sintered structural steels containing Mn, Cr, Si and Mo compacts were prepared based on sponge and water atomised iron powders and on Astaloy prealloyed powders. To these were admixed ferromanganese, ferroslicon, and graphite. The samples were sintered at temperatures 1120 and 1250°C in laboratory tube furnaces in hydrogen, hydrogen-nitrogen atmospheres with dew points better than -60°C or in nitrogen in a semiclosed container in a local microatmosphere. After sintering the samples were slowly cooled or sinterhardened. Generally resultant microstructures were inhomogeneous, consisted of pearlite/ bainite/martensite, but were characterised by an absence of oxide networks. Sintering studies performed over a range of compositions have shown that superior strength, ranging beyond 900 MPa, along with reasonable tensile elongation, can be achieved with these new steels.

  11. Strain-enhanced sintering of iron powders

    Energy Technology Data Exchange (ETDEWEB)

    Amador, D.R.; Torralba, J.M. [Universidad Carlos III de Madrid, Departamento de Ciencias de Materiales e Ingenieria Metalurgica, Leganes, Madrid (Spain); Monge, M.A.; Pareja, R. [Universidad Carlos III de Madrid, Departamento de Fisica, Madrid (Spain)

    2005-02-01

    Sintering of ball-milled and un-milled Fe powders has been investigated using dilatometry, X-ray, density, and positron annihilation techniques. A considerable sintering enhancement is found in milled powders showing apparent activation energies that range between 0.44 and 0.80 eV/at. The positron annihilation results, combined with the evolution of the shrinkage rate with sintering temperature, indicate generation of lattice defects during the sintering process of milled and un-milled powders. The sintering enhancement is attributed to pipe diffusion along the core of moving dislocations in the presence of the vacancy excess produced by plastic deformation. Positron annihilation results do not reveal the presence of sintering-induced defects in un-milled powders sintered above 1200 K, the apparent activation energy being in good agreement with that for grain-boundary diffusion in {gamma}-Fe. (orig.)

  12. Composition of ammonia-oxidizing archaea and their contribution to nitrification in a high-temperature hot spring

    Science.gov (United States)

    Chen, S.; Peng, X.-T.; Xu, H.-C.; Ta, K.-W.

    2015-10-01

    The oxidation of ammonia by microbes and associated organisms has been shown to occur in diverse natural environments. However, the contribution of ammonia-oxidizing archaea to nitrification in high-temperature environments remains unclear. Here, we studied in situ ammonia oxidation rates and the abundance of ammonia-oxidizing archaea (AOA) in surface and bottom sediments at 77 °C in the Gongxiaoshe hot spring, Tengchong, Yunnan, China. The in situ ammonia oxidation rates measured by the 15N-NO3- pool dilution technique in the surface sinter and bottom sediments were 4.8 and 5.3 nmol N g-1 h-1, respectively. Relative abundances of Crenarchaea in both samples were determined by fluorescence in situ hybridization (FISH). Phylogenetic analysis of 16S rRNA genes showed high sequence similarity to thermophilic "Candidatus Nitrosocaldus yellowstonii", which represented the most abundant operation taxonomic units (OTU) in both sediments. Furthermore, bacterial amoA was not detected in this study. Quantitative PCR (qPCR) indicated that AOA and 16S rRNA genes were present in the range of 2.75 to 9.80 × 105 and 0.128 to 1.96 × 108 gene copies g-1 sediment. The cell-specific nitrification rates were estimated to be in the range of 0.41 to 0.79 fmol N archaeal cell-1 h-1, which is consistent with earlier estimates in estuary environments. This study demonstrated that AOA were widely involved in nitrification in this hot spring. It further indicated the importance of archaea rather than bacteria in driving the nitrogen cycle in terrestrial geothermal environments.

  13. Preparation and characterization of amorphous SiO2 coatings deposited by mirco-arc oxidation on sintered NdFeB permanent magnets

    International Nuclear Information System (INIS)

    Xu, J.L.; Xiao, Q.F.; Mei, D.D.; Zhong, Z.C.; Tong, Y.X.; Zheng, Y.F.; Li, L.

    2017-01-01

    Amorphous SiO 2 coatings were prepared on sintered NdFeB magnets by micro-arc oxidation (MAO) in silicate solution. The surface and cross-sectional morphologies, element and phase composition, corrosion resistance and magnetic properties of the coatings were investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectroscopy (XPS), potentiodynamic polarization test and physical properties measurements system (PPMS). The results showed that the surface morphologies of the coatings exhibited the “coral reef” like structure, different from the typical MAO porous structure. With increasing the voltages, the thickness of the coatings increased from 12.72 to 19.90 µm, the content of Si element increased, while the contents of Fe, Nd and P elements decreased. The coatings were mainly composed of amorphous SiO 2 and a few amorphous Fe 2 O 3 and Nd 2 O 3 . The amorphous SiO 2 coatings presented excellent thermal shock resistance, while the thermal shock resistance decreased with increasing the voltages. The corrosion resistance of the coatings increased with increasing the voltages, and it could be enhanced by one order of magnitude compared to the uncoated NdFeB magnets. The MAO coatings slightly decreased the magnetic properties of the NdFeB samples in different degrees. - Highlights: • Amorphous SiO 2 coatings were prepared on sintered NdFeB magnets by micro-arc oxidation. • The coatings presented excellent thermal shock resistance. • The corrosion resistance could be enhanced by one order of magnitude. • The MAO coatings slightly decreased the magnetic properties of the NdFeB samples.

  14. A Reactive Oxide Overlayer on Rh Nanoparticles during CO Oxidation and Its Size Dependence Studied by in Situ Ambient Pressure XPS

    International Nuclear Information System (INIS)

    Grass, Michael E.; Zhang, Yawen; Butcher, Derek R.; Park, Jeong Y.; Li, Yimin; Bluhm, Hendrik; Bratlie, Kaitlin M.; Zhang, Tianfu; Somorjai, Gabor A.

    2008-01-01

    CO oxidation is one of the most studied heterogeneous reactions, being scientifically and industrially important, particularly for removal of CO from exhaust streams and preferential oxidation for hydrogen purification in fuel cell applications. The precious metals Ru, Rh, Pd, Pt, and Au are most commonly used for this reaction because of their high activity and stability. Despite the wealth of experimental and theoretical data, it remains unclear what is the active surface for CO oxidation under catalytic conditions for these metals. In this communication, we utilize in situ synchrotron ambient pressure X-ray photoelectron spectroscopy (APXPS) to monitor the oxidation state at the surface of Rh nanoparticles during CO oxidation and demonstrate that the active catalyst is a surface oxide, the formation of which is dependent on particle size. The amount of oxide formed and the reaction rate both increase with decreasing particle size.

  15. Hydrous pyrolysis/oxidation process for in situ destruction of chlorinated hydrocarbon and fuel hydrocarbon contaminants in water and soil

    Science.gov (United States)

    Knauss, Kevin G.; Copenhaver, Sally C.; Aines, Roger D.

    2000-01-01

    In situ hydrous pyrolysis/oxidation process is useful for in situ degradation of hydrocarbon water and soil contaminants. Fuel hydrocarbons, chlorinated hydrocarbons, polycyclic aromatic hydrocarbons, petroleum distillates and other organic contaminants present in the soil and water are degraded by the process involving hydrous pyrolysis/oxidation into non-toxic products of the degradation. The process uses heat which is distributed through soils and water, optionally combined with oxygen and/or hydrocarbon degradation catalysts, and is particularly useful for remediation of solvent, fuel or other industrially contaminated sites.

  16. Solid-state sintering of tungsten heavy alloys

    International Nuclear Information System (INIS)

    Gurwell, W.E.

    1994-10-01

    Solid-state sintering is a technologically important step in the fabrication of tungsten heavy alloys. This work addresses practical variables affecting the sinterability: powder particle size, powder mixing, and sintering temperature and time. Compositions containing 1 to 10 micrometer (μM) tungsten (W) powders can be fully densified at temperatures near the matrix solidus. Blending with an intensifier bar provided good dispersion of elemental powders and good as-sintered mechanical properties under adequate sintering conditions. Additional ball milling increases powder bulk density which primarily benefits mold and die filling. Although fine, 1 μm W powder blends have high sinterability, higher as-sintered ductilities are reached in shorter sintering times with coarser, 5 μm W powder blends; 10μm W powder blends promise the highest as-sintered ductilities due to their coarse microstructural W

  17. Profile of yttrium segregation in BaCe0,9Y0,1O3-δ as function of sintering temperature

    International Nuclear Information System (INIS)

    Hosken, C.M.; Souza, D.P.F. de

    2010-01-01

    Researches on solid oxide fuel cells indicate barium cerate perovskite as a very attractive material for using as electrolyte due to its high protonic conductivity. The objective of this work is investigate the yttrium segregation during sintering of BaCe 0,9 Y 0,1 O 3-δ doped with Zn O as a sintering aid. The powders were prepared by citrate process. Powders were isostatic pressed into pellets and sintered in air at 1200, 1275, 1325 and 1400 deg C. The samples were characterized by scanning electron microscopy, X-ray diffraction and impedance spectroscopy. Secondary phase containing Yttrium and Cerium was detected as sintering temperature increased. Increase of the lattice parameter and activation energy for electrical conductivity were also detected on samples sintered at 1400 deg C. (author)

  18. Influence of the starch content and sintering temperature on the processing of porous zirconia substrates

    International Nuclear Information System (INIS)

    Albano, Maria P; Garrido, Liliana B

    2008-01-01

    Porous ceramics are used as electrodes in fuel cells, separators in batteries, filters, etc. Thin porous substrates of zirconium stabilized with yttrium oxide (ZSY) are used as anodes in solid oxide fuel cells. One way to obtain a porous band is to mix starch particles during the preparation stage of the ZSY suspension. The starch burns during the removal of the binder and leaves stable pores that are not eliminated in the subsequent sintering stage. This work used the band pouring process to produce porous bands of ZSY with porosities of 29% to 53% using starch as a transitory additive. Concentrated aqueous suspensions of ZSY were prepared with different contents of starch and of an acrylic latex binder. The influence of the fraction of starch volume and of the temperature on the sintering behavior and on the final micro structure of the bands was studied. The total porosity of the bands was higher than the fractions in volume of added starch, due to the presence of closed porosity in the matrix. The deviations compared to the porosity predicted based on the fractions in the volume of starch, were greater as the starch content increased. The percentage of open porosity in the sintered bands depended on the fraction in the volume of added starch and on the sintering temperature. When the fraction in volume of starch increased from 17.6% to 37.8% a gradual increase occurred in the opening of the porous structure. The contraction of the bands during sintering at a given temperature correlated with the density of the packing of ZSY (au)

  19. In Situ Synchrotron X-Ray Diffraction Characterization of the Synthesis of Graphene Oxide and Reduced Graphene Oxide

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2015-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) synthesised from GO, has a promising future in fields ranging from electronics to energy technologies[1]. GO may be synthesized by the modified Hummer’s method[2], where a mixture of potassium permanganate and concentrated sulfuric acid forms...... by placing a mixture of permanganate and sulphuric acid in a capillary next to graphite. The synthesis was then initiated by gently pushing the fluid mixture into the powder with N2 gas. The in situ XRD of the GO synthesis showed how the oxidation reaction proceeds in three separate stages, as seen in Figure...... 1. The first stage was the dissolution of potassium permanganate, followed by an intercalation stage and subsequent formation of crystalline material. The GO 001 diffraction peak was observed early during the synthesis, in the second stage, and the intensity of the 001 diffraction increased during...

  20. Alumina-zirconium ceramics synthesis by selective laser sintering/melting

    International Nuclear Information System (INIS)

    Shishkovsky, I.; Yadroitsev, I.; Bertrand, Ph.; Smurov, I.

    2007-01-01

    In the present paper, porous refractory ceramics synthesized by selective laser sintering/melting from a mixture of zirconium dioxide, aluminum and/or alumina powders are subjected to optical metallography and X-ray analysis to study their microstructure and phase composition depending on the laser processing parameters. It is shown that high-speed laser sintering in air yields ceramics with dense structure and a uniform distribution of the stabilizing phases. The obtained ceramic-matrix composites may be used as thermal and electrical insulators and wear resistant coating in solid oxide fuel cells, crucibles, heating elements, medical tools. The possibility to reinforce refractory ceramics by laser synthesis is shown on the example of tetragonal dioxide of zirconium with hardened micro-inclusion of Al 2 O 3 . By applying finely dispersed Y 2 O 3 powder inclusions, the type of the ceramic structure is significantly changed

  1. Sintering of MnCo2O4 coatings prepared by electrophoretic deposition

    DEFF Research Database (Denmark)

    Bobruk, M.; Molin, Sebastian; Chen, Ming

    2018-01-01

    Sintering of MnCo2O4 coatings prepared by electrophoretic deposition on steel substrates has been studied in air and in reducing-oxidizing atmosphere. Effect of temperature and pO2 on the resulting coating density was evaluated from scanning electron microscopy images of polished cross sections...

  2. Studying hardness, workability and minimum bending radius in selectively laser-sintered Ti–6Al–4V alloy samples

    Science.gov (United States)

    Galkina, N. V.; Nosova, Y. A.; Balyakin, A. V.

    2018-03-01

    This research is relevant as it tries to improve the mechanical and service performance of the Ti–6Al–4V titanium alloy obtained by selective laser sintering. For that purpose, sintered samples were annealed at 750 and 850°C for an hour. Sintered and annealed samples were tested for hardness, workability and microstructure. It was found that incomplete annealing of selectively laser-sintered Ti–6Al–4V samples results in an insignificant reduction in hardness and ductility. Sintered and incompletely annealed samples had a hardness of 32..33 HRC, which is lower than the value of annealed parts specified in standards. Complete annealing at temperature 850°C reduces the hardness to 25 HRC and ductility by 15...20%. Incomplete annealing lowers the ductility factor from 0.08 to 0.06. Complete annealing lowers that value to 0.025. Complete annealing probably results in the embrittlement of sintered samples, perhaps due to their oxidation and hydrogenation in the air. Optical metallography showed lateral fractures in both sintered and annealed samples, which might be the reason why they had lower hardness and ductility.

  3. Inversion defects in MgAl2O4 elaborated by pressureless sintering, pressureless sintering plus hot isostatic pressing, and spark plasma sintering

    International Nuclear Information System (INIS)

    Mussi, A.; Granger, G. Bernard; Addad, A.; Benameur, N.; Beclin, F.; Bataille, A.

    2009-01-01

    The distribution of inversion defects of Al was investigated in dense magnesium-aluminate spinel elaborated by pressureless sintering, pressureless sintering plus hot isostatic pressing, and spark plasma sintering. This study was conducted by energy electron loss spectroscopy analyses and more particularly by energy loss near edge structure investigations of the Al-L 2,3 edge. Several aspects are discussed with the purpose of understanding why charged defects dispersal reveals a special configuration.

  4. The effect of Cu addition and milling contaminations on the microstructure evolution of ball milled Al-Pb alloy during sintering

    International Nuclear Information System (INIS)

    Zhu, M.; Ouyang, L.Z.; Wu, Z.F.; Zeng, M.Q.; Li, Y.Y.; Zou, J.

    2006-01-01

    Al-10 wt.%Pb and Al-10 wt.%Pb-x wt.%Cu (x = 0-7.0) bulk alloys were prepared by sintering the mechanically alloyed powders at various temperatures. The microstructure changes of the as consolidated powders in the course of sintering were analyzed by differential scanning calorimetry, scanning electron microscopy, X-ray diffraction analysis and transmission electron microscopy. It has been found that, with respect to the Al-10 wt.%Pb-x wt.%Cu alloy, CuAl 2 and Cu 9 Al 4 phases formed in the milling process, and the amount of CuAl 2 phase increased while the Cu 9 Al 4 phase disappeared gradually in the sintering process. In both Al-10 wt.%Pb and Al-10 wt.%Pb-x wt.%Cu alloys, the sintering process results in the coarsening of Pb phase and the growth rate of Pb phase fulfills the Lifshitz-Slyozov-Wagner equation even though the size of the Pb phase was in nanometer range. The Pb particle exhibits cuboctahedral morphology and has a cubic to cubic orientation relationship with the Al matrix. The addition of Cu strongly depressed the growth rate of Pb. Contamination induced by milling has apparent influence on the microstructure of the sintered alloys. Al 7 Cu 2 Fe and aluminium oxide phases were identified in the sintered alloys. The cuboctahedral morphology of Pb particles was broken up by the presence of the oxide phase

  5. Characterization of In-Situ Cu–TiH2–C and Cu–Ti–C Nanocomposites Produced by Mechanical Milling and Spark Plasma Sintering

    Directory of Open Access Journals (Sweden)

    Nguyen Thi Hoang Oanh

    2017-03-01

    Full Text Available This study focuses on the fabrication and microstructural investigation of Cu–TiH2–C and Cu–Ti–C nanocomposites with different volume fractions (10% and 20% of TiC. Two mixtures of powders were ball milled for 10 h, consequently consolidated by spark plasma sintering (SPS at 900 and 1000 °C producing bulk materials with relative densities of 95–97%. The evolution process of TiC formation during sintering process was studied by using X-ray diffraction (XRD, scanning electron microscopy (SEM, and high resolution transmission electron microscopy (HRTEM. XRD patterns of composites present only Cu and TiC phases, no residual Ti phase can be detected. TEM images of composites with (10 vol % TiC sintered at 900 °C show TiC nanoparticles about 10–30 nm precipitated in copper matrix, most of Ti and C dissolved in the composite matrix. At the higher sintering temperature of 1000 °C, more TiC precipitates from Cu–TiH2–C than those of Cu–Ti–C composite, particle size ranges from 10 to 20 nm. The hardness of both nanocomposites also increased with increasing sintering temperature. The highest hardness values of Cu–TiH2–C and Cu–Ti–C nanocomposites sintered at 1000 °C are 314 and 306 HV, respectively.

  6. In situ oxidation state profiling of nickel hexacyanoferrate derivatized electrodes using line-imaging Raman spectroscopy and multivariate calibration

    International Nuclear Information System (INIS)

    Haight, S.M.; Schwartz, D.T.

    1999-01-01

    Metal hexacyanoferrate compounds show promise as electrochemically switchable ion exchange materials for use in the cleanup of radioactive wastes such as those found in storage basins and underground tanks at the Department of Energy's Hanford Nuclear Reservation. Reported is the use of line-imaging Raman spectroscopy for the in situ determination of oxidation state profiles in nickel hexacyanoferrate derivatized electrodes under potential control in an electrochemical cell. Line-imaging Raman spectroscopy is used to collect 256 contiguous Raman spectra every ∼5 microm from thin films (ca. 80 nm) formed by electrochemical derivatization of nickel electrodes. The cyanide stretching region of the Raman spectrum of the film is shown to be sensitive to iron oxidation state and is modeled by both univariate and multivariate correlations. Although both correlations fit the calibration set well, the multivariate (principle component regression or PCR) model's predictions of oxidation state are less sensitive to noise in the spectrum, yielding a much smoother oxidation state profile than the univariate model. Oxidation state profiles with spatial resolution of approximately 5 microm are shown for a nickel hexacyanoferrate derivatized electrode in reduced, intermediate, and oxidized states. In situ oxidation state profiles indicate that the 647.1 nm laser illumination photo-oxidizes the derivatized electrodes. This observation is confirmed using photoelectrochemical methods

  7. Comparison of Ti(C,N)-based cermets processed by hot-pressing sintering and conventional pressureless sintering

    International Nuclear Information System (INIS)

    Xu, Qingzhong; Ai, Xing; Zhao, Jun; Qin, Weizhen; Wang, Yintao; Gong, Feng

    2015-01-01

    Highlights: • The HP sintered Ti(C,N)-based cermets exhibit high hardness with fine grain size. • The PLS sintered cermets possess high mechanical properties with low porosity. • The applied pressure can rearrange particles and contribute to grain refinement. • The heating rate can greatly affect the solid and liquid phase sintering of cermets. - Abstract: A suitable sintering method is important to obtain the Ti(C,N)-based cermets with superior properties. In this paper, Ti(C,N)-based cermets were fabricated by hot-pressing sintering (HP) and conventional pressureless sintering (PLS) technology, respectively, to investigate the influence of different sintering methods on the microstructure and mechanical properties of cermets materials. The microstructure, fracture morphology, indention cracks and phase composition were observed and detected using scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The transverse rupture strength (TRS), Vickers hardness (HV) and fracture toughness (K IC ) were also measured. The results reveal that all of the Ti(C,N)-based cermets exhibit core–rim microstructures with black cores, white cores and grey rims embedded into metal binder phases. The grain size of the samples fabricated by HP is much finer and the structure is more compact than those fabricated by PLS, while there exist pores in the HP sintered samples. The sintering process has no influence on the phase composition of cermets, but affects the phase content and crystallinity. The samples fabricated by PLS present higher transverse rupture strength, fracture toughness and density than samples fabricated by HP. However, the HP sintered samples possess a higher hardness

  8. Sintering Process and Mechanical Property of MWCNTs/HDPE Bulk Composite.

    Science.gov (United States)

    Ming-Wen, Wang; Tze-Chi, Hsu; Jie-Ren, Zheng

    2009-08-01

    Studies have proved that increasing polymer matrices by carbon nanotubes to form structural reinforcement and electrical conductivity have significantly improved mechanical and electrical properties at very low carbon nanotubes loading. In other words, increasing polymer matrices by carbon nanotubes to form structural reinforcement can reduce friction coefficient and enhance anti-wear property. However, producing traditional MWCNTs in polymeric materix is an extremely complicated process. Using melt-mixing process or in situ polymerization leads to better dispersion effect on composite materials. In this study, therefore, to simplify MWCNTs /HDPE composite process and increase dispersion, powder was used directly to replace pellet to mix and sinter with MWCNTs. The composite bulks with 0, 0.5, 1, 2 and 4% nanotube content by weight was analyzed under SEM to observe nanotubes dispersion. At this rate, a MWCNTs/HDPE composite bulk with uniformly dispersed MWCNTs was achieved, and through the wear bench (Pin-on-Disk), the wear experiment has accomplished. Accordingly, the result suggests the sintered MWCNTs/HDPE composites amplify the hardness and wear-resist property.

  9. Expeditious low-temperature sintering of copper nanoparticles with thin defective carbon shells

    Science.gov (United States)

    Kim, Changkyu; Lee, Gyoungja; Rhee, Changkyu; Lee, Minku

    2015-04-01

    The realization of air-stable nanoparticles, well-formulated nanoinks, and conductive patterns based on copper is a great challenge in low-cost and large-area flexible printed electronics. This work reports the synthesis of a conductively interconnected copper structure via thermal sintering of copper inks at a low temperature for a short period of time, with the help of thin defective carbon shells coated onto the copper nanoparticles. Air-stable copper/carbon core/shell nanoparticles (typical size ~23 nm, shell thickness ~1.0 nm) are prepared by means of an electric explosion of wires. Gaseous oxidation of the carbon shells with a defective structure occurs at 180 °C, impacting the choice of organic solvents as well as the sintering conditions to create a crucial neck formation. Isothermal oxidation and reduction treatment at 200 °C for only about 10 min yields an oxide-free copper network structure with an electrical resistivity of 25.1 μΩ cm (14.0 μΩ cm at 250 °C). Finally, conductive copper line patterns are achieved down to a 50 μm width with an excellent printing resolution (standard deviation ~4.0%) onto a polyimide substrate using screen printing of the optimized inks.The realization of air-stable nanoparticles, well-formulated nanoinks, and conductive patterns based on copper is a great challenge in low-cost and large-area flexible printed electronics. This work reports the synthesis of a conductively interconnected copper structure via thermal sintering of copper inks at a low temperature for a short period of time, with the help of thin defective carbon shells coated onto the copper nanoparticles. Air-stable copper/carbon core/shell nanoparticles (typical size ~23 nm, shell thickness ~1.0 nm) are prepared by means of an electric explosion of wires. Gaseous oxidation of the carbon shells with a defective structure occurs at 180 °C, impacting the choice of organic solvents as well as the sintering conditions to create a crucial neck formation

  10. Production of sintered alumina from powder; optimization of the sinterized parameters for the maximum mechanical resistence

    International Nuclear Information System (INIS)

    Rocha, J.C. da.

    1981-02-01

    Pure, sinterized alumina and the optimization of the parameters of sinterization in order to obtain the highest mechanical resistence are discussed. Test materials are sinterized from a fine powder of pure alumina (Al 2 O 3 ), α phase, at different temperatures and times, in air. The microstructures are analysed concerning porosity and grain size. Depending on the temperature or the time of sinterization, there is a maximum for the mechanical resistence. (A.R.H.) [pt

  11. Microstructural comparison of effects of hafnium and titanium additions in spark-plasma-sintered Fe-based oxide-dispersion strengthened alloys

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Yina, E-mail: huangyina1981@hotmail.com [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); School of Electronic Science & Applied Physics, Hefei University of Technology, Hefei, Anhui 230009 (China); Zhang, Hongtao [Department of Materials, Loughborough University, Leicestershire, LE11 3TU (United Kingdom); Auger, Maria A.; Hong, Zuliang [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); Ning, Huanpo [School of Engineering of Materials Science, Queen Mary University of London, London, E1 4NS (United Kingdom); Nanoforce Technology Ltd, London, E1 4NS (United Kingdom); Gorley, Michael J. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); CCFE, Culham Science Centre, Abingdon, Oxon, OX14 3DB (United Kingdom); Grant, Patrick S. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); Reece, Michael J.; Yan, Haixue [School of Engineering of Materials Science, Queen Mary University of London, London, E1 4NS (United Kingdom); Nanoforce Technology Ltd, London, E1 4NS (United Kingdom); Roberts, Steve G. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); CCFE, Culham Science Centre, Abingdon, Oxon, OX14 3DB (United Kingdom)

    2017-04-15

    Two oxide dispersion strengthened alloys: 14Cr-0.25Y{sub 2}O{sub 3}-0.22Hf (wt.%) and Fe-14Cr-0.25Y{sub 2}O{sub 3}-0.4Ti (wt.%) were fabricated by mechanical alloying and subsequently consolidated by spark plasma sintering (SPS). Electron backscatter diffraction showed grain sizes in the range 0.5–15 μm in both alloys. Transmission electron microscopy and scanning transmission electron microscopy showed a homogeneous distribution of nano-oxides precipitated during SPS. Using high resolution transmission electron microscopy, energy dispersive X-ray spectroscopy and atom probe tomography, several different oxide phases were found in both alloys, but the majority of dispersoids were Y-Hf-O type in Fe-14Cr-0.25Y{sub 2}O{sub 3}-0.22Hf and Y-Ti-O type in Fe-14Cr-0.25Y{sub 2}O{sub 3}-0.4Ti. There were a variety of orientation relationships between the different dispersoids and the ferritic matrix. Both alloys had dispersoid densities of ∼10{sup 23}/m{sup 3}, with average diameters of 4.3 nm and 3.5 nm in the 0.22Hf and 0.4Ti containing alloys, respectively. Per atom added, Hf (0.07 at.%) is suggested to be more potent than Ti (0.46 at.%) in refining the nano-oxides.

  12. Guideline tests on the corrosion of sintered uranium oxide by lead and sodium about 450 deg. C; Essais d'orientation sur la corrosion de l'oxyde d'uranium fritte par le plomb et le sodium aux environs de 450 deg. C

    Energy Technology Data Exchange (ETDEWEB)

    Portnoff, A.; Pointud, R.

    1958-05-15

    Within the frame of the investigation of behaviour of a fuel element (such as UO{sub 2}) under irradiation, the authors report the study of the physical-chemical action of the coolant at different temperatures on the body to be irradiated. Thus, sintered uranium oxide has been submitted to corrosion by lead and by sodium during 250 hours at temperatures between 400 and 500 C. The physical characteristics of the UO{sub 2} powder and of different sintered UO{sub 2} pellets produced from this powder under different sintering processes are indicated, as well as the results of a spectrographic analysis of the sintered UO{sub 2}. Corrosion devices, treatments and obtained results are reported for corrosion by lead and by sodium. In the latter case, extraction processes are discussed (using butyl alcohol, or melting in vaseline oil)

  13. Analysis of wear in organic and sintered friction materials used in small wind energy converters

    Directory of Open Access Journals (Sweden)

    Jorge Alberto Lewis Esswein Junior

    2008-09-01

    Full Text Available Wind energy converters of small size used in isolated units to generate electrical energy must present low maintenance cost to such facilities economically viable. The aspect to be analyzed in cost reduction is the brake system, since in isolated systems the use of brake is more frequent reducing the brake pads life time. This study aims at analyzing the wear behavior of some materials used in brake pads. An organic material was analyzed comparing it with a commercial brake pad, and the sintered material was developed and tested. The materials behaviors were evaluated in both wear and friction coefficient. The sintered samples were made by powder metallurgy. The composition was compacted at 550 MPa and sintered in a furnace with controlled atmosphere to avoid oxidation. Despite the different compositions of the two types of materials, they presented a very similar wear; however, the sintered material presented a higher friction coefficient. An adjustment in the braking system of the wind generator might be proposed to use the sintered brake pad, due to its higher friction coefficient. Consequently, the braking action becomes lower, reducing the wear rate of the material.

  14. XPERT DESIGN AND DIAGNOSTICS' (XDD) IN-SITU CHEMICAL OXIDATION PROCESS USING POTASSIUM PERMANGANATE (KMNO4)

    Science.gov (United States)

    Xpert Design and Diagnostic's (XDD)potassium permanganate in situ chemical oxidation (ISCO) process was evaluated under the EPA Superfund Innovative Technology Evaluation (SITE) Program at the former MEC Building site located in Hudson, New Hampshire. At this site, both soil and ...

  15. Mixed oxide fuel pellet and manufacturing method thereof

    International Nuclear Information System (INIS)

    Yuda, Ryoichi; Ito, Ken-ichi; Masuda, Hiroshi.

    1993-01-01

    In a method of manufacturing nuclear fuel pellets which comprises compression molding a mixed oxide powder containing UO 2 and PuO 2 followed by sintering, a sintering agent having a composition comprising about 40 to 80 wt% of SiO 2 and the balance of Al 2 O 3 is mixed to a mixed oxide at a ratio of about 40ppm to about 0.5 wt% based on the total amount of the mixed oxide and the sintering agent, to prepare a mixture. The mixture is molded into a compression product and then sintered at a weakly acidic atmosphere at a temperature of about 1500degC to 1800degC. With such procedures, the sintering agent forms an eutectic product of a single liquid phase, PuO 2 is dispersed over the entire region of the pellet by way of the liquid phase, formation of a solid solution phase is promoted to annihilate a free PuO 2 phase. Further, growth of crystal grains is promoted. Accordingly, since the MOX fuel pellets prepared according to the present invention have a uniform solid solution state, and no free PuO 2 phase remains, increase of FP gas emission due to local nuclear fission of Pu can be avoided. (T.M.)

  16. Method for in situ carbon deposition measurement for solid oxide fuel cells

    Science.gov (United States)

    Kuhn, J.; Kesler, O.

    2014-01-01

    Previous methods to measure carbon deposition in solid oxide fuel cell (SOFC) anodes do not permit simultaneous electrochemical measurements. Electrochemical measurements supplemented with carbon deposition quantities create the opportunity to further understand how carbon affects SOFC performance and electrochemical impedance spectra (EIS). In this work, a method for measuring carbon in situ, named here as the quantification of gasified carbon (QGC), was developed. TGA experiments showed that carbon with a 100 h residence time in the SOFC was >99.8% gasified. Comparison of carbon mass measurements between the TGA and QGC show good agreement. In situ measurements of carbon deposition in SOFCs at varying molar steam/carbon ratios were performed to further validate the QGC method, and suppression of carbon deposition with increasing steam concentration was observed, in agreement with previous studies. The technique can be used to investigate in situ carbon deposition and gasification behavior simultaneously with electrochemical measurements for a variety of fuels and operating conditions, such as determining conditions under which incipient carbon deposition is reversible.

  17. Room Temperature Electrochemical Sintering of Zn Microparticles and Its Use in Printable Conducting Inks for Bioresorbable Electronics.

    Science.gov (United States)

    Lee, Yoon Kyeung; Kim, Jeonghyun; Kim, Yerim; Kwak, Jean Won; Yoon, Younghee; Rogers, John A

    2017-10-01

    This study describes a conductive ink formulation that exploits electrochemical sintering of Zn microparticles in aqueous solutions at room temperature. This material system has relevance to emerging classes of biologically and environmentally degradable electronic devices. The sintering process involves dissolution of a surface passivation layer of zinc oxide in CH 3 COOH/H 2 O and subsequent self-exchange of Zn and Zn 2+ at the Zn/H 2 O interface. The chemical specificity associated with the Zn metal and the CH 3 COOH/H 2 O solution is critically important, as revealed by studies of other material combinations. The resulting electrochemistry establishes the basis for a remarkably simple procedure for printing highly conductive (3 × 10 5 S m -1 ) features in degradable materials at ambient conditions over large areas, with key advantages over strategies based on liquid phase (fusion) sintering that requires both oxide-free metal surfaces and high temperature conditions. Demonstrations include printed magnetic loop antennas for near-field communication devices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Synthesis, vacuum sintering and dielectric characterization of zirconia (t-ZrO2) nanopowder

    International Nuclear Information System (INIS)

    Pazhani, R.; Padma Kumar, H.; Varghese, Angeo; Moses Ezhil Raj, A.; Solomon, Sam; Thomas, J.K.

    2011-01-01

    Highlights: → A single step auto-igniting combustion synthesis was employed for the preparation of nanocrystalline ZrO 2 . → Detailed structural analysis was carried out using XRD and FT-IR techniques. → Micro strain analysis of the asprepared nanocrystalline ZrO 2 was carried out. → A sintered density of above 98% of the theoretical value was obtained using vacuum sintering techniques. → The dielectric properties of vacuum sintered ZrO 2 were measured for a frequency range from 10 KHz to 10 MHz. - Abstract: Phase pure zirconium oxide powders have been synthesized using the single step auto-ignition combustion method, the particles were nanometer sized (20 nm) and the size distribution was very narrow (3.4 nm). Systematic structural characterization revealed the t-ZrO 2 and indexed for its tetragonal structure (a = 3.5975 A and c = 5.1649 A). Calculated microstrain in most of the plane indicated the presence of compressive stress (65-288 MPa) along various planes of the particles. Observed space group (P4 2 /nmc) revealed the presence of cations in the 8e positions (0.75, 0.25, 0.75) and the anions in the 16 h positions (0.25, 0.25, 0.4534). The metal-oxide (Zr-O) band observed at the low wavenumber region further confirmed the phase purity of the as-prepared ZrO 2 nanopowders. Peaks at the binding energy positions 2.042 and 0.525 keV in the energy dispersive X-ray spectrum revealed oxygen deficient zirconia. The particle size estimated by TEM was in good agreement with the results obtained through X-ray line broadening (20.81 nm) measurements. The nanopowders were sintered to above 98% of the theoretical density by using vacuum sintering technique at a relatively low temperature of 1300 deg. C. Stable tetragonal ZrO 2 experimentally yield the permittivity value of about 28 at 10 MHz.

  19. In Situ Spectroscopy and Mechanistic Insights into CO Oxidation on Transition-Metal-Substituted Ceria Nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Elias, Joseph S.; Stoerzinger, Kelsey A.; Hong, Wesley T.; Risch, Marcel; Giordano, Livia [Dipartimento; Mansour, Azzam N. [Naval; Shao-Horn, Yang

    2017-09-12

    Herein we investigate the reaction intermediates formed during CO oxidation on copper-substituted ceria nanoparticles (Cu0.1Ce0.9O2–x) by means of in situ spectroscopic techniques and identify an activity descriptor that rationalizes a trend with other metal substitutes (M0.1Ce0.9O2–x, M = Mn, Fe, Co, Ni). In situ X-ray absorption spectroscopy (XAS) performed under catalytic conditions demonstrates that O2– transfer occurs at dispersed copper centers, which are redox active during catalysis. In situ XAS reveals a dramatic reduction at the copper centers that is fully reversible under catalytic conditions, which rationalizes the high catalytic activity of Cu0.1Ce0.9O2–x. Ambient pressure X-ray photoelectron spectroscopy (AP-XPS) and in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) show that CO can be oxidized to CO32– in the absence of O2. We find that CO32– desorbs as CO2 only under oxygen-rich conditions when the oxygen vacancy is filled by the dissociative adsorption of O2. These data, along with kinetic analyses, lend support to a mechanism in which the breaking of copper–oxygen bonds is rate-determining under oxygen-rich conditions, while refilling the resulting oxygen vacancy is rate-determining under oxygen-lean conditions. On the basis of these observations and density functional calculations, we introduce the computed oxygen vacancy formation energy (Evac) as an activity descriptor for substituted ceria materials and demonstrate that Evac successfully rationalizes the trend in the activities of M0.1Ce0.9O2–x catalysts that spans three orders of magnitude. The applicability of Evac as a useful design descriptor is demonstrated by the catalytic performance of the ternary oxide Cu0.1La0.1Ce0.8O2–x, which has an apparent activation energy rivaling those of state-of-the-art Au/TiO2 materials. Thus, we suggest that cost-effective catalysts for CO oxidation can be rationally designed by judicious choice of substituting

  20. Effect of carbon and titanium carbide on sintering behaviour of zirconium diboride

    International Nuclear Information System (INIS)

    Mishra, S.K.; Pathak, L.C.

    2008-01-01

    Systematic sintering studies on the ZrB 2 powder were carried out with the addition of carbon (C) in the range of 0 2 . The addition of C also found to inhibit the grain size and fine grained ZrB 2 -C composite could be obtained with high densification. The increased densification with the C addition was due to removal of oxygen impurities on the ZrB 2 powder surfaces that prevented the commonly observed exaggerated grain growth through evaporation condensation of oxide phases during sintering of boride ceramics. At higher percentages of C addition, the densification rates decreased due to increased volume fraction of second phase that acted as diffusion barrier

  1. Development of an in-situ multi-component reinforced Al-based metal matrix composite by direct metal laser sintering technique — Optimization of process parameters

    International Nuclear Information System (INIS)

    Ghosh, Subrata Kumar; Bandyopadhyay, Kaushik; Saha, Partha

    2014-01-01

    In the present investigation, an in-situ multi-component reinforced aluminum based metal matrix composite was fabricated by the combination of self-propagating high-temperature synthesis and direct metal laser sintering process. The different mixtures of Al, TiO 2 and B 4 C powders were used to initiate and maintain the self-propagating high-temperature synthesis by laser during the sintering process. It was found from the X-ray diffraction analysis and scanning electron microscopy that the reinforcements like Al 2 O 3 , TiC, and TiB 2 were formed in the composite. The scanning electron microscopy revealed the distribution of the reinforcement phases in the composite and phase identities. The variable parameters such as powder layer thickness, laser power, scanning speed, hatching distance and composition of the powder mixture were optimized for higher density, lower porosity and higher microhardness using Taguchi method. Experimental investigation shows that the density of the specimen mainly depends upon the hatching distance, composition and layer thickness. On the other hand, hatching distance, layer thickness and laser power are the significant parameters which influence the porosity. The composition, laser power and layer thickness are the key influencing parameters for microhardness. - Highlights: • The reinforcements such as Al 2 O 3 , TiC, and TiB 2 were produced in Al-MMC through SHS. • The density is mainly influenced by the material composition and hatching distance. • Hatching distance is the major influencing parameter on porosity. • The material composition is the significant parameter to enhance the microhardness. • The SEM micrographs reveal the distribution of TiC, TiB 2 and Al 2 O 3 in the composite

  2. Oxide ceramics

    International Nuclear Information System (INIS)

    Ryshkewitch, E.; Richerson, D.W.

    1985-01-01

    The book explores single-phase ceramic oxide systems from the standpoint of physical chemistry and technology. This second edition also focuses on advances in technology since publication of the original edition. These include improvements in raw materials and forming and sintering techniques, and the major role that oxide ceramics have had in development of advanced products and processes. The text is divided into five major sections: general fundamentals of oxide ceramics, advances in aluminum oxide technology, advances in zirconia technology, and advances in beryllium oxide technology

  3. Status of Research on Selective Laser Sintering of Nanomaterials for Flexible Electronics Fabrication

    International Nuclear Information System (INIS)

    Ko, Seung Hwan

    2011-01-01

    A plastic-compatible low-temperature metal deposition and patterning process is essential for the fabrication of flexible electronics because they are usually built on a heat-sensitive flexible substrate, for example plastic, fabric, paper, or metal foil. There is considerable interest in solution-processible metal nanoparticle ink deposition and patterning by selective laser sintering. It provides flexible electronics fabrication without the use of conventional photolithography or vacuum deposition techniques. We summarize our recent progress on the selective laser sintering of metals and metal oxide nanoparticles on a polymer substrate to realize flexible electronics such as flexible displays and flexible solar cells. Future research directions are also discussed

  4. Sintering studies on iron-carbon-copper compacts

    Directory of Open Access Journals (Sweden)

    Perianayagam Philomen-D-Anand Raj

    2016-01-01

    Full Text Available Sintered Iron-Carbon-Copper parts are among the most widely used powder metallurgy product in automobile. In this paper, studies have been carried out to find out the sintering characteristics of iron-carbon-copper compacts when sintered in nitrogen atmosphere. The effects of various processing parameters on the sintering characteristics were studied. The various processing parameters considered were compaction pressure, green density and sintering temperature. The sintering characteristics determined were sintered density, porosity, dimensional change, micro hardness and radial crush strength. The results obtained have been discussed on the basis of micro structural observations. The characteristics of SEM fractography were also used to determine the mechanism of fracture. The fracture energy is strongly dependent on density of the compact.

  5. Preparation and characterization of amorphous SiO{sub 2} coatings deposited by mirco-arc oxidation on sintered NdFeB permanent magnets

    Energy Technology Data Exchange (ETDEWEB)

    Xu, J.L., E-mail: jlxu@nchu.edu.cn [Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001 (China); School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Xiao, Q.F.; Mei, D.D. [School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Zhong, Z.C., E-mail: zzhong2014@sina.com [The Institute for Rare Earth Magnetic Materials and Devices, Jiangxi University of Science and Technology, Ganzhou 341000 (China); Tong, Y.X. [Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001 (China); Zheng, Y.F., E-mail: yfzheng@pku.edu.cn [Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001 (China); Li, L. [Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001 (China)

    2017-03-15

    Amorphous SiO{sub 2} coatings were prepared on sintered NdFeB magnets by micro-arc oxidation (MAO) in silicate solution. The surface and cross-sectional morphologies, element and phase composition, corrosion resistance and magnetic properties of the coatings were investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectroscopy (XPS), potentiodynamic polarization test and physical properties measurements system (PPMS). The results showed that the surface morphologies of the coatings exhibited the “coral reef” like structure, different from the typical MAO porous structure. With increasing the voltages, the thickness of the coatings increased from 12.72 to 19.90 µm, the content of Si element increased, while the contents of Fe, Nd and P elements decreased. The coatings were mainly composed of amorphous SiO{sub 2} and a few amorphous Fe{sub 2}O{sub 3} and Nd{sub 2}O{sub 3}. The amorphous SiO{sub 2} coatings presented excellent thermal shock resistance, while the thermal shock resistance decreased with increasing the voltages. The corrosion resistance of the coatings increased with increasing the voltages, and it could be enhanced by one order of magnitude compared to the uncoated NdFeB magnets. The MAO coatings slightly decreased the magnetic properties of the NdFeB samples in different degrees. - Highlights: • Amorphous SiO{sub 2} coatings were prepared on sintered NdFeB magnets by micro-arc oxidation. • The coatings presented excellent thermal shock resistance. • The corrosion resistance could be enhanced by one order of magnitude. • The MAO coatings slightly decreased the magnetic properties of the NdFeB samples.

  6. Optimisation of Copper Oxide Impregnation on Carbonised Oil Palm Empty Fruit Bunch for Nitric Oxide Removal using Response Surface Methodology

    Science.gov (United States)

    Ahmad, Norhidayah; Yong, Sing Hung; Ibrahim, Naimah; Ali, Umi Fazara Md; Ridwan, Fahmi Muhammad; Ahmad, Razi

    2018-03-01

    Oil palm empty fruit bunch (EFB) was successfully modified with phosphoric acid hydration followed by impregnation with copper oxide (CuO) to synthesize CuO modified catalytic carbon (CuO/EFBC) for low-temperature removal of nitric oxide (NO) from gas streams. CuO impregnation was optimised through response surface methodology (RSM) using Box-Behnken Design (BBD) in terms of metal loading (5-20%), sintering temperature (200-800˚C) and sintering time (2-6 hours). The model response for the variables was NO adsorption capacity, which was obtained from an up-flow column adsorption experiment with 100 mL/min flow of 500 ppm NO/He at different operating conditions. The optimum operating variables suggested by the model were 20% metal loading, 200˚C sintering temperature and 6 hours sintering time. A good agreement (R2 = 0.9625) was achieved between the experimental data and model prediction. ANOVA analysis indicated that the model terms (metal loading and sintering temperature) are significant (Prob.>F less than 0.05).

  7. Optimisation of Copper Oxide Impregnation on Carbonised Oil Palm Empty Fruit Bunch for Nitric Oxide Removal using Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Ahmad Norhidayah

    2018-01-01

    Full Text Available Oil palm empty fruit bunch (EFB was successfully modified with phosphoric acid hydration followed by impregnation with copper oxide (CuO to synthesize CuO modified catalytic carbon (CuO/EFBC for low-temperature removal of nitric oxide (NO from gas streams. CuO impregnation was optimised through response surface methodology (RSM using Box-Behnken Design (BBD in terms of metal loading (5-20%, sintering temperature (200-800˚C and sintering time (2-6 hours. The model response for the variables was NO adsorption capacity, which was obtained from an up-flow column adsorption experiment with 100 mL/min flow of 500 ppm NO/He at different operating conditions. The optimum operating variables suggested by the model were 20% metal loading, 200˚C sintering temperature and 6 hours sintering time. A good agreement (R2 = 0.9625 was achieved between the experimental data and model prediction. ANOVA analysis indicated that the model terms (metal loading and sintering temperature are significant (Prob.>F less than 0.05.

  8. In situ investigation of ordering phase transformations in FePt magnetic nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Wittig, James E., E-mail: j.wittig@vanderbilt.edu [Interdisciplinary Materials Science, Vanderbilt University, PMB 351683, 2301 Vanderbilt Place, Nashville, TN 37232 (United States); Bentley, James, E-mail: bentleyj48@gmail.com [Materials Science and Technology Division, Oak Ridge National Laboratory, PO Box 2008, Oak Ridge, TN 37831-6376 (United States); Allard, Lawrence F., E-mail: allardlfjr@ornl.gov [Materials Science and Technology Division, Oak Ridge National Laboratory, PO Box 2008, Oak Ridge, TN 37831-6376 (United States)

    2017-05-15

    In situ high-resolution electron microscopy was used to reveal information at the atomic level for the disordered-to-ordered phase transformation of equiatomic FePt nanoparticles that can exhibit outstanding magnetic properties after transforming from disordered face-centered-cubic into the tetragonal L1{sub 0} ordered structure. High-angle annular dark-field imaging in the scanning transmission electron microscope provided sufficient contrast between the Fe and Pt atoms to readily monitor the ordering of the atoms during in situ heating experiments. However, during continuous high-magnification imaging the electron beam influenced the kinetics of the transformation so annealing had to be performed with the electron beam blanked. At 500 °C where the reaction rate was relatively slow, observation of the transformation mechanisms using this sequential imaging protocol revealed that ordering proceeded from (002) surface facets but was incomplete and multiple-domain particles were formed that contained anti-phase domain boundaries and anti-site defects. At 600 and 700 °C, the limitations of sequential imaging were revealed as a consequence of increased transformation kinetics. Annealing for only 5 min at 700 °C produced complete single-domain L1{sub 0} order; such single-domain particles were more spherical in shape with (002) facets. The in situ experiments also provided information concerning nanoparticle sintering, coalescence, and consolidation. Although there was resistance to complete sintering due to the crystallography of L1{sub 0} order, the driving force from the large surface-area-to-volume ratio resulted in considerable nanoparticle coalescence, which would render such FePt nanoparticles unsuitable for use as magnetic recording media. Comparison of the in situ data acquired using the protocol described above with parallel ex situ annealing experiments showed that identical behavior resulted in all cases. - Highlights: • HAADF STEM imaging reveals the

  9. Tungsten and molybdenum with oxide dispersion, production and properties

    International Nuclear Information System (INIS)

    Haerdtle, S.; Schmidberger, R.

    1989-01-01

    By the reaction spray process metal powders with dispersed metal oxides can be produced in one step. The systems investigated here are tungsten and molybdenum with 0,5% resp. 5% La 2 O 3 , Y 2 O 3 and ZrO 2 . The oxides with diameters below 0,5μm are finely dispersed within the metal powder particles. The sinterability of the powders depends on the oxide content. Maximum density at an oxide content of 0,5% is about 96% at a sintering temperature of 1600 0 C. The type of oxide influences the densification versus temperature but not the final density. 5 refs., 11 figs. (Author)

  10. Fabrication of Cr-doped UO2 Fuel Pellet using Liquid Phase Sintering

    International Nuclear Information System (INIS)

    Kim, Dong Joo; Yang, Jae Ho; Kim, Keon Sik; Rhee, Young Woo; Kim, Jong Hun; Oh, Jang Soo; Koo, Yang Hyun

    2013-01-01

    An enhancement of the thermal conductivity of a pellet can be obtained by the addition of a higher thermal conductive material in the pellet. In addition, the resistance to the PCI can be increased through a plasticity increase of the pellet. Thermal conductivity of ceramic materials is generally lower than that of metallic materials. The thermal conductivity of uranium oxide which is a typical ceramic material is low as well. The steep temperature gradient in the fuel pellet results from the low thermal conductivity. Therefore, the thermal conductivity improvement of a nuclear fuel pellet can enhance the fuel performance in various aspects. The lower centerline temperature of a fuel pellet affects the enhancement of fuel safety as well as fuel pellet integrity during nuclear reactor operation. Besides, the nuclear reactor power can be uprated due to the higher safety margin. So, many researches to enhance the thermal conductivity of nuclear fuel pellet have been performed in various ways. To improve the thermal conductivity of UO 2 pellet, an appropriate arrangement of the high thermal conductive material in UO 2 matrix is one of the various methods. We intended to control a placement of chromium as the high thermal conductive material. The metallic chromium and chromium oxide were arranged in a grain boundary of UO 2 using a liquid phase sintering method. The liquid phase sintering of Cr-doped UO 2 pellet could be adjusted using a control of an oxygen potential in sintering atmosphere

  11. Design of Magnetic Gelatine/Silica Nanocomposites by Nanoemulsification: Encapsulation versus in Situ Growth of Iron Oxide Colloids

    Directory of Open Access Journals (Sweden)

    Joachim Allouche

    2014-07-01

    Full Text Available The design of magnetic nanoparticles by incorporation of iron oxide colloids within gelatine/silica hybrid nanoparticles has been performed for the first time through a nanoemulsion route using the encapsulation of pre-formed magnetite nanocrystals and the in situ precipitation of ferrous/ferric ions. The first method leads to bi-continuous hybrid nanocomposites containing a limited amount of well-dispersed magnetite colloids. In contrast, the second approach allows the formation of gelatine-silica core-shell nanostructures incorporating larger amounts of agglomerated iron oxide colloids. Both magnetic nanocomposites exhibit similar superparamagnetic behaviors. Whereas nanocomposites obtained via an in situ approach show a strong tendency to aggregate in solution, the encapsulation route allows further surface modification of the magnetic nanocomposites, leading to quaternary gold/iron oxide/silica/gelatine nanoparticles. Hence, such a first-time rational combination of nano-emulsion, nanocrystallization and sol-gel chemistry allows the elaboration of multi-component functional nanomaterials. This constitutes a step forward in the design of more complex bio-nanoplatforms.

  12. In-situ sequential laser transfer and laser reduction of graphene oxide films

    Science.gov (United States)

    Papazoglou, S.; Petridis, C.; Kymakis, E.; Kennou, S.; Raptis, Y. S.; Chatzandroulis, S.; Zergioti, I.

    2018-04-01

    Achieving high quality transfer of graphene on selected substrates is a priority in device fabrication, especially where drop-on-demand applications are involved. In this work, we report an in-situ, fast, simple, and one step process that resulted in the reduction, transfer, and fabrication of reduced graphene oxide-based humidity sensors, using picosecond laser pulses. By tuning the laser illumination parameters, we managed to implement the sequential printing and reduction of graphene oxide flakes. The overall process lasted only a few seconds compared to a few hours that our group has previously published. DC current measurements, X-Ray Photoelectron Spectroscopy, X-Ray Diffraction, and Raman Spectroscopy were employed in order to assess the efficiency of our approach. To demonstrate the applicability and the potential of the technique, laser printed reduced graphene oxide humidity sensors with a limit of detection of 1700 ppm are presented. The results demonstrated in this work provide a selective, rapid, and low-cost approach for sequential transfer and photochemical reduction of graphene oxide micro-patterns onto various substrates for flexible electronics and sensor applications.

  13. In situ chemical oxidative polymerization preparation of poly(3,4-ethylenedioxythiophene)/graphene nanocomposites with enhanced thermoelectric performance.

    Science.gov (United States)

    Xu, Kongli; Chen, Guangming; Qiu, Dong

    2015-05-01

    Three different in situ chemical oxidative polymerization routes, that is, (A) spin-coating and subsequent liquid layer polymerization, (B) spin-coating followed by vapor phase polymerization, and (C) in situ polymerization and then post-treatment by immersion in ethylene glycol (EG), have been developed to achieve poly(3,4-ethylenedioxythiophene)/reduced graphene oxide (PEDOT/rGO) nanocomposites. As demonstrated by scanning electron microscopic and energy-dispersive X-ray spectroscopic techniques, PEDOT has been successfully coated on the surface of the rGO nanosheets by each of the three preparation routes. Importantly, all of the nanocomposites display a greatly enhanced thermoelectric performance (power factors) relative to those of the corresponding neat PEDOT. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Investigation of the sintering mechanisms for (U,Am)O{sub 2} pellets obtained by CRMP process

    Energy Technology Data Exchange (ETDEWEB)

    Caisso, M. [CEA, Centre de Marcoule, DEN, DTEC/SECA/LFC, F-30207 Bagnols-sur-Ceze (France); CEA, Centre de Marcole, DEN, DRCP/SERA/LCAR, F-30207 Bagnols-sur-Ceze (France); Institut Europeen des Membranes, UMR 5635 CNRS-ENSCM-UM, CC047, Campus Triolet, Universite de Montpellier, F-34095 Montpellier Cedex 5 (France); Boulesteix, R.; Maitre, A. [SPCTS, UMR 7315 CNRS-Universite de Limoges-ENSCI, Centre Europeen de la Ceramique, 12 Rue Atlantis, F-87068 Limoges (France); Picart, S.; Delahaye, T. [CEA, Centre de Marcole, DEN, DRCP/SERA/LCAR, F-30207 Bagnols-sur-Ceze Cedex (France); Ayral, A. [Institut Europeen des Membranes, UMR 5635 CNRS-ENSCM-UM, CC047, Campus Triolet Universite de Montpellier, F-34095 Montpellier Cedex 5 (France)

    2016-07-01

    The use of CRMP (Calcined Resin Microsphere Pelletization) process for AmBB (Americium Bearing Blankets) fabrication is today a key research axis in americium transmutation domain, where its very high activity requires minimization of powder dissemination. In this aim, the use of oxide microspheres as compaction precursors is a promising clean alternative to powder metallurgy. Understanding the different steps of densification during CRMP pellet sintering thus appears as fundamental to obtain final materials with the specific features required for AmBB. The densification curve recorded in dynamic conditions shows different sintering steps. A first decrease of shrinkage rate happens at low temperature, around 1100 K. This phenomenon is not normally observed in the sintering of conventional powders. Chemical and microstructural studies were performed on (U,Am)O{sub 2} and also on (Ce,Gd)O{sub 2} surrogate compound to highlight the causes of this low-temperature sintering step. Multi-scale reorganization finally appears as the sole explanation, through the sintering of nano-metric aggregate present in the green pellet and related to the morphology of the starting microspheres employed as pelletization precursors. (authors)

  15. Studies on frequency dependent electrical and dielectric properties of sintered zinc oxide pellets: effects of Al-doping

    Science.gov (United States)

    Tewari, S.; Ghosh, A.; Bhattacharjee, A.

    2016-11-01

    Sintered pellets of zinc oxide (ZnO), both undoped and Al-doped are prepared through a chemical process. Dopant concentration of Aluminium in ZnO [Al/Zn in weight percentage (wt%)] is varied from 0 to 3 wt%. After synthesis structural characterisation of the samples are performed with XRD and SEM-EDAX which confirm that all the samples are of ZnO having polycrystalline nature with particle size from 108.6 to 116 nm. Frequency dependent properties like a.c. conductivity, capacitance, impedance and phase angle are measured in the frequency range 10 Hz to 100 kHz as a function of temperature (in the range 25-150 °C). Nature of a.c. conductivity in these samples indicates hopping type of conduction arising from localised defect states. The frequency and temperature dependent properties under study are found to be as per correlated barrier hoping model. Dielectric and impedance properties studied in the samples indicate distributed relaxation, showing decrease of relaxation time with temperature.

  16. Study and fabrication of solid oxide fuel cells through tape casting and co-sintering; Etude et realisation par coulage en bande et co-frittage de cellules de pile a combustible a oxydes solides

    Energy Technology Data Exchange (ETDEWEB)

    Grosjean, A

    2004-11-15

    This work is dedicated to the devising of a low-cost fabrication process of solid oxide fuel cells (SOFC). Technical requirements impose the shaping method: stripe casting as well as the materials used: Yttria-stabilized zirconia (YSZ), nickel and lanthanum manganite doped with strontium (LSM). In order to comply with environmental requirements the developed process uses an aqueous barbotine solvent. We get electrodes and the electrolyte separately, the use of an absorbent drying process has enabled us to join 3 layers to form an elementary cell with great interfacial homogeneity. The resistance of the cell to sintering has been improved through the symmetrization of the deformations of the cell. In order to interpret the low electrical properties of the cell and its quick damaging, transmission microscopy studies have been performed. These studies have shown 2 facts. First, 2 isolating phases appear at the cathode (at the LSM/YSZ interface) because of a too high sintering temperature and secondly, a quick clustering of nickel grains appears during cell operation that leads to a local loss of the nickel grid percolation. This problem has been solved by increasing the size of nickel oxide grains from 0.5 {mu}m to 3 {mu}m) to stabilize the microstructure. The issue of the reactivity at the LSM/YSZ interfaces was tackled in 2 different ways, we have tried to lower the sintering temperature by using a zirconia nano-powder first and then by replacing zirconia in the electrolyte by gadolinium-doped ceria. The use of zirconia nano-powder has failed to decrease sintering temperature while preserving the electrolyte density and the use of ceria has triggered instabilities that have not yet been solved. Despite all these drawbacks, this process allows the fabrication of an excellent anode/electrolyte interface. (A.C.)

  17. Effect Of SiC Particles On Sinterability Of Al-Zn-Mg-Cu P/M Alloy

    Directory of Open Access Journals (Sweden)

    Rudianto H.

    2015-06-01

    Full Text Available Premix Al-5.5Zn-2.5Mg-0.5Cu alloy powder was analyzed as matrix in this research. Gas atomized powder Al-9Si with 20% volume fraction of SiC particles was used as reinforcement and added into the alloy with varied concentration. Mix powders were compacted by dual action press with compaction pressure of 700 MPa. High volume fraction of SiC particles gave lower green density due to resistance of SiC particles to plastic deformation during compaction process and resulted voids between particles and this might reduce sinterability of this mix powder. Sintering was carried out under ultra high purity nitrogen gas from 565°-580°C for 1 hour. High content of premix Al-5.5Zn-2.5Mg-0.5Cu alloy powder gave better sintering density and reached up to 98% relative. Void between particles, oxide layer on aluminum powder and lower wettability between matrix and reinforcement particles lead to uncompleted liquid phase sintering, and resulted on lower sintering density and mechanical properties on powder with high content of SiC particles. Mix powder with wt90% of Alumix 431D and wt10% of Al-9Si-vf20SiC powder gave higher tensile strength compare to another mix powder for 270 MPa. From chemical compositions, sintering precipitates might form after sintering such as MgZn2, CuAl2 and Mg2Si. X-ray diffraction, DSC-TGA, and SEM were used to characterize these materials.

  18. Synthesis of lithium nickel cobalt manganese oxide cathode materials by infrared induction heating

    Science.gov (United States)

    Hsieh, Chien-Te; Chen, Yu-Fu; Pai, Chun-Ting; Mo, Chung-Yu

    2014-12-01

    This study adopts an in-situ infrared (IR) sintering incorporated with carbonization technique to synthesize carbon-coated LiNi1/3Co1/3Mn1/3O2 (LNCM) cathode materials for Li-ion batteries. Compared with electric resistance heating, the in-situ IR sintering is capable of rapidly producing highly-crystalline LNCM powders at 900 °C within a short period, i.e., 3 h in this case. Glucose additive is employed to serve a carbon precursor, which is carbonized and coated over the surface of LNCM crystals during the IR sintering process. The electrochemical performance of LNCM cathodes is well examined by charge-discharge cycling at 0.1-5C. An appropriate carbon coating is capable of raising discharge capacity (i.e., 181.5 mAh g-1 at 0.1C), rate capability (i.e., 75.0 mAh g-1 at 5C), and cycling stability (i.e., capacity retention: 94.2% at 1C after 50 cycles) of LNCM cathodes. This enhanced performance can be ascribed to the carbon coating onto the external surface of LNCM powders, creating an outer circuit of charge-transfer pathway and preventing cathode corrosion from direct contact to the electrolyte. Accordingly, the in-situ IR sintering technique offers a potential feasibility for synthesizing cathode materials commercially in large scale.

  19. Pressureless sintering of whisker-toughened ceramic composites

    Science.gov (United States)

    Tiegs, T.N.

    1993-05-04

    A pressureless sintering method is disclosed for use in the production of whisker-toughened ceramic composites wherein the sintered density of composites containing up to about 20 vol. % SiC whiskers is improved by reducing the average aspect ratio of the whiskers to from about 10 to about 20. Sintering aids further improve the density, permitting the production of composites containing 20 vol. % SiC with sintered densities of 94% or better of theoretical density by a pressureless sintering method.

  20. Influence of sintering temperature on mechanical properties of spark plasma sintered pre-alloyed Ti-6Al-4 V powder

    Energy Technology Data Exchange (ETDEWEB)

    Muthuchamy, A.; Patel, Paridh; Rajadurai, M. [VIT Univ., Vellore, Tamil Nadu (India); Chaurisiya, Jitendar K. [NIT, Suratkal (India); Annamalai, A. Raja [VIT Univ., Vellore, Tamil Nadu (India). Centre for Innovative Manufacturing Research

    2018-04-01

    Spark plasma sintering provides faster heating that can create fully, or near fully, dense samples without significant grain growth. In this study, pre-alloyed Ti-6Al-4 V powder compact samples produced through field assisted sintering in a spark plasma sintering machine are compared as a function of consolidation temperature. The effect of sintering temperature on the densification mechanism, microstructural evolution and mechanical properties of spark plasma sintered Ti-6Al-4 V alloy compacts was investigated in detail. The compact, sintered at 1100 C, exhibited near net density, highest hardness and strength as compared to the other compacts processed at a temperature lower than 1100 C.

  1. Analysis of the conductivity of commercial easy sintering grade 3 mol% Y{sub 2}O{sub 3}-ZrO{sub 2} materials

    Energy Technology Data Exchange (ETDEWEB)

    Badwal, Sukhvinder P.S.; Ciacchi, Fabio T.; Giampietro, Kristine M. [CSIRO, Manufacturing and Infrastructure Technology, Private Bag 33, Clayton South 3169, Victoria (Australia)

    2005-01-14

    Fine grain zirconia-yttria materials are required for enhanced performance in solid oxide fuel cells and related devices and in applications requiring good thermo-mechanical properties. Materials with about 3 mol% Y{sub 2}O{sub 3}-ZrO{sub 2} composition are good electrolyte materials for solid oxide fuel cell, ceramic membrane oxygen separation and a number of related devices because of their superior mechanical properties and ease of fabrication into thin self-supporting structures in comparison with a material in the 8-10 mol% Y{sub 2}O{sub 3}-ZrO{sub 2} composition range. In this study, sintering behaviour, impedance studies, four-probe DC conductivity measurements and microstructure analysis has been performed on various easy sintering grade materials from two commercial powder suppliers. These materials achieve near theoretical density at sintering temperatures as low as 1350-1400C. For direct comparison of the conductivity and impedance behaviour in easy sintering grade materials, several other 3 mol% Y{sub 2}O{sub 3}-ZrO{sub 2} powders were also investigated. The total ionic conductivity at 850C in easy sintering grade materials is comparable with normal-grade commercial materials of similar composition despite a slightly higher grain boundary impedance at lower temperatures (below circa 450C). There were no obvious differences in the grain boundary thickness, calculated from the impedance data, of normal and easy sintering grade materials.

  2. Laser sintering of metal powders on top of sintered layers under multiple-line laser scanning

    International Nuclear Information System (INIS)

    Xiao Bin; Zhang Yuwen

    2007-01-01

    A three-dimensional numerical model for multiple-line sintering of loose powders on top of multiple sintered layers under the irradiation of a moving Gaussian laser beam is carried out. The overlaps between vertically deposited layers and adjacent lines which strengthen bonding are taken into account. The energy equation is formulated using the temperature transforming model and solved by the finite volume method. The effects of the number of the existing sintered layers, porosity and initial temperature coupled with the optimal combination laser intensity and scanning velocity are presented. The results show that the liquid pool moves slightly towards the negative scanning direction and the shape of the liquid pool becomes shallower with higher scanning velocity. A higher laser intensity is needed to achieve the required overlaps when the number of the existing sintered layers increases. Increasing porosity or initial temperature enhances the sintering process and thus less intensity is needed for the overlap requirement

  3. Full densification of inkjet-printed copper conductive tracks on a flexible substrate utilizing a hydrogen plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Kwon, Young-Tae [Department of Fusion Chemical Engineering, Hanyang University, Ansan 15588 (Korea, Republic of); Lee, Young-In [Department of Materials Science and Engineering, Seoul National University of Science and Technology, Seoul 01811 (Korea, Republic of); Kim, Seil [Department of Fusion Chemical Engineering, Hanyang University, Ansan 15588 (Korea, Republic of); Lee, Kun-Jae [Department of Energy Engineering, Dankook University, Cheonan 31116 (Korea, Republic of); Choa, Yong-Ho, E-mail: choa15@hanyang.ac.kr [Department of Fusion Chemical Engineering, Hanyang University, Ansan 15588 (Korea, Republic of)

    2017-02-28

    Highlights: • Hydrogen thermally- and plasma- treatments are applied to reduce and sinter the inkjet-printed copper patterns at low temperature. • Plasma sintered Cu patterns have fully densified microstructure with the resistivity of 3.23 μW cm. • Cu conductive track with dense microstructure remains its electrical resistivity after 1 month. • Thermal sintered Cu patterns show a relatively poor microstructure and high resistivity. - Abstract: Low temperature sintering techniques are crucial in developing flexible printed electronics. In this work, we demonstrate a novel hydrogen plasma sintering method that achieves a full reduction and densification of inkjet-printed patterns using a copper complex ion ink. After inkjet printing on polyethylene terephthalate (PET) substrates, both hydrogen plasma and conventional hydrogen thermal treatment were employed to compare the resulting microstructures, electrical properties and anti-oxidation behavior. The plasma treated pattern shows a fully densified microstructure with a resistivity of 3.23 μΩ cm, while the thermally treated pattern shows a relatively poor microstructure and high resistivity. In addition, the hydrogen plasma-treated copper pattern retains its electrical resistivity for one month without any significant decrease. This novel hydrogen plasma sintering technique could be used to produce conductive patterns with excellent electrical properties, allowing for highly reliable flexible printed electronics.

  4. Oriented Arrays of Graphene in a Polymer Matrix by in situ Reduction of Graphite Oxide Nanosheets

    KAUST Repository

    Ansari, Seema; Kelarakis, Antonios; Estevez, Luis; Giannelis, Emmanuel P.

    2010-01-01

    Graphite oxide-Nafion hybrids with a high degree of alignment are cast from aqueous solution in the absence of any external field and reduced in situ by exposure to hydrazine to produce graphene-Nafion hybrids. Dramatic enhancement of electrical

  5. Structural Investigation of Sodium Layered Oxides Via in Situ Synchrotron X-Ray Diffraction

    DEFF Research Database (Denmark)

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

    2015-01-01

    electrochemical reaction is generally considered to be a pivotal feature for understanding the relationship between layered structures and electrochemical properties. Here the structure, phase stability, and electrochemical properties of two kinds of layered oxides, P2 and O3, are investigated through in......-situ synchrotron XRD experiments. A capillary Na-based cell is designed to minimize interference in other substances such as a separator or external battery parts. This approach could give us to obtain clear diffraction patterns with high intensity during electrochemical reaction in a short period of time without...... further relaxation step. We carefully scrutinized reversible structural phase transformations during electrochemical reaction of P2 and O3-layered compounds based on in situ analysis, and detailed results will be discussed....

  6. In-situ XPS analysis of oxidized and reduced plasma deposited ruthenium-based thin catalytic films

    Science.gov (United States)

    Balcerzak, Jacek; Redzynia, Wiktor; Tyczkowski, Jacek

    2017-12-01

    A novel in-situ study of the surface molecular structure of catalytically active ruthenium-based films subjected to the oxidation (in oxygen) and reduction (in hydrogen) was performed in a Cat-Cell reactor combined with a XPS spectrometer. The films were produced by the plasma deposition method (PEMOCVD). It was found that the films contained ruthenium at different oxidation states: metallic (Ru0), RuO2 (Ru+4), and other RuOx (Ru+x), of which content could be changed by the oxidation or reduction, depending on the process temperature. These results allow to predict the behavior of the Ru-based catalysts in different redox environments.

  7. In situ spectroscopic monitoring of CO2 reduction at copper oxide electrode.

    Science.gov (United States)

    Wang, Liying; Gupta, Kalyani; Goodall, Josephine B M; Darr, Jawwad A; Holt, Katherine B

    2017-04-28

    Copper oxide modified electrodes were investigated as a function of applied electrode potential using in situ infrared spectroscopy and ex situ Raman and X-ray photoelectron spectroscopy. In deoxygenated KHCO 3 electrolyte bicarbonate and carbonate species were found to adsorb to the electrode during reduction and the CuO was reduced to Cu(i) or Cu(0) species. Carbonate was incorporated into the structure and the CuO starting material was not regenerated on cycling to positive potentials. In contrast, in CO 2 saturated KHCO 3 solution, surface adsorption of bicarbonate and carbonate was not observed and adsorption of a carbonato-species was observed with in situ infrared spectroscopy. This species is believed to be activated, bent CO 2 . On cycling to negative potentials, larger reduction currents were observed in the presence of CO 2 ; however, less of the charge could be attributed to the reduction of CuO. In the presence of CO 2 CuO underwent reduction to Cu 2 O and potentially Cu, with no incorporation of carbonate. Under these conditions the CuO starting material could be regenerated by cycling to positive potentials.

  8. Sintered indium-tin oxide particles induce pro-inflammatory responses in vitro, in part through inflammasome activation.

    Directory of Open Access Journals (Sweden)

    Melissa A Badding

    Full Text Available Indium-tin oxide (ITO is used to make transparent conductive coatings for touch-screen and liquid crystal display electronics. As the demand for consumer electronics continues to increase, so does the concern for occupational exposures to particles containing these potentially toxic metal oxides. Indium-containing particles have been shown to be cytotoxic in cultured cells and pro-inflammatory in pulmonary animal models. In humans, pulmonary alveolar proteinosis and fibrotic interstitial lung disease have been observed in ITO facility workers. However, which ITO production materials may be the most toxic to workers and how they initiate pulmonary inflammation remain poorly understood. Here we examined four different particle samples collected from an ITO production facility for their ability to induce pro-inflammatory responses in vitro. Tin oxide, sintered ITO (SITO, and ventilation dust particles activated nuclear factor kappa B (NFκB within 3 h of treatment. However, only SITO induced robust cytokine production (IL-1β, IL-6, TNFα, and IL-8 within 24 h in both RAW 264.7 mouse macrophages and BEAS-2B human bronchial epithelial cells. Our lab and others have previously demonstrated SITO-induced cytotoxicity as well. These findings suggest that SITO particles activate the NLRP3 inflammasome, which has been implicated in several immune-mediated diseases via its ability to induce IL-1β release and cause subsequent cell death. Inflammasome activation by SITO was confirmed, but it required the presence of endotoxin. Further, a phagocytosis assay revealed that pre-uptake of SITO or ventilation dust impaired proper macrophage phagocytosis of E. coli. Our results suggest that adverse inflammatory responses to SITO particles by both macrophage and epithelial cells may initiate and propagate indium lung disease. These findings will provide a better understanding of the molecular mechanisms behind an emerging occupational health issue.

  9. In situ functionalization and PEO coating of iron oxide nanocrystals using seeded emulsion polymerization.

    Science.gov (United States)

    Kloust, Hauke; Schmidtke, Christian; Feld, Artur; Schotten, Theo; Eggers, Robin; Fittschen, Ursula E A; Schulz, Florian; Pöselt, Elmar; Ostermann, Johannes; Bastús, Neus G; Weller, Horst

    2013-04-16

    Herein we demonstrate that seeded emulsion polymerization is a powerful tool to produce multiply functionalized PEO coated iron oxide nanocrystals. Advantageously, by simple addition of functional surfactants, functional monomers, or functional polymerizable linkers-solely or in combinations thereof-during the seeded emulsion polymerization process, a broad range of in situ functionalized polymer-coated iron oxide nanocrystals were obtained. This was demonstrated by purposeful modulation of the zeta potential of encapsulated iron oxide nanocrystals and conjugation of a dyestuff. Successful functionalization was unequivocally proven by TXRF. Furthermore, the spatial position of the functional groups can be controlled by choosing the appropriate spacers. In conclusion, this methodology is highly amenable for combinatorial strategies and will spur rapid expedited synthesis and purposeful optimization of a broad scope of nanocrystals.

  10. In situ characterization of uranium and americium oxide solid solution formation for CRMP process: first combination of in situ XRD and XANES measurements.

    Science.gov (United States)

    Caisso, Marie; Picart, Sébastien; Belin, Renaud C; Lebreton, Florent; Martin, Philippe M; Dardenne, Kathy; Rothe, Jörg; Neuville, Daniel R; Delahaye, Thibaud; Ayral, André

    2015-04-14

    Transmutation of americium in heterogeneous mode through the use of U1-xAmxO2±δ ceramic pellets, also known as Americium Bearing Blankets (AmBB), has become a major research axis. Nevertheless, in order to consider future large-scale deployment, the processes involved in AmBB fabrication have to minimize fine particle dissemination, due to the presence of americium, which considerably increases the risk of contamination. New synthesis routes avoiding the use of pulverulent precursors are thus currently under development, such as the Calcined Resin Microsphere Pelletization (CRMP) process. It is based on the use of weak-acid resin (WAR) microspheres as precursors, loaded with actinide cations. After two specific calcinations under controlled atmospheres, resin microspheres are converted into oxide microspheres composed of a monophasic U1-xAmxO2±δ phase. Understanding the different mechanisms during thermal conversion, that lead to the release of organic matter and the formation of a solid solution, appear essential. By combining in situ techniques such as XRD and XAS, it has become possible to identify the key temperatures for oxide formation, and the corresponding oxidation states taken by uranium and americium during mineralization. This paper thus presents the first results on the mineralization of (U,Am) loaded resin microspheres into a solid solution, through in situ XAS analysis correlated with HT-XRD.

  11. Studies on the sintering of copper powder compacts

    International Nuclear Information System (INIS)

    Elmasry, M.A.A.; Abadir, M.F.; Mahdy, A.N.; Elkinawy, W.S.

    1995-01-01

    Solid state sintering behavior of cylindrical compacts, (1 cm diameter and 1 cm height), made of copper powder was studied within a range of compacting pressure of 75 up to 300 MPa, sintering temperature of 600 up to to 900 degree C, and sintering time of 5 up to 60 min in a reducing atmosphere composed of H2 and N 2 gases with a volumetric ratio 3:1. The green and the sintered densities were found to to increase with the compacting pressure. Higher sintering temperature, and time favour increased sintered density. probable mechanisms during the initial stage of sintering were disclosed. It was found that low pressures cause dilation of closed pores, and vice versa. At low pressures and temperatures the surface diffusion mechanism is favoured, While high temperatures favour lattice diffusion mechanism. at high pressures, the lattice diffusion mechanism is suppressed while surface diffusion predominates. Density and hence shrinkage were also found to increase with the increase of sintering time, While its rate increases with the increase of sintering temperature. the influence of sintering conditions on the hardness of the compacts was studied. An increase in hardness, When higher compacting pressures and higher sintering temperatures were adopted, has bee obtained. 11 figs

  12. Multiple recycling of NdFeB-type sintered magnets

    Energy Technology Data Exchange (ETDEWEB)

    Zakotnik, M. [Department of Metallurgy and Materials, University of Birmingham, Edgbaston, Birmingham B15 2TT (United Kingdom)], E-mail: miha.zakotnik@gmail.com; Harris, I.R.; Williams, A.J. [Department of Metallurgy and Materials, University of Birmingham, Edgbaston, Birmingham B15 2TT (United Kingdom)

    2009-02-05

    Some fully dense, sintered NdFeB-type magnets (employed in VCM disc drives) have been subjected to a recycling process using the hydrogen decrepitation (HD) process. After a brief milling treatment, the powder was aligned, pressed and re-sintered and this procedure was repeated four times with a progressive fall in the density and in the magnetic properties. The chemical analysis indicated that this was due to the progressive oxidation of the Nd-rich material and to some Nd loss by evaporation. The procedure was then repeated but with the addition (blending) of a fine powder of neodymium hydride after the first cycle. It was found that the addition of 1 at.% of neodymium at each stage was sufficient to maintain the density and the magnetic properties of the recycled magnets up to and including the 4th cycle. Inductively coupled plasma (ICP) and metallographic analysis indicated that the neodymium hydride additions compensated for the neodymium loss due to evaporation and to oxidation so that the proportion of Nd-rich material remained approximately constant. The additional amount of Nd{sub 2}O{sub 3} in the blended recycled magnets appeared to inhibit grain growth on the 3rd and 4th cycles when compared to that of the unblended magnets. The next challenge is to see if the process can be scaled-up to an industrial scale.

  13. Interpretation of Frenkel’s theory of sintering considering evolution of activated pores: III. Determination of equilibrium sintering time

    Directory of Open Access Journals (Sweden)

    Yu C.L.

    2015-01-01

    Full Text Available In this article, the Frenkel’s theory of liquid-phase sintering was interpreted regarding pores as the activated volume. The mathematical model established by Nikolić et al. was used to infer the equilibrium sintering time at varied sintering temperatures during the isothermal sintering of codierite glass by Giess et al. Through the calculation, the equilibrium time at 800ºC, 820ºC, 840ºC and 860ºC is inferred to be 7014.42mins, 1569.65mins, 368.92mins and 114.61mins, respectively. The equilibrium time decreases as the temperature increases. And the theoretical value is in good accordance with the experimental results. Thus, the model established by Nikolić et al. can be applied successfully to predict the equilibrium sintering time of the cordierite glass at varied temperatures during isothermal sintering.

  14. In-situ TEM visualization of vacancy injection and chemical partition during oxidation of Ni-Cr nanoparticles.

    Science.gov (United States)

    Wang, Chong-Min; Genc, Arda; Cheng, Huikai; Pullan, Lee; Baer, Donald R; Bruemmer, Stephen M

    2014-01-14

    Oxidation of alloy often involves chemical partition and injection of vacancies. Chemical partition is the consequence of selective oxidation, while injection of vacancies is associated with the differences of diffusivity of cations and anions. It is far from clear as how the injected vacancies behave during oxidation of metal. Using in-situ transmission electron microscopy, we captured unprecedented details on the collective behavior of injected vacancies during oxidation of metal, featuring an initial multi-site oxide nucleation, vacancy supersaturation, nucleation of a single cavity, sinking of vacancies into the cavity and accelerated oxidation of the particle. High sensitive energy dispersive x-ray spectroscopy mapping reveals that Cr is preferentially oxidized even at the initial oxidation, leading to a structure that Cr oxide is sandwiched near the inner wall of the hollow particle. The work provides a general guidance on tailoring of nanostructured materials involving multi-ion exchange such as core-shell structured composite nanoparticles.

  15. In situ tribochemical sulfurization of molybdenum oxide nanotubes.

    Science.gov (United States)

    Rodríguez Ripoll, Manel; Tomala, Agnieszka; Gabler, Christoph; DraŽić, Goran; Pirker, Luka; Remškar, Maja

    2018-02-15

    MoS 2 nanoparticles are typically obtained by high temperature sulfurization of organic and inorganic precursors under a S rich atmosphere and have excellent friction reduction properties. We present a novel approach for making the sulfurization unnecessary for MoO 3 nanotubes during the synthesis process for friction and wear reduction applications while simultaneously achieving a superb tribological performance. To this end, we report the first in situ sulfurization of MoO 3 nanotubes during sliding contact in the presence of sulfur-containing lubricant additives. The sulfurization leads to the tribo-chemical formation of a MoS 2 -rich low-friction tribofilm as verified using Raman spectroscopy and can be achieved both during sliding contact and under extreme pressure conditions. Under sliding contact conditions, MoO 3 nanotubes in synergy with sulfurized olefin polysulfide and pre-formed zinc dialkyl dithiophosphate tribofilms achieve an excellent friction performance. Under these conditions, the tribochemical sulfurization of MoO 3 nanotubes leads to a similar coefficient of friction to the one obtained using a model nanolubricant containing MoS 2 nanotubes. Under extreme pressure conditions, the in situ sulfurization of MoO 3 nanotubes using sulfurized olefin polysulfide results in a superb load carrying capacity capable of outperforming MoS 2 nanotubes. The reason is that while MoO 3 nanotubes are able to continuously sulfurize during sliding contact conditions, MoS 2 nanotubes progressively degrade by oxidation thus losing lubricity.

  16. Development of an in-situ multi-component reinforced Al-based metal matrix composite by direct metal laser sintering technique — Optimization of process parameters

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, Subrata Kumar, E-mail: subratagh82@gmail.com [Department of Mechanical Engineering, National Institute of Technology Agartala, Tripura 799055 (India); Bandyopadhyay, Kaushik; Saha, Partha [Department of Mechanical Engineering, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India)

    2014-07-01

    In the present investigation, an in-situ multi-component reinforced aluminum based metal matrix composite was fabricated by the combination of self-propagating high-temperature synthesis and direct metal laser sintering process. The different mixtures of Al, TiO{sub 2} and B{sub 4}C powders were used to initiate and maintain the self-propagating high-temperature synthesis by laser during the sintering process. It was found from the X-ray diffraction analysis and scanning electron microscopy that the reinforcements like Al{sub 2}O{sub 3}, TiC, and TiB{sub 2} were formed in the composite. The scanning electron microscopy revealed the distribution of the reinforcement phases in the composite and phase identities. The variable parameters such as powder layer thickness, laser power, scanning speed, hatching distance and composition of the powder mixture were optimized for higher density, lower porosity and higher microhardness using Taguchi method. Experimental investigation shows that the density of the specimen mainly depends upon the hatching distance, composition and layer thickness. On the other hand, hatching distance, layer thickness and laser power are the significant parameters which influence the porosity. The composition, laser power and layer thickness are the key influencing parameters for microhardness. - Highlights: • The reinforcements such as Al{sub 2}O{sub 3}, TiC, and TiB{sub 2} were produced in Al-MMC through SHS. • The density is mainly influenced by the material composition and hatching distance. • Hatching distance is the major influencing parameter on porosity. • The material composition is the significant parameter to enhance the microhardness. • The SEM micrographs reveal the distribution of TiC, TiB{sub 2} and Al{sub 2}O{sub 3} in the composite.

  17. Surface properties of nanostructured NiO undergoing electrochemical oxidation in 3-methoxy-propionitrile

    Science.gov (United States)

    Bonomo, Matteo; Marrani, Andrea Giacomo; Novelli, Vittoria; Awais, Muhammad; Dowling, Denis P.; Vos, Johannes G.; Dini, Danilo

    2017-05-01

    Nanostructured nickel oxide (NiO) was deposited in the configuration of thin film (thickness, l = 2-6 μm) onto fluorine-doped tin oxide (FTO) substrates via plasma-assisted rapid discharge sintering (RDS). Electrochemical cycling of RDS NiO in 3-methoxy-propionitrile (3-MPN) revealed two characteristic peaks of NiO oxidation which were associated to the surface-confined redox processes Ni(II) → Ni(III) and Ni(III) → Ni(IV). Grazing angle X-ray photoelectron spectroscopy (XPS) was conducted ex-situ on NiO electrodes in both pristine and oxidized states. Oxidized NiO samples for XPS experiments were obtained in the potentiostatic mode through the polarization of NiO at its two characteristic potentials of oxidation. The XPS analysis allowed to ascertain the electronic structure of the nanoporous NiO framework, and verify the adsorption of perchlorate and chloride anions onto NiO surface due to the compensation of the charge stored in oxidized NiO. XPS also revealed that the spectrum within the region characteristic of Ni 2p ionization does not vary considerably with the state of charge of the nickel centres. This finding is in evident contrast to what has been observed for the same system when it undergoes electrochemical oxidation in aqueous electrolyte.

  18. TEM in situ micropillar compression tests of ion irradiated oxide dispersion strengthened alloy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, K.H., E-mail: kaylayano@u.boisestate.edu [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Swenson, M.J. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Wu, Y. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd, Idaho Falls, ID, 83401 (United States); Wharry, J.P. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Purdue University, 400 Central Drive, West Lafayette, IN 47907 (United States)

    2017-01-15

    The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe{sup 2+} ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension ≤100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

  19. Modeling the microstructural evolution during constrained sintering

    DEFF Research Database (Denmark)

    Bjørk, Rasmus; Frandsen, Henrik Lund; Tikare, V.

    A numerical model able to simulate solid state constrained sintering of a powder compact is presented. The model couples an existing kinetic Monte Carlo (kMC) model for free sintering with a finite element (FE) method for calculating stresses on a microstructural level. The microstructural response...... to the stress field as well as the FE calculation of the stress field from the microstructural evolution is discussed. The sintering behavior of two powder compacts constrained by a rigid substrate is simulated and compared to free sintering of the same samples. Constrained sintering result in a larger number...

  20. In-situ synthesis of magnetic iron-oxide nanoparticle-nanofibre composites using electrospinning

    International Nuclear Information System (INIS)

    Burke, Luke; Mortimer, Chris J.; Curtis, Daniel J.; Lewis, Aled R.; Williams, Rhodri; Hawkins, Karl; Maffeis, Thierry G.G.; Wright, Chris J.

    2017-01-01

    We demonstrate a facile, one-step process to form polymer scaffolds composed of magnetic iron oxide nanoparticles (MNPs) contained within electrospun nano- and micro-fibres of two biocompatible polymers, Poly(ethylene oxide) (PEO) and Poly(vinyl pyrrolidone) (PVP). This was achieved with both needle and free-surface electrospinning systems demonstrating the scalability of the composite fibre manufacture; a 228 fold increase in fibre fabrication was observed for the free-surface system. In all cases the nanoparticle-nanofibre composite scaffolds displayed morphological properties as good as or better than those previously described and fabricated using complex multi-stage techniques. Fibres produced had an average diameter (Needle-spun: 125 ± 18 nm (PEO) and 1.58 ± 0.28 μm (PVP); Free-surface electrospun: 155 ± 31 nm (PEO)) similar to that reported previously, were smooth with no bead defects. Nanoparticle-nanofibre composites were characterised using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS) (Nanoparticle average diameter ranging from 8 ± 3 nm to 27 ± 5 nm), XRD (Phase of iron oxide nanoparticles identified as magnetite) and nuclear magnetic resonance relaxation measurements (NMR) (T1/T2: 32.44 for PEO fibres containing MNPs) were used to verify the magnetic behaviour of MNPs. This study represents a significant step forward for production rates of magnetic nanoparticle-nanofibre composite scaffolds by the electrospinning technique. - Graphical abstract: We present a novel facile, one-step process for the in-situ synthesis of magnetic iron oxide nanoparticle-nanofibre composites using both needle and free-surface electrospinning. This is a significant step forward for production rates of magnetic nanoparticle-nanofibre scaffolds both in terms of fibre and nanoparticle production. - Highlights: • We present a novel process for the in-situ synthesis of magnetic iron oxide nanoparticle

  1. In-situ synthesis of magnetic iron-oxide nanoparticle-nanofibre composites using electrospinning

    Energy Technology Data Exchange (ETDEWEB)

    Burke, Luke; Mortimer, Chris J. [Biomaterials, Biofouling and Biofilms Engineering Laboratory (B3EL), Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Curtis, Daniel J.; Lewis, Aled R.; Williams, Rhodri [Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Hawkins, Karl [Centre for NanoHealth (CNH), Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Maffeis, Thierry G.G. [Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Wright, Chris J., E-mail: c.wright@swansea.ac.uk [Biomaterials, Biofouling and Biofilms Engineering Laboratory (B3EL), Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Centre for NanoHealth (CNH), Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom)

    2017-01-01

    We demonstrate a facile, one-step process to form polymer scaffolds composed of magnetic iron oxide nanoparticles (MNPs) contained within electrospun nano- and micro-fibres of two biocompatible polymers, Poly(ethylene oxide) (PEO) and Poly(vinyl pyrrolidone) (PVP). This was achieved with both needle and free-surface electrospinning systems demonstrating the scalability of the composite fibre manufacture; a 228 fold increase in fibre fabrication was observed for the free-surface system. In all cases the nanoparticle-nanofibre composite scaffolds displayed morphological properties as good as or better than those previously described and fabricated using complex multi-stage techniques. Fibres produced had an average diameter (Needle-spun: 125 ± 18 nm (PEO) and 1.58 ± 0.28 μm (PVP); Free-surface electrospun: 155 ± 31 nm (PEO)) similar to that reported previously, were smooth with no bead defects. Nanoparticle-nanofibre composites were characterised using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS) (Nanoparticle average diameter ranging from 8 ± 3 nm to 27 ± 5 nm), XRD (Phase of iron oxide nanoparticles identified as magnetite) and nuclear magnetic resonance relaxation measurements (NMR) (T1/T2: 32.44 for PEO fibres containing MNPs) were used to verify the magnetic behaviour of MNPs. This study represents a significant step forward for production rates of magnetic nanoparticle-nanofibre composite scaffolds by the electrospinning technique. - Graphical abstract: We present a novel facile, one-step process for the in-situ synthesis of magnetic iron oxide nanoparticle-nanofibre composites using both needle and free-surface electrospinning. This is a significant step forward for production rates of magnetic nanoparticle-nanofibre scaffolds both in terms of fibre and nanoparticle production. - Highlights: • We present a novel process for the in-situ synthesis of magnetic iron oxide nanoparticle

  2. Development of titanium based biocomposite by powder metallurgy processing with in situ forming of Ca-P phases

    Energy Technology Data Exchange (ETDEWEB)

    Karanjai, Malobika [International Advanced Research Centre for Powder Metallurgy and New Materials, Balapur P.O., Hyderabad 500005, Andhra Pradesh (India)]. E-mail: malobika@arci.res.in; Sundaresan, Ranganathan [International Advanced Research Centre for Powder Metallurgy and New Materials, Balapur P.O., Hyderabad 500005, Andhra Pradesh (India); Rao, Gummididala Venkata Narasimha [International Advanced Research Centre for Powder Metallurgy and New Materials, Balapur P.O., Hyderabad 500005, Andhra Pradesh (India); Mohan, Tallapragada Raja Rama [Metallurgical Engineering and Materials Science Department, Indian Institute of Technology, Powai, Mumbai 400076, Maharashtra (India); Kashyap, Bhagwati Prasad [Metallurgical Engineering and Materials Science Department, Indian Institute of Technology, Powai, Mumbai 400076, Maharashtra (India)

    2007-02-25

    Composites of titanium and calcium-phosphorus phases were developed by powder metallurgy processing and evaluated for bioactivity. Titanium hydride powder and precursors of calcium and phosphorus in the form of calcium carbonate and di-ammonium hydrogen orthophosphate were mixed in different proportions, compacted and calcined in different atmospheres. The calcined compacts were subsequently crushed, recompacted and sintered in vacuum. In situ formation of bioactive phases like hydroxylapatite, tricalcium phosphate and calcium titanate during the calcination and sintering steps was studied using X-ray diffraction. The effect of calcination atmosphere on density, interconnected porosity, phase composition and modulus of rupture of sintered composites was examined. The sintered composites were immersed in simulated body fluid for 7 days to observe their in vitro behaviour with XRD and FTIR spectroscopic identification of deposits. Composites with 10 wt% precursors sintered from vacuum calcined powder gave the best results in terms of bioactive phases, density and strength.

  3. Master sintering curves of two different alumina powder compacts

    Directory of Open Access Journals (Sweden)

    Vaclav Pouchly

    2009-12-01

    Full Text Available Concept of Master Sintering Curve is a strong tool for optimizing sintering schedule. The sintering behaviour can be predicted, and sintering activation energy can be calculated with the help of few dilatometric measurements. In this paper an automatic procedure was used to calculate Master Sintering Curves of two different alumina compacts. The sintering activation energies were determined as 640 kJ/mol for alumina with particle size of 240 nm, respective 770 kJ/mol for alumina with particle size of 110 nm. The possibility to predict sintering behaviour with the help of Master Sintering Curve was verified.

  4. Residual stresses in a co-sintered SOC half-cell during post-sintering cooling

    DEFF Research Database (Denmark)

    Charlas, Benoit; Chatzichristodoulou, Christodoulos; Brodersen, Karen

    2014-01-01

    .e. the reference temperature (Tref) or the strain difference based on the curvature. This approximation gives good results for bilayers with a defined cooling temperature profile, where the curvature of the bilayer defines a unique balance between the two unknown residual stress states in the two layers......Due to the thermal expansion mismatch between the layers of a Solid Oxide Cell, residual stresses (thermal stresses) develop during the cooling after sintering. Residual stresses can induce cell curvature for asymmetric cells but more importantly they also result in more fragile cells. Depending...... on the loading conditions, the additional stress needed to break the cells can indeed be smaller due to the initial thermo-mechanical stress state. The residual stresses can for a bilayer cell be approximated by estimating the temperature at which elastic stresses start to build up during the cooling, i...

  5. Measures for the reduction of sinter formations in tunnels

    Science.gov (United States)

    Harer, Gerhard

    2017-09-01

    A considerable part of the maintenance costs of tunnel structures is related to the inspection, maintenance and repair of the drainage system. The drainage system of tunnels is frequently clogged with Calcium precipitates. Cleaning and water conditioning are costintensive for operating companies. Apart from the direct costs associated with inspection, maintenance and repair works of the drainage system indirect costs are generated, such as by the blocking of the tunnel while inspection, maintenance or repair or by the reduction of the permitted operation speed. Sintering and clogging of the drainage systems is mainly caused by dissolution of cement minerals in concrete and mortar and/or by inadequate design and construction of the drainage system and/or grubby workmanship. With long-term studies and in-situ experiments in Austria traffic tunnels the specific input factors for sinter mechanism have been identified and appropriate counter measures could be defined. In particular modified mix designs for shotcretes and mortars have proven to bring a significant beneficial effect. By means of constructional measures and by the application of hardness stabilizers a further reduction of hard deposits inside the drainage system is achievable. The paper will deal with the specific aspects and will propose adequate counter measures.

  6. HAp physical investigation - the effect of sintering temperature

    International Nuclear Information System (INIS)

    Mohd Reusmaazran Yusof; Idris Besar; Rusnah Mustaffa; Cik Rohaida Che Hak

    2004-01-01

    The paper presents the effect of sintering temperature on the physical properties of porous hydroxyapatite (HAp). In this study, the HAp was prepared using polymeric sponge techniques with different binder concentration. The sintering process was carried out in air for temperature ranging from 1200 degree C to 1600 degree C. Different physical properties namely density and porosity were observed at different sintering temperatures. The HAp prepared with higher PVP binder showed a slightly decreased in apparent density with increasing sintering temperature, while those HAp prepared with lower PVP showed a slightly increase in apparent density with increasing sintering temperature. The total porosity was found to be approximately constant in the whole sintering temperature range. However, closed porosity decreases with increasing sintering temperature for HAp prepared by lower binder concentration. On the other hand, the HAp prepared by higher binder concentration HAp showed increasing closed porosity with increasing sintering temperature. Other features such as the influence of sintering temperatures on grain and strut also be presented in this paper. (Author)

  7. "In-Situ Chemical Oxidation" - Sessions: #6 Technology Development, Process Fundamentals, Mechanisms;#7 Advantages and Disadvantages; #9 Oxidant Selection; #10 Bench- and Pilot-Scale Studies; #11 Monitoring; #12 Field-Scale Implementation; #13 Chemical Oxidation Regeneration of Granular Activated Carbon

    Science.gov (United States)

    A series of seven technical presentations involving chemical oxidation will be given to faculty, graduate students, and environmental professionals at the Chinese Academy of Sciences in Beijing, China (April 21-22, 2010). Chemical oxidation technologies include in-situ chemical o...

  8. Influence of calcium oxide level and time of exposure to sugarcane on in vitro and in situ digestion kinetics

    Science.gov (United States)

    Experiments were carried out to evaluate, using in vitro and in situ techniques, the effects of three inclusion levels of calcium oxide (0, 5, and 10 g/kg of sugarcane fresh matter) and four exposure times (0, 24, 48, and 72 h) of sugarcane to calcium oxide on the chemical composition and digestive ...

  9. Nano-composite powders Ag-SnO2 prepared by reactive milling sintering and microstructural evolution

    International Nuclear Information System (INIS)

    Lorrain, Nathalie

    2000-01-01

    This work aims at controlling the synthesis and the sintering of nano-composite powders Ag-SnO 2 in order to obtain a dense and nano-structured material for electrical contact as a substitute of the toxic compound Ag - CdO. The powder is prepared by reactive milling from silver oxide (Ag 2 O) and silver bronze (Ag 3 Sn) powders. This process leads to a fine dispersion of silver and tin oxide nanometer sized particles. We first studied the mechanisms of reaction promoted by milling in vacuum and in air. A two-stage oxidation of tin in Ag 3 Sn occurs: during forced contact with Ag 2 O, tin oxidises in SnO, then in SnO 2 . In air, gaseous oxygen also participates to the oxidation of tin in SnO 2 but the reaction is slower because of the formation of silver carbonates from a reaction of Ag 2 O with CO 2 .Then the sintering behaviour of the nano-composite powder as a function of the compacting pressure and of the heating rate has been studied. We show: (i) a diffusion of pure silver towards porosity and free surfaces (exo-diffusion) which destroys the nano-structure and (ii) a severe de-densification. We show that the origin of these phenomena is due to carbonates on to the Ag 2 O starting powder, which are incorporated, in the milled Ag-SnO 2 powder in course of milling; during sintering, decomposition gases generate internal stresses. Low stresses lead to a diffusional creep with exo-diffusion whereas high stresses induce an intensive de-densification by local plastic deformation but no exo-diffusion. A modelling shows that exo-diffusion is limited by heating very quickly a strongly compacted powder that contains a high quantity of carbonates. The experimental results confirm the predictions of the model. Finally, we propose solutions allowing a full densification and a process for decreasing the tin oxide concentration. (author) [fr

  10. Fabrication of in-situ grown graphene reinforced Cu matrix composites

    Science.gov (United States)

    Chen, Yakun; Zhang, Xiang; Liu, Enzuo; He, Chunnian; Shi, Chunsheng; Li, Jiajun; Nash, Philip; Zhao, Naiqin

    2016-01-01

    Graphene/Cu composites were fabricated through a graphene in-situ grown approach, which involved ball-milling of Cu powders with PMMA as solid carbon source, in-situ growth of graphene on flaky Cu powders and vacuum hot-press sintering. SEM and TEM characterization results indicated that graphene in-situ grown on Cu powders guaranteed a homogeneous dispersion and a good combination between graphene and Cu matrix, as well as the intact structure of graphene, which was beneficial to its strengthening effect. The yield strength of 244 MPa and tensile strength of 274 MPa were achieved in the composite with 0.95 wt.% graphene, which were separately 177% and 27.4% enhancement over pure Cu. Strengthening effect of in-situ grown graphene in the matrix was contributed to load transfer and dislocation strengthening. PMID:26763313

  11. High-Pressure Spark Plasma Sintering (HP SPS): A Promising and Reliable Method for Preparing Ti-Al-Si Alloys.

    Science.gov (United States)

    Knaislová, Anna; Novák, Pavel; Cygan, Sławomir; Jaworska, Lucyna; Cabibbo, Marcello

    2017-04-27

    Ti-Al-Si alloys are prospective material for high-temperature applications. Due to low density, good mechanical properties, and oxidation resistance, these intermetallic alloys can be used in the aerospace and automobile industries. Ti-Al-Si alloys were prepared by powder metallurgy using reactive sintering, milling, and spark plasma sintering. One of the novel SPS techniques is high-pressure spark plasma sintering (HP SPS), which was tested in this work and applied to a Ti-10Al-20Si intermetallic alloy using a pressure of 6 GPa and temperatures ranging from 1318 K (1045 °C) to 1597 K (1324 °C). The low-porosity consolidated samples consist of Ti₅Si₃ silicides in an aluminide (TiAl) matrix. The hardness varied between 720 and 892 HV 5.

  12. Characterization and sintering of niobium-ATR alumina

    International Nuclear Information System (INIS)

    Sibuya, N.H.; Iwasaki, H.; Suzuki, C.K.; Pinatti, D.G.

    1987-01-01

    In the niobium aluminothermy a slag is produced, composed mostly of alumina and other compounds such as niobium oxide and silica. The phase composition of this ATR alumina was characterized by X-ray powder diffractometry, and afterwards this alumina was subjected to leaching processes. It was noticed that the original content of 70% α-alumina in slag rose to 95% after the calcination. ATR alumina (leached and calcined, and without any treatment) was used to make pressed bodies which were fired in air at 1200 to 1400 0 C for 1 to 10,5 hours; and in vacuum at 1550 to 1800$0C for 2 hours. Characterization was done by density measurements, X-ray diffractometry and ultrasonic analysis. Ultrasonic analysis of some vacuum fired bodies showed londitudinal velocities close to the value found in literature. Correlation of several techniques measurements disclosed the niobium oxide interference in sintering. (Author) [pt

  13. Brush-Painting and Photonic Sintering of Copper Oxide and Silver Inks on Wood and Cardboard Substrates to Form Antennas for UHF RFID Tags

    Directory of Open Access Journals (Sweden)

    Erja Sipilä

    2016-01-01

    Full Text Available Additive deposition of inks with metallic inclusions provides compelling means to embed electronics into versatile structures. The need to integrate electronics into environmentally friendly components and structures increases dramatically together with the increasing popularity of the Internet of Things. We demonstrate a novel brush-painting method for depositing copper oxide and silver inks directly on wood and cardboard substrates and discuss the optimization of the photonic sintering process parameters for both materials. The optimized parameters were utilized to manufacture passive ultra high frequency (UHF radio frequency identification (RFID tag antennas. The results from wireless testing show that the RFID tags based on the copper oxide and silver ink antennas on wood substrate are readable from ranges of 8.5 and 11 meters, respectively, and on cardboard substrate from read ranges of 8.5 and 12 meters, respectively. These results are well sufficient for many future wireless applications requiring remote identification with RFID.

  14. A new UO2 sintering technology for the recycling of defective fuel pellets

    International Nuclear Information System (INIS)

    Song, K. W.; Kim, K. S.; Jeong, Y. H.

    1998-01-01

    A new UO 2 sintering technology to recycle defective UO 2 pellets has been developed. The defective UO 2 pellets were oxidized in an air to produce U 3 O 8 powder, and the U 3 O 8 powder was mixed with fresh AUC-UO 2 powder in the range of 10 to 100 wt%. Nb 2 O 5 and TiO 2 are added to the mixed powder. The mixed powder was pressed and sintered at 1680 deg C for 4 hours in hydrogen. The density of UO 2 pellets without sintering agents decreased linearly with the U 3 O 8 content at the rate of 0.2 %TD per 1 wt% U 3 O 8 , and the density was below 93.5 %TD at the U 3 O 8 contents above 10 wt%. However, the mixed UO 2 and U 3 O 8 powder containing Nb 2 O 5 (≥0.3 wt%) and TiO 2 (≥0.1 wt%) yielded a sintered density above 94 %TD in all ranges of U 3 O 8 contents. It was found that higher mixing ratios of U 3 O 8 to UO 2 powder did not affect the grain size of UO 2 pellets under the addition of Nb 2 O 5 , but decreased the grain size of UO 2 pellets under the addition of TiO 2 . The doped UO 2 pellets have grain sizes larger than 20 μm, and have small density gain after re-sintering test, owing to large pores. Therefore, the sintering agents such as Nb 2 O 5 and TiO 2 can make highly densified UO 2 pellets from the powder comprising a large amount of U 3 O 8 powder

  15. Reaction behavior of SO2 in the sintering process with flue gas recirculation.

    Science.gov (United States)

    Yu, Zhi-Yuan; Fan, Xiao-Hui; Gan, Min; Chen, Xu-Ling; Chen, Qiang; Huang, Yun-Song

    2016-07-01

    The primary goal of this paper is to reveal the reaction behavior of SO2 in the sinter zone, combustion zone, drying-preheating zone, and over-wet zone during flue gas recirculation (FGR) technique. The results showed that SO2 retention in the sinter zone was associated with free-CaO in the form of CaSO3/CaSO4, and the SO2 adsorption reached a maximum under 900ºC. SO2 in the flue gas came almost from the combustion zone. One reaction behavior was the oxidation of sulfur in the sintering mix when the temperature was between 800 and 1000ºC; the other behavior was the decomposition of sulfite/sulfate when the temperature was over 1000ºC. However, the SO2 adsorption in the sintering bed mainly occurred in the drying-preheating zone, adsorbed by CaCO3, Ca(OH)2, and CaO. When the SO2 adsorption reaction in the drying-preheating zone reached equilibrium, the excess SO2 gas continued to migrate to the over-wet zone and was then absorbed by Ca(OH)2 and H2O. The emission rising point of SO2 moved forward in combustion zone, and the concentration of SO2 emissions significantly increased in the case of flue gas recirculation (FGR) technique. Aiming for the reuse of the sensible heat and a reduction in exhaust gas emission, the FGR technique is proposed in the iron ore sintering process. When using the FGR technique, SO2 emission in exhaust gas gets changed. In practice, the application of the FGR technique in a sinter plant should be cooperative with the flue gas desulfurization (FGD) technique. Thus, it is necessary to study the influence of the FGR technique on SO2 emissions because it will directly influence the demand and design of the FGD system.

  16. Sintering of composite

    International Nuclear Information System (INIS)

    Bordia, R.K.; Scherer, G.W.

    1988-01-01

    Several constitutive laws have been used in the literature to predict the response of sintering bodies under external and internal stress fields. These analyses are based on the assumptions of linear and isotropic behavior. The authors provide a critical examination of these equations and show that some of the available constitutive laws predict a negative Poisson's ratio. These laws have been used to analyze sintering of ceramic matrix composites with rigid inclusions and predict large values of the internal stresses and significant retardation of the densification of composites. Since a negative value of Poisson's ratio has never been observed in sinter - forging experiments, the authors conclude that either the stresses are small (as predicted by the constitutive laws with positive Poisson's ratio) or the basic assumption of linearity and isotropy used in all the analyses is incorrect. Finally, the authors discuss some phenomena that could be important in understanding the densification of ceramic matrix composites

  17. Catalytic non-thermal plasma reactor for the decomposition of a ...

    Indian Academy of Sciences (India)

    2016-08-26

    Aug 26, 2016 ... Among the catalytic study, MnOx/SMF (manganese oxide on sintered metal fibres electrode) shows better performance, probably due to the formation of active oxygen species by in situ decomposition of ozone on the catalyst surface. Water vapour further enhanced the performance due to the in situ ...

  18. Monitoring the in-situ oxide growth on uranium by ultraviolet-visible reflectance spectroscopy

    Science.gov (United States)

    Schweke, Danielle; Maimon, Chen; Chernia, Zelig; Livneh, Tsachi

    2012-11-01

    We demonstrate the in-situ monitoring of oxide growth on U-0.1 wt. % Cr by means of UV-visible reflectance spectroscopy in the thickness range of ˜20-150 nm. Two different approaches are presented: In the "modeling approach," we employ a model for a metallic substrate covered by a dielectric layer, while taking into account the buildup of oxygen gradient and surface roughness. Then, we fit the simulated spectra to the experimental one. In the "extrema analysis," we derive an approximated analytical expression, which relates the oxide thickness to the position of the extrema in the reflectance spectra based on the condition for optical interference of the reflected light. Good agreement is found between the values extracted by the two procedures. Activation energy of ˜21 kcal/mole was obtained by monitoring the oxide growth in the temperature range of 22-90 °C. The upper bound for the thickness determination is argued to be mostly dictated by cracking and detachment processes in the formed oxide.

  19. Fabrication of mullite-bonded porous SiC ceramics from multilayer-coated SiC particles through sol-gel and in-situ polymerization techniques

    Science.gov (United States)

    Ebrahimpour, Omid

    In this work, mullite-bonded porous silicon carbide (SiC) ceramics were prepared via a reaction bonding technique with the assistance of a sol-gel technique or in-situ polymerization as well as a combination of these techniques. In a typical procedure, SiC particles were first coated by alumina using calcined powder and alumina sol via a sol-gel technique followed by drying and passing through a screen. Subsequently, they were coated with the desired amount of polyethylene via an in-situ polymerization technique in a slurry phase reactor using a Ziegler-Natta catalyst. Afterward, the coated powders were dried again and passed through a screen before being pressed into a rectangular mold to make a green body. During the heating process, the polyethylene was burnt out to form pores at a temperature of about 500°C. Increasing the temperature above 800°C led to the partial oxidation of SiC particles to silica. At higher temperatures (above 1400°C) derived silica reacted with alumina to form mullite, which bonds SiC particles together. The porous SiC specimens were characterized with various techniques. The first part of the project was devoted to investigating the oxidation of SiC particles using a Thermogravimetric analysis (TGA) apparatus. The effects of particle size (micro and nano) and oxidation temperature (910°C--1010°C) as well as the initial mass of SiC particles in TGA on the oxidation behaviour of SiC powders were evaluated. To illustrate the oxidation rate of SiC in the packed bed state, a new kinetic model, which takes into account all of the diffusion steps (bulk, inter and intra particle diffusion) and surface oxidation rate, was proposed. Furthermore, the oxidation of SiC particles was analyzed by the X-ray Diffraction (XRD) technique. The effect of different alumina sources (calcined Al2O 3, alumina sol or a combination of the two) on the mechanical, physical, and crystalline structure of mullite-bonded porous SiC ceramics was studied in the

  20. Influence of surface topography on the surface durability of steam oxidised sintered iron

    Directory of Open Access Journals (Sweden)

    José Daniel Biasoli de Mello

    2005-06-01

    Full Text Available Durability of surfaces has been reported as the main factor affecting tribological behavior of steam oxidised sintered iron. The presence of surface pores and their negative influence on load bearing capacity, suggest that surface topography might play an important role on the durability of the oxide layer. In this paper, the influence of compaction pressure and powder grade on surface topography, and as a consequence, its effect on the tribological behavior of steam oxidised sintered iron has been analysed. Specimens prepared from atomised iron powders with different sizes were compacted using 4 different pressures, sintered, and then subjected to steam treatment. Tribological characterisation was carried out in a reciprocating sliding wear test. Although the processing parameters affected the surface topography to a considerable extent, the main influence may be attributed to powder grade. A strong influence of surface topography on the durability distance, evaluated in terms of the evolution of contact resistance with total sliding distance, has been highlighted. Surfaces which were smoother and had high load-carrying capacity were always associated with a higher durability distance.

  1. Corrosion of beryllium oxide

    International Nuclear Information System (INIS)

    Elston, J.; Caillat, R.

    1958-01-01

    Data are reported on the volatilization rate of beryllium oxide in moist air depending on temperature and water vapour concentration. They are concerned with powder samples or sintered shapes of various densities. For sintered samples, the volatilization rate is very low under the following conditions: - temperature: 1300 deg. C, - water vapour concentration in moist air: 25 g/m 3 , - flow rate: 12 I/hour corresponding to a speed of 40 m/hour on the surface of the sample. For calcinated powders (1300 deg. C), grain growth has been observed under a stream of moist air at 1100 deg. C. For instance, grain size changes from 0,5 to at least 2 microns after 500 hours of exposure at this temperature. Furthermore, results data are reported on corrosion of sintered beryllium oxide in pressurized water. At 250 deg. C, under a pressure of 40 kg/cm 2 water is very slightly corrosive; however, internal strains are revealed. Finally, some features on the corrosion in liquid sodium are exposed. (author) [fr

  2. Reduction of surface erosion caused by helium blistering in sintered beryllium and sintered aluminum powder

    International Nuclear Information System (INIS)

    Das, S.K.; Kaminsky, M.

    1976-01-01

    Studies have been conducted to find materials with microstructures which minimize the formation of blisters. A promising class of materials appears to be sintered metal powder with small average grain sizes and low atomic number Z. Studies of the surface erosion of sintered aluminum powder (SAP 895) and of aluminum held at 400 0 C due to blistering by 100 keV helium ions have been conducted and the results are compared to those obtained earlier for room temperature irradiation. A significant reduction of the erosion rate in SAP 895 in comparison to annealed aluminum and SAP 930 is observed. In addition results on the blistering of sintered beryllium powder (type I) irradiated at room temperature and 600 0 C by 100 keV helium ions are given. These results will be compared with those reported recently for vacuum cast beryllium foil and a foil of sintered beryllium powder (type II) which was fabricated differently, than type I. For room temperature irradiation only a few blisters could be observed in sintered beryllium powder type I and type II and they are smaller in size and in number than in vacuum cast beryllium. For irradiation at 600 0 C large scale exfoliation of blisters was observed for vacuum cast beryllium but much less exfoliation was seen for sintered beryllium powder, type I, and type II. The results show a reduction in erosion rate cast beryllium, for both room temperature and 600 0 C

  3. Direct Observations of Oxygen-induced Platinum Nanoparticle Ripening Studied by In Situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Chorkendorff, Ib; Dahl, Søren

    2010-01-01

    This study addresses the sintering mechanism of Pt nanoparticles dispersed on a planar, amorphous Al2O3 support as a model system for a catalyst for automotive exhaust abatement. By means of in situ transmission electron microscopy (TEM), the model catalyst was monitored during the exposure to 10...

  4. Science of sintering and its future

    International Nuclear Information System (INIS)

    Ristic, M.M.

    1975-01-01

    Some new books published by M.Yu. Baljshin, V.A. Ivensen, V.V. Skorohod and others are characterized by the wish to give a complete approach to the problems of sintering theory. Bearing just this in mind while writing the book ''An Essay on the Generalization of Sintering Theory'' (G.V.Samsonov, M.M. Ristic with the collaborators) an idea was born: to ask the most eminent scientists in this field to present their own opinions on the theme ''The Science of Sintering and Modern Views on its Future''. There were formed 18 questions, given in the appendix to be answered. The received answers were presented in 10 chapters of this book. The fourth part of the book consists of papers of eminent scientists engaged in the field of sintering science (some of which were published here for the first time). This material is published in the book with the consent of the authors and these original contributions provide a more profound knowledge of sintering. The initial idea, that the book should have a monograph character and in which the answers would serve as some data on the latest notions of the science of sintering, was somewhat changed since the original opinions of individual scientists are given in the book and these, are sometimes very contradictory. This, in fact, gives the book a special charm because the unsolved problems in the science of sintering are most evidently stressed in this way

  5. Factors Affecting the Sintering of UO2 Pellets

    International Nuclear Information System (INIS)

    El-Hakim, E.; Afifi, Y.K.

    1999-01-01

    Sintering of UO 2 pellets is affected by many parameters such as; UO 2 powder parameters, the conditions followed for preparing the green UO 2 pellets and the sintering scheme(heating and cooling rate, soaking time and temperature). The aim of this work is to study the effect of some these parameters on the characteristics of the sintered UO 2 pellets were qualified according to the technical specifications of Candu fuel. Pressed green pellets at different pressing force (15 to 50 k N) were sintered at 1650 ±20 degree for two hours to study the effect of pressing force on the sintered pellets characteristics; visual inspection, pellet dimensions, density and shrinkage ratio. Compacted green pellets at a pressing force of 48 k N were sintered at different sintering temperature (1600± 20 degree, 1650 ±20 degree, 1700± 20 degree) for two hours to study the effect of sintering temperature on the sintered pellets characteristics. The effect of the heating rate (200,300 and 400 degree per hour) on the sintered pellets characteristics was also investigated. It was found that the pressing force used to compact the green pellets had an effect on the density of the sintered pellets. Pellets pressed at 15 k N have a density of 10.3 g/cm 3 while, those pressed at 50 k N have a density of 10.6 g/cm 3. It was observed that increasing the heating rate to 400 degree /h lead to cracked pellets

  6. Rapid immobilization of simulated radioactive soil waste by microwave sintering.

    Science.gov (United States)

    Zhang, Shuai; Shu, Xiaoyan; Chen, Shunzhang; Yang, Huimin; Hou, Chenxi; Mao, Xueli; Chi, Fangting; Song, Mianxin; Lu, Xirui

    2017-09-05

    A rapid and efficient method is particularly necessary in the timely disposal of seriously radioactive contaminated soil. In this paper, a series of simulated radioactive soil waste containing different contents of neodymium oxide (3-25wt.%) has been successfully vitrified by microwave sintering at 1300°C for 30min. The microstructures, morphology, element distribution, density and chemical durability of as obtained vitrified forms have been analyzed. The results show that the amorphous structure, homogeneous element distribution, and regular density improvement are well kept, except slight cracks emerge on the magnified surface for the 25wt.% Nd 2 O 3 -containing sample. Moreover, all the vitrified forms exhibit excellent chemical durability, and the leaching rates of Nd are kept as ∼10 -4 -10 -6 g/(m 2 day) within 42days. This demonstrates a potential application of microwave sintering in radioactive contaminated soil disposal. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Hot water extraction with in situ wet oxidation: Kinetics of PAHs removal from soil

    International Nuclear Information System (INIS)

    Dadkhah, Ali A.; Akgerman, Aydin

    2006-01-01

    Finding environmentally friendly and cost-effective methods to remediate soils contaminated with polycyclic aromatic hydrocarbons (PAHs) is currently a major concern of researchers. In this study, a series of small-scale semi-continuous extractions - with and without in situ wet oxidation - were performed on soils polluted with PAHs, using subcritical water (i.e. liquid water at high temperatures and pressures, but below the critical point) as the removal agent. Experiments were performed in a 300 mL reactor using an aged soil sample. To find the desorption isotherms and oxidation reaction rates, semi-continuous experiments with residence times of 1 and 2 h were performed using aged soil at 250 deg. C and hydrogen peroxide as oxidizing agent. In all combined extraction and oxidation flow experiments, PAHs in the remaining soil after the experiments were almost undetectable. In combined extraction and oxidation no PAHs could be detected in the liquid phase after the first 30 min of the experiments. Based on these results, extraction with hot water, if combined with oxidation, should reduce the cost of remediation and can be used as a feasible alternative technique for remediating contaminated soils and sediments

  8. Sintering behavior, microstructure and properties of TiC-FeCr hard alloy

    Institute of Scientific and Technical Information of China (English)

    Farid Akhtar; Shiju Guo; Jawid Askari; Jianjun Tian

    2007-01-01

    TiC based cermets were produced with FeCr,as a binder,by conventional P/M (powder metallurgy) to near >97% of the theoretical density.Sintering temperature significantly affects the mechanical properties of the composite.The sintering temperature of>1360 ℃ caused severe chemical reaction between TiC particles and the binder phase.In the TiC-FeCr cermets,the mechanical properties did not vary linearly with the carbide content.Optimum mechanical properties were found in the composite containing 57wt%TiC reinforcement,when sintered at 1360 ℃ for 1 h.Use of carbon as an additive enhanced the mechanical properties of the composites.Cermets containing carbon as an additive with 49wt% TiC exhibited attractive mechanical properties.The microstructure of the developed composite contained less or no debonding,representing good wettability of the binder with TiC particles.Homogeneous distribution of the TiC particles ensured the presence of isotropic mechanical properties and homogeneous distribution of stresses in the composite.Preliminary experiments for evaluation of the oxidation resistance of FeCr bonded TiC cermets indicate that they are more resistant than WC-Co hardmetals.

  9. Modeling of sintering of functionally gradated materials

    International Nuclear Information System (INIS)

    Gasik, M.; Zhang, B.

    2001-01-01

    The functionally gradated materials (FGMs) are distinguished from isotropic materials by gradients of composition, phase distribution, porosity, and related properties. For FGMs made by powder metallurgy, sintering control is one of the most important factors. In this study sintering process of FGMs is modeled and simulated with a computer. A new modeling approach was used to formulate equation systems and the model for sintering of gradated hard metals, coupled with heat transfer and grain growth. A FEM module was developed to simulate FGM sintering in conventional, microwave and hybrid conditions, to calculate density, stress and temperature distribution. Behavior of gradated WC-Co hardmetal plate and cone specimens was simulated for various conditions, such as mean particle size, green density distribution and cobalt gradation parameter. The results show that the deformation behavior and stress history of graded powder compacts during heating, sintering and cooling could be predicted for optimization of sintering process. (author)

  10. Properties, structure and machnining capabilities sintered corundum abrasives

    Directory of Open Access Journals (Sweden)

    Cz.J. Niżankowski

    2010-07-01

    Full Text Available The diversity of sintered corundum abrasives used in both bonded and in the embankment of abrasive tools currently poses substantialproblems for their choice of technology to specific tasks. Therefore performed a comparative study of ownership structures and capacitiesof elected representatives machnining sintered corundum abrasives of different generations, and this is normal sintered alumina,submicrocrystalline alumina sintered and nanocrystalline alumina sintered. Were studied some properties of a set of abrasive particles,physicochemical properties and structural and mechanical and technological properties. The studies used the method of microscopicmeasurement to determine the shape of abrasive particles, the pycnometer to determine the density of abrasive, a spectrometer todetermine the chemical composition of the magnetic analyzer for determining the magnetic fraction, scanning electron microscope toanalysis of abrasive grains and a special position to designate the machining capacity abrasive grains. The results showed a significantincrease in machining capacity sintered corundum abrasives with increasing degree of fragmentation of the crystallites sintered corundum abrasives and distinctive bands in the emerging microchip. The originality of the development provides a comparative summary ofproperties of sintered corundum abrasives of different generations and functions obtained by the author making the change in value indexof machininhcapacity grit from cutting speeds for different generations of sintered corundum.

  11. Determination of rare earth elements, hafnium and cadmium in sintered pellets of mixed thorium and uranium oxides by neutron activation

    International Nuclear Information System (INIS)

    Cardoso, S.N.M.

    1987-01-01

    This work shows the development of a method for determination of the rare-earth elements (Eu, Sm, Dy and Gd), Hf and Cd contents in sinterized U and Th mixed oxides by neutron activation analysis. The sample is dissolved in nitric/fluoridric (0,1% HF) medium, to dryness and redissolved in 6N HCl solution. The Hf is extracted into organic phase (0,5 M TTA/benzene), irradiated and analysed through 181 Hf isotope energy peak. The aqueous phase is treated with NH 4 OH for the precipitation of hidroxides. Then, these are dissolved in 6N HNO 3 solution. The extraction of U and Th is made in two steps, one with TBP/CCl 4 and another with 0,5 M TTA/C 6 H 6 . Then the rare-earth elements and Cd are irradiated and determined by gamma spectrometry. (author) [pt

  12. In situ screen-printed BaZr{sub 0.1}Ce{sub 0.7}Y{sub 0.2}O{sub 3-{delta}} electrolyte-based protonic ceramic membrane fuel cells with layered SmBaCo{sub 2}O{sub 5+x} cathode

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Bin; Dong, Yingchao; Zhang, Shangquan; Hu, Mingjun; Zhou, Yang; Meng, Guangyao [Department of Materials Science and Engineering, University of Science and Technology of China (USTC), Hefei, Anhui 230026 (China); Yan, Ruiqiang [Department of Materials Engineering, Taizhou University, Linhai, Zhejiang 317000 (China)

    2009-01-15

    In order to develop a simple and cost-effective route to fabricate protonic ceramic membrane fuel cells (PCMFCs) with layered SmBaCo{sub 2}O{sub 5+x} (SBCO) cathode, a dense BaZr{sub 0.1}Ce{sub 0.7}Y{sub 0.2}O{sub 3-{delta}} (BZCY) electrolyte was fabricated on a porous anode by in situ screen printing. The porous NiO-BaZr{sub 0.1}Ce{sub 0.7}Y{sub 0.2}O{sub 3-{delta}} (NiO-BZCY) anode was directly prepared from metal oxide (NiO, BaCO{sub 3}, ZrO{sub 2}, CeO{sub 2} and Y{sub 2}O{sub 3}) by a simple gel-casting process. An ink of metal oxide (BaCO{sub 3}, ZrO{sub 2}, CeO{sub 2} and Y{sub 2}O{sub 3}) powders was then employed to deposit BaZr{sub 0.1}Ce{sub 0.7}Y{sub 0.2}O{sub 3-{delta}} (BZCY) thin layer by an in situ reaction-sintering screen printing process on NiO-BZCY anode. The bi-layer with 25 {mu}m dense BZCY electrolyte was obtained by co-sintering at 1400 C for 5 h. With layered SBCO cathode synthesized by gel-casting on the bi-layer, single cells were assembled and tested with H{sub 2} as fuel and the static air as oxidant. A high open-circuit potential of 1.01 V, a maximum power density of 382 mW cm{sup -2}, and a low polarization resistance of the electrodes of 0.15 {omega} cm{sup 2} was achieved at 700 C. (author)

  13. Voltammetric, in-situ spectroelectrochemical and in-situ electrocolorimetric characterization of phthalocyanines

    Energy Technology Data Exchange (ETDEWEB)

    Koca, Atif [Department of Chemical Engineering, Faculty of Engineering, Marmara University, Goeztepe, 34722 Istanbul (Turkey)], E-mail: akoca@eng.marmara.edu.tr; Bayar, Serife; Dincer, Hatice A. [Department of Chemistry, Technical University of Istanbul, Maslak, 34469 Istanbul (Turkey); Gonca, Erguen [Department of Chemistry, Fatih University, TR34500 B.Cekmece, Istanbul (Turkey)

    2009-04-01

    In this work, electrochemical, and in-situ spectroelectrochemical characterization of the metallophthalocyanines bearing tetra-(1,1-(dicarbethoxy)-2-(2-methylbenzyl))-ethyl 3,10,17,24-tetra chloro groups were performed. Voltammetric and in-situ spectroelectrochemical measurements show that while cobalt phthalocyanine complex gives both metal-based and ring-based redox processes, zinc and copper phthalocyanines show only ring-based reduction and oxidation processes. The redox processes are generally diffusion-controlled, reversible and one-electron transfer processes. Differently lead phthalocyanine demetallized during second oxidation reaction while it was stable during reduction processes. An in-situ electrocolorimetric method, based on the 1931 CIE (Commission Internationale de l'Eclairage) system of colorimetry, has been applied to investigate the color of the electro-generated anionic and cationic forms of the complexes for the first time in this study.

  14. Full densification of inkjet-printed copper conductive tracks on a flexible substrate utilizing a hydrogen plasma sintering

    Science.gov (United States)

    Kwon, Young-Tae; Lee, Young-In; Kim, Seil; Lee, Kun-Jae; Choa, Yong-Ho

    2017-02-01

    Low temperature sintering techniques are crucial in developing flexible printed electronics. In this work, we demonstrate a novel hydrogen plasma sintering method that achieves a full reduction and densification of inkjet-printed patterns using a copper complex ion ink. After inkjet printing on polyethylene terephthalate (PET) substrates, both hydrogen plasma and conventional hydrogen thermal treatment were employed to compare the resulting microstructures, electrical properties and anti-oxidation behavior. The plasma treated pattern shows a fully densified microstructure with a resistivity of 3.23 μΩ cm, while the thermally treated pattern shows a relatively poor microstructure and high resistivity. In addition, the hydrogen plasma-treated copper pattern retains its electrical resistivity for one month without any significant decrease. This novel hydrogen plasma sintering technique could be used to produce conductive patterns with excellent electrical properties, allowing for highly reliable flexible printed electronics.

  15. Effect of sintering temperature on structure of C-B4C-SiC composites with silicon additive

    International Nuclear Information System (INIS)

    Wu Lijun; Academia Sinica, Shenyang; Huang Qizhong; Yang Qiaoqin; Zhao Lihu; Xu Zhongyu

    1996-01-01

    Carbon materials possess good electric conductivity, heat conductivity, corrosion-resistance, self-lubrication and hot-shocking resistance, and are easily machined. However, they have low mechanical strength, and are easily oxidized in air at high temperature. On the contrary, ceramic materials have high mechanical strength and hardness, and have good wear-resistance and oxidation-resistance. However, they have the shortages of poor thermal-shock resistance lubrication, and are difficult to machine. Therefore, carbon/ceramic composites with the advantages of both carbon and ceramic materials have been widely studied in the recent years. Huang prepared C-B 4 C-SiC composites with the free sintering method and the hot pressing method, and studied the effects of Si, Al, Al 2 O 3 , Ni and Ti additives on the properties of the composites. The results showed that these additives could improve the properties of the composites. Zhao et al. studies the structure of C-B 4 C-SiC composites with Si additive sintered at 2,000 C and found two c-center monoclinic phases. In this paper, the authors discussed the effect of the sintering temperature on the structure of C-B 4 C-SiC composites with Si additive by means of transmission electron microscope (TEM) and x-ray diffractometer (XRD)

  16. Layer by Layer Ex-Situ Deposited Cobalt-Manganese Oxide as Composite Electrode Material for Electrochemical Capacitor.

    Science.gov (United States)

    Rusi; Chan, P Y; Majid, S R

    2015-01-01

    The composite metal oxide electrode films were fabricated using ex situ electrodeposition method with further heating treatment at 300°C. The obtained composite metal oxide film had a spherical structure with mass loading from 0.13 to 0.21 mg cm(-2). The structure and elements of the composite was investigated using X-ray diffraction (XRD) and energy dispersive X-ray (EDX). The electrochemical performance of different composite metal oxides was studied by cyclic voltammetry (CV) and galvanostatic charge-discharge (CD). As an active electrode material for a supercapacitor, the Co-Mn composite electrode exhibits a specific capacitance of 285 Fg(-1) at current density of 1.85 Ag(-1) in 0.5 M Na2SO4 electrolyte. The best composite electrode, Co-Mn electrode was then further studied in various electrolytes (i.e., 0.5 M KOH and 0.5 M KOH/0.04 M K3Fe(CN) 6 electrolytes). The pseudocapacitive nature of the material of Co-Mn lead to a high specific capacitance of 2.2 x 10(3) Fg(-1) and an energy density of 309 Whkg(-1) in a 0.5 M KOH/0.04 M K3Fe(CN) 6 electrolyte at a current density of 10 Ag(-1). The specific capacitance retention obtained 67% of its initial value after 750 cycles. The results indicate that the ex situ deposited composite metal oxide nanoparticles have promising potential in future practical applications.

  17. Nanoscale size effect in in situ titanium based composites with cell viability and cytocompatibility studies

    Energy Technology Data Exchange (ETDEWEB)

    Miklaszewski, Andrzej, E-mail: andrzej.miklaszewski@put.poznan.pl [Institute of Materials Science and Engineering, Poznan University of Technology, Jana Pawla II 24, 61-138 Poznan (Poland); Jurczyk, Mieczysława U. [Division Mother' s and Child' s Health, Poznan University of Medical Sciences, Polna 33, 60-535 Poznan (Poland); Kaczmarek, Mariusz [Department of Immunology, Chair of Clinical Immunology, Poznan University of Medical Sciences, Rokietnicka 5D, 60-806 Poznan (Poland); Paszel-Jaworska, Anna; Romaniuk, Aleksandra; Lipińska, Natalia [Department of Clinical Chemistry and Molecular Diagnostics, Poznan University of Medical Sciences, Przybyszewskiego 49, 60-355 Poznan (Poland); Żurawski, Jakub [Department of Immunobiochemistry, Chair of Biology and Environmental Sciences, Poznan University of Medical Sciences, Rokietnicka 8, 60-806 Poznan (Poland); Urbaniak, Paulina [Department of Cell Biology, Poznan University of Medical Sciences, Rokietnicka 5D, 60-806 Poznan (Poland); Jurczyk, Mieczyslaw [Institute of Materials Science and Engineering, Poznan University of Technology, Jana Pawla II 24, 61-138 Poznan (Poland)

    2017-04-01

    Novel in situ Metal Matrix Nanocomposite (MMNC) materials based on titanium and boron, revealed their new properties in the nanoscale range. In situ nanocomposites, obtained through mechanical alloying and traditional powder metallurgy compaction and sintering, show obvious differences to their microstructural analogue. A unique microstructure connected with good mechanical properties reliant on the processing conditions favour the nanoscale range of results of the Ti-TiB in situ MMNC example. The data summarised in this work, support and extend the knowledge boundaries of the nanoscale size effect that influence not only the mechanical properties but also the studies on the cell viability and cytocompatibility. Prepared in the same bulk, in situ MMNC, based on titanium and boron, could be considered as a possible candidate for dental implants and other medical applications. The observed relations and research conclusions are transferable to the in situ MMNC material group. Aside from all the discussed relations, the increasing share of these composites in the ever-growing material markets, heavily depends on the attractiveness and a possible wider application of these composites as well as their operational simplicity presented in this work. - Highlights: • Nano and microscale size precursor influence the final composite microstructure and properties. • Obtained from the nanoscale precursor sinters, characterise with a uniform and highly dispersed microstructure • Mechanical properties favoured Nano scale size precursor • Boron addition could be significantly reduced for moderate properties range. • A possible candidate for dental implants and other medical applications.

  18. Master sintering curve: A practical approach to its construction

    Directory of Open Access Journals (Sweden)

    Pouchly V.

    2010-01-01

    Full Text Available The concept of a Master Sintering Curve (MSC is a strong tool for optimizing the sintering process. However, constructing the MSC from sintering data involves complicated and time-consuming calculations. A practical method for the construction of a MSC is presented in the paper. With the help of a few dilatometric sintering experiments the newly developed software calculates the MSC and finds the optimal activation energy of a given material. The software, which also enables sintering prediction, was verified by sintering tetragonal and cubic zirconia, and alumina of two different particle sizes.

  19. Lutetium oxide-based transparent ceramic scintillators

    Science.gov (United States)

    Seeley, Zachary; Cherepy, Nerine; Kuntz, Joshua; Payne, Stephen A.

    2016-01-19

    In one embodiment, a transparent ceramic of sintered nanoparticles includes gadolinium lutetium oxide doped with europium having a chemical composition (Lu.sub.1-xGd.sub.x).sub.2-YEu.sub.YO.sub.3, where X is any value within a range from about 0.05 to about 0.45 and Y is any value within a range from about 0.01 to about 0.2, and where the transparent ceramic exhibits a transparency characterized by a scatter coefficient of less than about 10%/cm. In another embodiment, a transparent ceramic scintillator of sintered nanoparticles, includes a body of sintered nanoparticles including gadolinium lutetium oxide doped with a rare earth activator (RE) having a chemical composition (Lu.sub.1-xGd.sub.x).sub.2-YRE.sub.YO.sub.3, where RE is selected from the group consisting of: Sm, Eu, Tb, and Dy, where the transparent ceramic exhibits a transparency characterized by a scatter coefficient of less than about 10%/cm.

  20. Two-dimensional simulation of sintering process

    International Nuclear Information System (INIS)

    Vasconcelos, Vanderley de; Pinto, Lucio Carlos Martins; Vasconcelos, Wander L.

    1996-01-01

    The results of two-dimensional simulations are directly applied to systems in which one of the dimensions is much smaller than the others, and to sections of three dimensional models. Moreover, these simulations are the first step of the analysis of more complex three-dimensional systems. In this work, two basic features of the sintering process are studied: the types of particle size distributions related to the powder production processes and the evolution of geometric parameters of the resultant microstructures during the solid-state sintering. Random packing of equal spheres is considered in the sintering simulation. The packing algorithm does not take into account the interactive forces between the particles. The used sintering algorithm causes the densification of the particle set. (author)

  1. Three-dimensional simulation of viscous-flow agglomerate sintering.

    Science.gov (United States)

    Kirchhof, M J; Schmid, H -J; Peukert, W

    2009-08-01

    The viscous-flow sintering of different agglomerate particle morphologies is studied by three-dimensional computer simulations based on the concept of fractional volume of fluid. For a fundamental understanding of particle sintering characteristics, the neck growth kinetics in agglomerate chains and in doublets consisting of differently sized primary particles is investigated. Results show that different sintering contacts in agglomerates even during the first stages are not completely independent from each other, even though differences are small. The neck growth kinetics of differently sized primary particles is determined by the smaller one up to a size difference by a factor of approximately 2, whereas for larger size differences, the kinetics becomes faster. In particular, the agglomerate sintering kinetics is investigated for particle chains of different lengths and for different particle morphologies each having ten primary particles and nine initial sintering contacts. For agglomerate chains, the kinetics approximately can be normalized by using the radius of the fully coalesced sphere. In general, different agglomerate morphologies show equal kinetics during the first sintering stages, whereas during advanced stages, compact morphologies show significantly faster sintering progress than more open morphologies. Hence, the overall kinetics cannot be described by simply using constant morphology correction factors such as fractal dimension or mean coordination number which are used in common sintering models. However, for the first stages of viscous-flow agglomerate sintering, which are the most important for many particle processes, a sintering equation is presented. Although we use agglomerates consisting of spherical primary particles, our methodology can be applied to other aggregate geometries as well.

  2. In-situ polymerization of polyaniline on the surface of graphene oxide for high electrochemical capacitance

    International Nuclear Information System (INIS)

    Li, Xinlu; Zhong, Qineng; Zhang, Xinlin; Li, Tongtao; Huang, Jiamu

    2015-01-01

    Conducting polymer polyaniline (PANI) was in-situ polymerized on the surface of graphene oxide (GO) to form PANI encapsulating GO nanocomposites. The morphology and microstructure were examined by scanning electron microscopy, X-ray diffraction and N 2 absorption/desorption analysis. Electrochemical properties were tested by cyclic voltammetry, galvanostatic charge/discharge cycles and electrochemical impedance spectroscopy. Experimental results showed that ethanol assisted the dispersion of GO in water and facilitated the diffusion of polymer monomers on GO. GO as a support material can provide sufficient reaction sites for the deposition of aniline to form the film-like GO/PANI composites. Capacitive performance illustrated that the in-situ polymerization of PANI on GO was effective in improving the specific capacitance and cycling stability. - Highlights: • GO/PANI nanocomposites were achieved by in-situ polymerization. • PANI was uniformly coated on the surface of GO with addition of ethanol. • GO/PANI show high specific capacitance and cycling stability

  3. Sintered ceramics having controlled density and porosity

    International Nuclear Information System (INIS)

    Brassfield, H.C.; DeHollander, W.R.; Nivas, Y.

    1980-01-01

    A new method was developed for sintering ceramic uranium dioxide powders, in which ammonium oxalate is admixed with the powder prior to being pressed into a cylindrical green body, so that the end-point density of the final nuclear-reactor fuel product can be controlled. When the green body is heated, the ammonium oxalate decomposes and leaves discrete porosity in the sintered body, which corresponds to the ammonium oxalate regions in the green body. Thus the end-point density of the sintered body is a function of the amount of ammonium oxalate added. The final density of the sintered product is about 90-97% of the theoretical. The addition of ammonium oxalate also allows control of the pore size and distribution throughout the fuel. The process leaves substantially no impurities in the sintered strucuture. (DN)

  4. Two steps sintering alumina doped with niobia

    International Nuclear Information System (INIS)

    Gomes, L.B.; Hatzfeld, J.; Heck, M.; Pokorny, A.; Bergmann, C.P.

    2014-01-01

    In this work, high surface area commercial alumina was doped with niobia and sintered in two steps in order to obtain dense materials with lower processing temperatures. The powders were milled and uniaxially pressed (200 MPa). The first step of sintering took place at 1100°C for 3, 6, 9 and 12 hours, followed by the second step at 1350°C for 3 hours. The relative density, porosity and water absorption of the samples were determined by the Archimedes method. The crystalline phases were analyzed by X-ray Diffraction (XRD) and the morphology of the samples after sintering, evaluated by Scanning Electron Microscopy (SEM). The results indicate that the use of niobia combined with the two steps sintering promotes an increase in the density of the material, even at lower sintering temperatures. (author)

  5. Freeform Fabrication of Magnetophotonic Crystals with Diamond Lattices of Oxide and Metallic Glasses for Terahertz Wave Control by Micro Patterning Stereolithography and Low Temperature Sintering

    Directory of Open Access Journals (Sweden)

    Maasa Nakano

    2013-04-01

    Full Text Available Micrometer order magnetophotonic crystals with periodic arranged metallic glass and oxide glass composite materials were fabricated by stereolithographic method to reflect electromagnetic waves in terahertz frequency ranges through Bragg diffraction. In the fabrication process, the photo sensitive acrylic resin paste mixed with micrometer sized metallic glass of Fe72B14.4Si9.6Nb4 and oxide glass of B2O3·Bi2O3 particles was spread on a metal substrate, and cross sectional images of ultra violet ray were exposed. Through the layer by layer stacking, micro lattice structures with a diamond type periodic arrangement were successfully formed. The composite structures could be obtained through the dewaxing and sintering process with the lower temperature under the transition point of metallic glass. Transmission spectra of the terahertz waves through the magnetophotonic crystals were measured by using a terahertz time domain spectroscopy.

  6. Effect of K3PO4 addition as sintering inhibitor during calcination of Y2O3 nanoparticles

    Science.gov (United States)

    Soga, K.; Okumura, Y.; Tsuji, K.; Venkatachalam, N.

    2009-11-01

    Erbium-doped yttrium oxide nanoparticle is one of the most important for fluorescence bioimaging under near infrared excitation. Particle size of it below 100 nm is an important requirement for a cellular bioimaging. However, the synthesis with such small particles is difficult at the calcination temperature above 1200 °C due to the sintering and crystal growth of the particles. In this study, yttrium oxide nanoparticles with average size of 30 nm were successfully synthesized by using K3PO4 as a sintering inhibitor during the calcination. A single phase of cubic Y2O3 as the resultant material was confirmed by XRD, which was also confirmed to emit a bright upconversion emission under 980-nm excitation. Improvement of chemical durability due to the introduction of phosphate group on the surface of the Y2O3 particles is also reported.

  7. Sintering and microstructure of ice: a review

    International Nuclear Information System (INIS)

    Blackford, Jane R

    2007-01-01

    Sintering of ice is driven by the thermodynamic requirement to decrease surface energy. The structural morphology of ice in nature has many forms-from snowflakes to glaciers. These forms and their evolution depend critically on the balance between the thermodynamic and kinetic factors involved. Ice is a crystalline material so scientific understanding and approaches from more conventional materials can be applied to ice. The early models of solid state ice sintering are based on power law models originally developed in metallurgy. For pressure sintering of ice, these are based on work on hot isostatic pressing of metals and ceramics. Recent advances in recognizing the grain boundary groove geometry between sintering ice particles require models that use new approaches in materials science. The newer models of sintering in materials science are beginning to incorporate more realistic processing conditions and microstructural complexity, and so there is much to be gained from applying these to ice in the future. The vapour pressure of ice is high, which causes it to sublime readily. The main mechanism for isothermal sintering of ice particles is by vapour diffusion; however other transport mechanisms certainly contribute. Plastic deformation with power law creep combined with recrystallization become important mechanisms in sintering with external pressure. Modern experimental techniques, low temperature scanning electron microscopy and x-ray tomography, are providing new insights into the evolution of microstructures in ice. Sintering in the presence of a small volume fraction of the liquid phase causes much higher bond growth rates. This may be important in natural snow which contains impurities that form a liquid phase. Knowledge of ice microstructure and sintering is beneficial in understanding mechanical behaviour in ice friction and the stability of snow slopes prone to avalanches. (topical review)

  8. Effect of Sintering Temperature and Applied Load on Anode-Supported Electrodes for SOFC Application

    Directory of Open Access Journals (Sweden)

    Xuan-Vien Nguyen

    2016-08-01

    Full Text Available Anode-supported cells are prepared by a sequence of hot pressing and co-sintering processes for solid oxide fuel cell (SOFC applications. Commercially available porous anode tape (NiO/YSZ = 50 wt %/50 wt %, anode tape (NiO/YSZ = 30 wt %/70 wt %, and YSZ are used as the anode substrate, anode functional layer, and electrolyte layer, respectively. After hot pressing, the stacked layers are then sintered at different temperatures (1250 °C, 1350 °C, 1400 °C and 1450 °C for 5 h in air. Different compressive loads are applied during the sintering process. An (La,SrMnO3 (LSM paste is coated on the post-sintered anode-supported electrolyte surface as the cathode, and sintered at different temperatures (1100 °C, 1150 °C, 1200 °C and 1250 °C for 2 h in air to generate anode-supported cells with dimensions of 60 × 60 mm2 (active reaction area of 50 × 50 mm2. SEM is used to investigate the anode structure of the anode-supported cells. In addition, confocal laser scanning microscopy is used to investigate the roughness of the cathode surfaces. At sintering temperatures of 1400 °C and 1450 °C, there is significant grain growth in the anode. Furthermore, the surface of the cathode is smoother at a firing temperature of 1200 °C. It is also found that the optimal compressive load of 1742 Pa led to a flatness of 168 µm/6 cm and a deformation of 0.72%. The open circuit voltage and power density of the anode-supported cell at 750 °C were 1.0 V and 178 mW·cm−2, respectively.

  9. Sintered cobalt-rare earth intermetallic product

    International Nuclear Information System (INIS)

    Benz, M.C.

    1975-01-01

    A process is described for preparing novel sintered cobalt--rare earth intermetallic products which can be magnetized to form permanent magnets having stable improved magnetic properties. A cobalt--rare earth metal alloy is formed having a composition which at sintering temperature falls outside the composition covered by the single Co 5 R intermetallic phase on the rare earth richer side. The alloy contains a major amount of the Co 5 R intermetallic phase and a second solid CoR phase which is richer in rare earth metal content than the Co 5 R phase. The specific cobalt and rare earth metal content of the alloy is substantially the same as that desired in the sintered product. The alloy, in particulate form, is pressed into compacts and sintered to the desired density. The sintered product is comprised of a major amount of the Co 5 R solid intermetallic phase and up to about 35 percent of the product of the second solid CoR intermetallic phase which is richer in rare earth metal content than the Co 5 R phase

  10. Sintering-alkaline processing of borosilicate ores of Tajikistan

    International Nuclear Information System (INIS)

    Nazarov, F.A.

    2018-01-01

    The aim of the work is to study the processes of decomposition of boron-containing ore by sintering with NaOH, finding the optimal parameters of the decomposition process, studying the kinetics of processes and developing the technological foundations for ore processing. The processes of borosilicate ore processing were studied by sintering with NaOH. Possible mechanisms of chemical reactions of the process of sintering-alkaline decomposition of boron-containing ore are established, the results of which are substantiated by physicochemical methods of analysis. A principal technological scheme for processing of borosilicate ores by a sintering-alkaline method has been developed. In the first chapter, data on alkaline and caking processes for processing boron-containing and aluminium comprising raw materials are available in the literature. Based on this, the directions of our own research are outlined. The second chapter is devoted to the study of the chemical and mineralogical compositions of borosilicate ores and their concentrates with the help of X-ray phase and chemical analysis methods, the stoichiometric calculation of the formation of aluminum, iron, and boron salts has been carried out, and a thermodynamic analysis of the processes of sintering borosilicate ores with alkali has been considered. The third chapter presents the results of a study of sintering-alkaline method of processing of initial borosilicate ore of the Ak-Arkhar Deposit and its concentrate without calcination and after calcination. The kinetics of sintering of borosilicate ores with sodium hydroxide was studied. The optimal conditions of borosilicate ore sintering before and after the preliminary calcination with alkali were determined. Optimal parameters of the sintering process have been found: sintering temperature 800-8500 deg C, duration of the process - 60 minutes, mass ratio of NaOH to raw materials 2: 1. The conditions for sintering of borosilicate concentrate with alkali have been

  11. Improving NASICON Sinterability through Crystallization under High Frequency Electrical Fields

    Directory of Open Access Journals (Sweden)

    Ilya eLisenker

    2016-03-01

    Full Text Available The effect of high frequency (HF electric fields on the crystallization and sintering rates of a lithium aluminum germanium phosphate (LAGP ion conducting ceramic was investigated. LAGP with the nominal composition Li1.5Al0.5Ge1.5(PO43 was crystallized and sintered, both conventionally and under effect of electrical field. Electrical field application, of 300V/cm at 1MHz, produced up to a 40% improvement in sintering rate of LAGP that was crystallized and sintered under the HF field. Heat sink effect of the electrodes appears to arrest thermal runaway and subsequent flash behavior. Sintered pellets were characterized using XRD, SEM, TEM and EIS to compare conventionally and field sintered processes. The as-sintered structure appears largely unaffected by the field as the sintering curves tend to converge beyond initial stages of sintering. Differences in densities and microstructure after 1 hour of sintering were minor with measured sintering strains of 31% vs. 26% with and without field, respectively . Ionic conductivity of the sintered pellets was evaluated and no deterioration due to the use of HF field was noted, though capacitance of grain boundaries due to secondary phases was significantly increased.

  12. Sintered-to-size FBR fuel

    International Nuclear Information System (INIS)

    Rasmussen, D.E.; Schaus, P.S.

    1984-04-01

    Fabrication of sintered-to-size PuO 2 -UO 2 fuel pellets was completed for testing of proposed FBR product specifications. Approximately 6000 pellets were fabricated to two nominal diameters and two densities by cold pressing and sintering to size. Process control and correlation between test and production batches are discussed

  13. In situ one-pot preparation of reduced graphene oxide/polyaniline composite for high-performance electrochemical capacitors

    International Nuclear Information System (INIS)

    Chen, Nali; Ren, Yapeng; Kong, Peipei; Tan, Lin; Feng, Huixia; Luo, Yongchun

    2017-01-01

    Highlights: • A new method to prepare reduced graphene oxide/polyaniline composite is developed. • Aniline serves as a reduction for graphene oxide under weak alkali condition. • Different characterizations confirm that GO can be effectively reduced by aniline. • A high specific capacitance of 524.4 F·g"−"1 is obtained at 0.5 A·g"−"1. - Abstract: Reduced graphene oxide/polyaniline (rGO/PANI) composites are prepared through an effective in situ one-pot synthesis route that includes the reduction of graphene oxide (GO) by aniline under weak alkali condition via hydrothermal method and then followed by in situ polymerization of aniline. X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscope and transmission electron microscope are employed to reveal that GO is successfully reduced by aniline under weak alkali condition and PANI can be deposited on the surfaces of reduced graphene oxide (rGO) sheets. The effect of rGO is optimized by tuning the mass ratios of aniline to GO to improve the electrochemical performance of rGO/PANI composites. The maximum specific capacitance of rGO/PANI composites achieves 524.4 F/g with a mass ratio of aniline to GO 10:1 at a current density of 0.5 A/g, in comparison to the specific capacitance of 397 F/g at the same current density of pure PANI. Particularly, the specific capacity retention rate is 81.1% after 2000 cycles at 100 mv/s scan rate, which is an improvement over that of pure PANI (55.5%).

  14. In situ one-pot preparation of reduced graphene oxide/polyaniline composite for high-performance electrochemical capacitors

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Nali [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); State Key Laboratory of Advanced Processing and Recycling of Nonferrous Metals, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Ren, Yapeng; Kong, Peipei; Tan, Lin [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Feng, Huixia, E-mail: fenghx@lut.cn [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Luo, Yongchun, E-mail: luoyc@lut.cn [State Key Laboratory of Advanced Processing and Recycling of Nonferrous Metals, Lanzhou University of Technology, Lanzhou 730050, Gansu (China)

    2017-01-15

    Highlights: • A new method to prepare reduced graphene oxide/polyaniline composite is developed. • Aniline serves as a reduction for graphene oxide under weak alkali condition. • Different characterizations confirm that GO can be effectively reduced by aniline. • A high specific capacitance of 524.4 F·g{sup −1} is obtained at 0.5 A·g{sup −1}. - Abstract: Reduced graphene oxide/polyaniline (rGO/PANI) composites are prepared through an effective in situ one-pot synthesis route that includes the reduction of graphene oxide (GO) by aniline under weak alkali condition via hydrothermal method and then followed by in situ polymerization of aniline. X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscope and transmission electron microscope are employed to reveal that GO is successfully reduced by aniline under weak alkali condition and PANI can be deposited on the surfaces of reduced graphene oxide (rGO) sheets. The effect of rGO is optimized by tuning the mass ratios of aniline to GO to improve the electrochemical performance of rGO/PANI composites. The maximum specific capacitance of rGO/PANI composites achieves 524.4 F/g with a mass ratio of aniline to GO 10:1 at a current density of 0.5 A/g, in comparison to the specific capacitance of 397 F/g at the same current density of pure PANI. Particularly, the specific capacity retention rate is 81.1% after 2000 cycles at 100 mv/s scan rate, which is an improvement over that of pure PANI (55.5%).

  15. A comparison study on the densification behavior and mechanical properties of gelcast vs conventionally formed B4C sintered conventionally and by microwaves

    International Nuclear Information System (INIS)

    Menchhofer, P.A.; Kiggans, J.O.; Morrow, M.S.; Schechter, D.E.

    1996-01-01

    The utilization of microwave energy for reaching high temperatures necessary to densify B 4 C powder is compared with conventional means of sintering by evaluating the mechanical properties after densification. Microwave energy has been shown to be an effective means for achieving high sintered densities, even though temperatures of ∼ 2,250 C are required. In this study, green preforms of B 4 C specimens were sintered by both conventional and microwave heating. This study also utilized an advanced forming method called ''Gelcasting'' developed at ORNL. Gelcasting is a fluid forming process whereby high solids suspensions of powders containing dissolved monomers are cast into a mold, then polymerized or ''gelled'' in situ. This investigation compares microstructures and mechanical properties of both Gelcast B 4 C and ''conventionally'' die-pressed B 4 C. The microstructures and final mechanical properties of B 4 C specimens are discussed

  16. Coarsening of Pd nanoparticles in an oxidizing atmosphere studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Chorkendorff, Ib; Dahl, Søren

    2016-01-01

    The coarsening of supported palladium nanoparticles in an oxidizing atmosphere was studied in situ by means of transmission electron microscopy (TEM). Specifically, the Pd nanoparticles were dispersed on a planar and amorphous Al2O3 support and were observed during the exposure to 10 mbar technical...... for the Ostwald ripening process indicates that the observed change in the particle size distribution can be accounted for by wetting of the Al2O3 support by the larger Pd nanoparticles....

  17. Influence of sintering parameters in the ferroelectric properties os strontium bismuth tantalate samples obtained by oxide mixture

    International Nuclear Information System (INIS)

    Souza, R.R. de; Pereira, A.S.; Sousa, V.C.; Egea, J.R.J.

    2012-01-01

    The family of compounds layered-type perovskite, know as Aurivilius presents great alternative not only by the absence of lead in the composition, but because the polarization retention, replacing PZT in FeRAM devices. The strontium bismuth tantalate (SrBi 2 Ta 2 O 9 ) or SBT is ferroelectric material that has attracted considerable interest, since it has high fatigue resistance, supporting high hysteresis loops, with the change in polarization.Checking polarization and depolarization currents stimulated by temperature it is possible to obtain, for example, information about the nature of charges and about the activation energy for the process of dielectric relaxation. For analysis of ferroelectric properties of this compound, it is essential to obtain specimens with a relative density around 95%. Thus, it is important the optimization of the sintering process in order to obtain a ceramic body with a high densification. The influence of sintering parameters to obtain SrBi 2 Ta 2 O 9 in the polarization properties and in the microstructure of sintered samples was investigated by thermostimulated currents and electronic microscopy, respectively. Results show that variation of these parameters may cause changes in the ferroelectric properties of the material. (author)

  18. Sintering of a class F fly ash

    Energy Technology Data Exchange (ETDEWEB)

    Joseph J. Biernacki; Anil K. Vazrala; H. Wayne Leimer [Tennessee Technological University, Cookeville, TN (United States). Department of Chemical Engineering

    2008-05-15

    The sinterability of a class F fly ash was investigated as a function of processing conditions including sintering temperature (1050-1200{sup o}C) and sintering time (0-90 min). Density, shrinkage, splitting tensile strength, water absorption and residual loss on ignition (RLOI) were evaluated as measures of sintering efficiency. Scanning electron microscopy (SEM), X-ray microanalysis and X-ray diffraction was used to examine microstructure and phase development due to processing. The results show that premature densification can inhibit complete carbon removal and that carbon combustion is influenced by both internal and external mass transfer conditions. 18 refs., 10 figs., 1 tab.

  19. In-situ GISAXS study on the oxidation behavior of liquid Ga on Ni(Cu)/Si substrates

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Weidong [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); Liu, Mingling [Department of Mechanical and Electrical Engineering, Qinhuangdao Institute of Technology, Qinhuangdao 066100 (China); Wu, Zhaojun [Department of Practice Teaching and Equipment Management, Qiqihar University, Qiqihar 161006 (China); Xing, Xueqing; Mo, Guang; Wu, Zhonghua [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Liu, Hong, E-mail: lhong68@sina.com.cn [School of Biomedical Engineering, Capital Medical University, Beijing 100069 (China)

    2015-11-01

    Liquid Ga could be used as a flexible heat-transfer medium or contact medium in the synchrotron-radiation-based instruments. The chemical stability of liquid Ga on other metal surface determines the serviceability of liquid Ga. In this paper, the oxidation evolutions of liquid Ga on Ni and Cu substrates have been investigated by in-situ grazing incidence small angle X-ray scattering (GISAXS) as a function of substrate temperature. The liquid Ga on Ni and Cu substrates shows different oxidation behaviors. A successive and slower oxidation from oxide clusters to oxide layer takes place with temperature increasing from 25 to 190 °C on the surface of the Ga/Ni/Si specimen, but a quick oxidation occurs on the entire surface of the Ga/Cu/Si specimen at the initial 25 °C. The subsequent heating increases the surface roughness of both liquid Ga, but increases simultaneously the surface curvature of the Ga/Cu/Si specimen. The understanding of the substrate-dependent oxidation behavior of liquid Ga is beneficial to its application as a heat-transfer medium.

  20. Sintering of nano crystalline o silicon carbide doping with

    Indian Academy of Sciences (India)

    Sinterable silicon carbide powders were prepared by attrition milling and chemical processing of an acheson type -SiC. Pressureless sintering of these powders was achieved by addition of aluminium nitride together with carbon. Nearly 99% sintered density was obtained. The mechanism of sintering was studied by ...

  1. Neutron powder investigations of Zr0.85Ca0.15O1.85 sinter material at temperatures up to 1100 K and with a simultaneously applied electric field

    International Nuclear Information System (INIS)

    Kahlert, H.; Boysen, H.; Frey, F.

    1998-01-01

    In situ neutron powder investigations of cubic stabilized zirconia [Zr 0.85 Ca 0.15 O 1.85 (CSZ15)] sinter material were performed at room temperature without an applied direct-current electric field and at 1100 K with and without an applied field, i.e. lasting ionic current. Experimental conditions (temperature, oxidizing atmosphere etc.) were chosen as close as possible to 'working conditions' of zirconia oxygen sensoric devices. To learn about field-induced structural changes and most probable ionic pathways, atomic displacement parameters were derived in the frame of a non-Gaussian Debye-Waller factor formalism for the oxygens. Probability-density-function maps and pseudo-potential (V eff ) maps indicate curved diffusion pathways of the oxygens close to the left angle 100 right angle directions. The action of the applied field is to lower the effective potential barriers. (orig.)

  2. Monitoring Sintering Burn-Through Point Using Infrared Thermography

    Directory of Open Access Journals (Sweden)

    Francisco G. Bulnes

    2013-08-01

    Full Text Available Sintering is a complex industrial process that applies heat to fine particles of iron ore and other materials to produce sinter, a solidified porous material used in blast furnaces. The sintering process needs to be carefully adjusted, so that the combustion zone reaches the bottom of the material just before the discharge end. This is known as the burnthrough point. Many different parameters need to be finely tuned, including the speed and the quantities of the materials mixed. However, in order to achieve good results, sintering control requires precise feedback to adjust these parameters. This work presents a sensor to monitor the sintering burn-through point based on infrared thermography. The proposed procedure is based on the acquisition of infrared images at the end of the sintering process. At this position, infrared images contain the cross-section temperatures of the mixture. The objective of this work is to process this information to extract relevant features about the sintering process. The proposed procedure is based on four steps: key frame detection, region of interest detection, segmentation and feature extraction. The results indicate that the proposed procedure is very robust and reliable, providing features that can be used effectively to control the sintering process.

  3. Luminescent hybrid lanthanide sulfates and lanthanide sulfonate-carboxylates with 1,10-phenanthroline involving in-situ oxidation of 2-mercaptonbenzoic acid

    International Nuclear Information System (INIS)

    Zhong, Jie-Cen; Wan, Fang; Sun, Yan-Qiong; Chen, Yi-Ping

    2015-01-01

    A series of lanthanide sulfates and lanthanide sulfonate-carboxylates, [Ln 2 (phen) 2 (SO 4 ) 3 (H 2 O) 2 ] n (I:Ln=Nd(1a), Sm(1b), Eu(1c), phen=1,10-phenanthroline) and [Ln(phen)(2-SBA)(BZA)] n (II: Ln=Sm(2a), Eu(2b), Dy(2c), 2-SBA=2-sulfobenzoate, BZA=benzoate) have been hydrothermally synthesized from lanthanide oxide, 2-mercaptonbenzoic acid with phen as auxiliary ligand and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectra, TG analyses and luminescence spectroscopy. Interestingly, SO 4 2− anions in I came from the in situ deep oxidation of thiol groups of 2-mercaptonbenzoic acid while 2-sulfobenzoate and benzoate ligands in II from the middle oxidation and desulfuration reactions of 2-mercaptonbenzoic acid. Compounds I are organic–inorganic hybrid lanthanide sulfates, which have rare one-dimensional column-like structures. Complexes II are binuclear lanthanide sulfonate-carboxylates with 2-sulfobenzoate and benzoate as bridges and 1,10-phenanthroline as terminal. Photoluminescence studies reveal that complexes I and II exhibit strong lanthanide characteristic emission bands in the solid state at room temperature. - Graphical abstract: Lanthanide sulfates and lanthanide sulfonate-carboxylates have been hydrothermally synthesized. Interestingly, sulfate anions, 2-sulfobenzoate and benzoate ligands came from the in situ oxidation and desulfuration reactions of 2-mercaptonbenzoic acid. - Highlights: • In situ oxidation and desulfuration reactions of 2-mercaptonbenzoic acid. • The organic–inorganic hybrid lanthanide sulfates with one-dimensional column-like structure. • The dinuclear lanthanide sulfonate-carboxylates. • The emission spectra exhibit the characteristic transition of 5 D 0 → 7 F J (J=0–4) of the Eu(III)

  4. Study of the Radical Chain Mechanism of Hydrocarbon Oxidation for In Situ Combustion Process

    Directory of Open Access Journals (Sweden)

    Alexandra Ushakova

    2017-01-01

    Full Text Available Despite the abundance of in situ combustion models of oil oxidation, many of the effects are still beyond consideration. For example, until now, initial stages of oxidation were not considered from a position of radical chain process. This is a serious difficulty for the simulation of oil recovery process that involves air injection. To investigate the initial stages of oxidation, the paper considers the sequence of chemical reactions, including intermediate short-living compounds and radicals. We have attempted to correlate the main stages of the reaction with areas of heat release observed in the experiments. The system of differential equations based on the equations of oxidation reactions was solved. Time dependence of peroxides formation and start of heat release is analytically derived for the initial stages. We have considered the inhibition of initial oxidation stages by aromatic oil compounds and have studied the induction time in dependence on temperature. Chain ignition criteria for paraffins and crude oil in presence of core samples were obtained. The calculation results are compared with the stages of oxidation that arise by high-pressure differential scanning calorimetry. According to experimental observations we have determined which reactions are important for the process and which can be omitted or combined into one as insignificant.

  5. The quantitative characterization of sintering of urania powders

    International Nuclear Information System (INIS)

    Das, P.; Kulkarni, U.D.

    1981-01-01

    This paper presents a unified approach towards characterization of the sintering behaviour of UO 2 powders in terms of their extrinsic properties. Empirical equations connecting the sintering index with various powder parameters have been set up. The influence of various powder parameters, either individually or as dimensionless/dimensional groups, on the sintering behaviour has been studied. The relative importance of these factors has also been analysed. A good polynomial fit has been obtained for variation of sintering index with some of the powder parameters and dimensionless/dimensional groups. The equations are expected to provide a good basis for assessing the sinterability of UO 2 powders. (Auth.)

  6. Improving NASICON Sinterability through Crystallization under High-Frequency Electrical Fields

    Energy Technology Data Exchange (ETDEWEB)

    Lisenker, Ilya; Stoldt, Conrad R., E-mail: stoldt@colorado.edu [Department of Mechanical Engineering, University of Colorado Boulder, Boulder, CO (United States)

    2016-03-31

    The effect of high-frequency (HF) electric fields on the crystallization and sintering rates of a lithium aluminum germanium phosphate (LAGP) ion conducting ceramic was investigated. LAGP with the nominal composition Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} was crystallized and sintered, both conventionally and under effect of electrical field. Electrical field application, of 300 V/cm at 1 MHz, produced up to a 40% improvement in sintering rate of LAGP that was crystallized and sintered under the HF field. Heat sink effect of the electrodes appears to arrest thermal runaway and subsequent flash behavior. Sintered pellets were characterized using X-ray diffraction, scanning electron microscope, TEM, and electrochemical impedance spectroscopy to compare conventionally and field-sintered processes. The as-sintered structure appears largely unaffected by the field as the sintering curves tend to converge beyond initial stages of sintering. Differences in densities and microstructure after 1 h of sintering were minor with measured sintering strains of 31 vs. 26% with and without field, respectively. Ionic conductivity of the sintered pellets was evaluated, and no deterioration due to the use of HF field was noted, though capacitance of grain boundaries due to secondary phases was significantly increased.

  7. Effects of surrounding powder in sintering process on the properties of Sb and Mn- doped barium-strontium titanate PTCR ceramics

    Directory of Open Access Journals (Sweden)

    Pornsuda Bomlai

    2006-05-01

    Full Text Available In this research, the effects of surrounding powder used during sintering of Sb and Mn doped bariumstrontium titanate (BST ceramics were studied. The ceramic samples were prepared by a conventional mixed-oxide method and placed on different powders during sintering. Phase formation, microstructure and PTCR behavior of the samples were then observed. Microstructures and PTCR behavior varied with the type of surrounding powder, whereas the crystal structure did not change. The surrounding powder has more effects on the shape of the grain than on the size. The grain size of samples was in the range of 5-20 μm. The most uniform grain size and the highest increase of the ratio of ρmax/ρRT were found to be about 106 for samples which had been sintered on Sb-doped BST powder. This value was an order of magnitude greater than for samples sintered on a powder of the equivalent composition to that of the sample pellet.

  8. Sintering of B4C powder obtained by a modified carbo-thermal reaction

    International Nuclear Information System (INIS)

    Rocha, R.M.; Kazumi, M.H.; Goncalves, D.P.; Melo, F.C.L.

    2005-01-01

    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 4 C is commercially manufactured by the carbo-thermal reduction of a mixture of boron oxide (B 2 O 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 2 O 2 . Thus, a modified carbo-thermal reaction is applied with an excess B 2 O 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 2 O 3 excess synthesized at 1700 deg. C/15 min. (authors)

  9. Effect of sintering conditions on the microstructural and mechanical characteristics of porous magnesium materials prepared by powder metallurgy.

    Science.gov (United States)

    Čapek, Jaroslav; Vojtěch, Dalibor

    2014-02-01

    There has recently been an increased demand for porous magnesium materials in many applications, especially in the medical field. Powder metallurgy appears to be a promising approach for the preparation of such materials. Many works have dealt with the preparation of porous magnesium; however, the effect of sintering conditions on material properties has rarely been investigated. In this work, we investigated porous magnesium samples that were prepared by powder metallurgy using ammonium bicarbonate spacer particles. The effects of the purity of the argon atmosphere and sintering time on the microstructure (SEM, EDX and XRD) and mechanical behaviour (universal loading machine and Vickers hardness tester) of porous magnesium were studied. The porosities of the prepared samples ranged from 24 to 29 vol.% depending on the sintering conditions. The purity of atmosphere played a significant role when the sintering time exceeded 6h. Under a gettered argon atmosphere, a prolonged sintering time enhanced diffusion connections between magnesium particles and improved the mechanical properties of the samples, whereas under a technical argon atmosphere, oxidation at the particle surfaces caused deterioration in the mechanical properties of the samples. These results suggest that a refined atmosphere is required to improve the mechanical properties of porous magnesium. © 2013.

  10. Effect of rigid inclusions on sintering

    International Nuclear Information System (INIS)

    Rahaman, M.N.; De Jonghe, L.C.

    1988-01-01

    The predictions of recent theoretical studies on the effect of inert, rigid inclusions on the sintering of ceramic powder matrices are examined and compared with experimental data. The densification of glass matrix composites with inclusion volume fractions of ≤0.15 can be adequately explained by Scherer's theory for viscous sintering with rigid inclusions. Inclusions cause a vast reduction in the densification rates of polycrystalline matrix composites even at low inclusion volume fractions. Models put forward to explain the sintering of polycrystalline matrix composites are discussed

  11. Experimental Investigation of In Situ Cleanable or Regenerative Filters for High Level Radioactive Waste Tanks

    International Nuclear Information System (INIS)

    Adamson, D.J.

    2000-01-01

    The Westinghouse Savannah River Company, located at the Savannah River Site (SRS) in Aiken, South Carolina, is currently testing two types of filter media for application as in situ regenerable/cleanable filters on high-level radioactive liquid waste tanks. Each of the 1.3 million-gallon tanks is equipped with an exhaust ventilation system to provide tank ventilation and to maintain the tank contents at approximately 1-in. water gauge vacuum to prevent the release of radioactive material to the environment. These systems are equipped with conventional, disposable, glass-fiber, High Efficiency Particulate Air (HEPA) filters that require frequent removal, replacement, and disposal. The need for routine replacements is often caused by accelerated filter loading due to the moist operating environment, which structurally weakens the filter media. This is not only costly, but subjects site personnel to radiation exposure and possible contamination. The types of filter media tested, as part of a National Energy Technology Laboratory procurement, were sintered metal and monolith ceramic. The media were subjected to a hostile environment to simulate conditions that challenge the tank ventilation systems. The environment promoted rapid filter plugging to maximize the number of filter loading/cleaning cycles that would occur in a specified period of time. The filters were challenged using non-radioactive, simulated high level waste materials and atmospheric dust, as these materials are most responsible for filter pluggage in the field. The filters were cleaned/regenerated in situ using an aqueous solution of dilute (10% volume) nitric acid. The study found that both filter media were insensitive to high humidity or moisture conditions and were easily cleaned in situ. The filters regenerated to approximately clean filter status even after numerous plugging and cleaning cycles. The filters were leak tested using poly alpha olefin aerosol at the beginning, middle, and end of the

  12. Low temperature sintering of fluorapatite glass-ceramics

    Science.gov (United States)

    Denry, Isabelle; Holloway, Julie A.

    2014-01-01

    Fluorapatite glass-ceramics have been shown to be excellent candidates as scaffold materials for bone grafts, however, scaffold production by sintering is hindered by concurrent crystallization of the glass. Our goal was to investigate the effect of Ca/Al ratio on the sintering behavior of Nb-doped fluorapatite-based glasses in the SiO2-Al2O3-P2O5-MgO-Na2O-K2O-CaO-CaF2 system. Glass compositions with Ca/Al ratio of 1 (A), 2 (B), 4 (C) and 19 (D) were prepared by twice melting at 1525°C for 3h. Glasses were either cast as cylindrical ingots or ground into powders. Disc-shaped specimens were prepared by either sectioning from the ingots or powder-compacting in a mold, followed by heat treatment at temperatures ranging between 700 and 1050°C for 1h. The density was measured on both sintered specimens and heat treated discs as controls. The degree of sintering was determined from these measurements. XRD showed that fluorapatite crystallized in all glass-ceramics. A high degree of sintering was achieved at 775°C for glass-ceramic D (98.99±0.04%), and 900°C for glass-ceramic C (91.31±0.10). Glass-ceramics A or B were only partially sintered at 1000°C (63.6±0.8% and 74.1±1.5%, respectively). SEM revealed a unique microstructure of micron-sized spherulitic fluorapatite crystals in glass-ceramics C and D. Increasing the Ca/Al ratio promoted low temperature sintering of fluorapatite glass-ceramics, which are traditionally difficult to sinter. PMID:24252652

  13. Characterization of oxidation resistance of stainless steels at high temperature by metallographic examinations and in-situ electrical resistance measurements; Charakterisierung der Oxidationsbestaendigkeit in nichtrostenden Staehlen bei hoher Temperatur durch Metallographische Untersuchungen und In-Situ-Messungen des elektrischen Widerstands

    Energy Technology Data Exchange (ETDEWEB)

    Bruncko, Mihael; Rudolf, Rebeka; Anzel, Ivan [Maribor Univ. (Slovenia). Faculty of Mechanical Engineering; Mehrabi, Kambiz [Pankl Drivetrain Systems GmbH und Co. KG, Kapfenberg (Austria); Kneissl, Albert C. [Leoben Univ. (Austria). Dept. of Physical Metallurgy and Materials Testing

    2013-07-01

    Practically all metals and alloys survive high-temperature exposure by growing oxide scales and/or by precipitation of the oxide particles in the matrix. Formed products can grow in shape of external oxide layers on surfaces, or as discrete oxide particles precipitated in a metal matrix. The first case represents external oxidation, and the other case is called internal oxidation. These processes are very important, because they determine the properties and applicability of metallic materials. Generally, they are undesired, because they cause deterioration of the mechanical properties and decomposition of metallic material. On the other side, the controlled process of external oxidation could be used for formation of protective coatings and the internal oxidation for dispersion strengthening of materials. In this paper we present monitoring of high-temperature oxidation of X12Cr13 stainless steel by in-situ electrical resistance measurements at different annealing temperatures in the air atmosphere. We determined the kinetics of oxide scale formation and its morphology with additional metallographic examination made by optical and scanning electron microscopy. The results of this research work show that in-situ monitoring and characterization of high-temperature oxidation present a strong tool that will contribute to a better fundamental understanding of the phenomena that occur during high-temperature oxidation of metallic materials. (orig.)

  14. Effects of in situ plasma treatment on optical and electrical properties of index-matched transparent conducting oxide layer

    International Nuclear Information System (INIS)

    Lim, Yong Hwan; Yoo, Hana; Choi, Bum Ho; Kim, Young Baek; Lee, Jong Ho; Shin, Dong Chan

    2010-01-01

    We investigated the effects of in situ plasma-treatment on optical and electrical properties of index-matched indium tin oxide (IMITO) thin film. To render the IMITO-coated surface hydrophilic and study the optical and electrical characteristics, we performed in situ oxygen plasma post-treatment without breaking vacuum. The 94.6% transmittance in the visible wavelength range (400-700 nm) increased on average to 96.4% and the maximum transmittance reached 98% over a broad wavelength range. The surface roughness and sheet resistance improved from 0.9 nm and 200 Ω/sq to 0.0905 nm and 100 Ω/sq, respectively, by in situ plasma post-treatment. We confirmed by contact angle measurement that the hydrophobic IMITO surface was altered to hydrophilic. The improved optical and electrical characteristics of in situ plasma-treated IMITO makes it adequate for high-resolution liquid crystal on silicon displays.

  15. A finite difference model of the iron ore sinter process

    OpenAIRE

    Muller, J.; de Vries, T.L.; Dippenaar, B.A.; Vreugdenburg, J.C.

    2015-01-01

    Iron ore fines are agglomerated to produce sinter, which is an important feed material for blast furnaces worldwide. A model of the iron ore sintering process has been developed with the objective of being representative of the sinter pot test, the standard laboratory process in which the behaviour of specific sinter feed mixtures is evaluated. The model aims to predict sinter quality, including chemical quality and physical strength, as well as key sinter process performance parameters such ...

  16. Study of scrap recovery for mixed oxide pellet by means of UO2+5wt.%CeO2

    International Nuclear Information System (INIS)

    Joung, Chang Young; Kim, Si Hyung; Kim, Han Soo; Lee, Yong Woo

    2000-01-01

    The recovery method of scrap powder was established using UO 2 -5wt.%CeO 2 powder in the way of of technology development of scrap recovery and recycle in the mixed oxide pellet fabrication process. And pellet density and microstructure, which depend on quantity of scrap, powder treatment method, and sintering condition, was analyzed. As a result of oxidation of sintered pellet in the air the powdering at below 400 degrees C occurred smoothly, and at above 400 degrees C powdering process was not proceeding well as temperature increased and powder particle size grew bigger. M 3 O 8 scrap powder which was powdered through oxidation method was added to UO 2 -5wt.%CeO 2 mixed powder. The results after the powder was treated by means of mixing, crushing, attrition milling, pelletizing, and sintering showed that its density and grain size in the case of reductive sintering decreased as scrap addition increased, but the result in the case of crushing showed increase in grain size. In attrition milling case both density and grain size showed the tendency of increase, particularly grain size grew up to 12 μm. In the oxidative sintering with scrap added mixed powder sintering was accelerated under the oxygen environment and the effect of powder treatment showed the tendency of relatively decreasing. (Hong, J. S.)

  17. Design of sintering-stable heterogeneous catalysts

    DEFF Research Database (Denmark)

    Gallas-Hulin, Agata

    One of the major issues in the use of metal nanoparticles in heterogeneous catalysis is sintering. Sintering occurs at elevated temperatures because of increased mobility of nanoparticles, leading to their agglomeration and, as a consequence, to the deactivation of the catalyst. It is an emerging...... problem especially for the noble metals-based catalysis. These metals being expensive and scarce, it is worth developing catalyst systems which preserve their activity over time. Encapsulation of nanoparticles inside zeolites is one of the ways to prevent sintering. Entrapment of nanoparticles inside...

  18. Second-Order Biomimicry: In Situ Oxidative Self-Processing Converts Copper(I)/Diamine Precursor into a Highly Active Aerobic Oxidation Catalyst.

    Science.gov (United States)

    McCann, Scott D; Lumb, Jean-Philip; Arndtsen, Bruce A; Stahl, Shannon S

    2017-04-26

    A homogeneous Cu-based catalyst system consisting of [Cu(MeCN) 4 ]PF 6 , N , N '-di- tert -butylethylenediamine (DBED), and p -( N , N -dimethylamino)pyridine (DMAP) mediates efficient aerobic oxidation of alcohols. Mechanistic study of this reaction shows that the catalyst undergoes an in situ oxidative self-processing step, resulting in conversion of DBED into a nitroxyl that serves as an efficient cocatalyst for aerobic alcohol oxidation. Insights into this behavior are gained from kinetic studies, which reveal an induction period at the beginning of the reaction that correlates with the oxidative self-processing step, EPR spectroscopic analysis of the catalytic reaction mixture, which shows the buildup of the organic nitroxyl species during steady state turnover, and independent synthesis of oxygenated DBED derivatives, which are shown to serve as effective cocatalysts and eliminate the induction period in the reaction. The overall mechanism bears considerable resemblance to enzymatic reactivity. Most notable is the "oxygenase"-type self-processing step that mirrors generation of catalytic cofactors in enzymes via post-translational modification of amino acid side chains. This higher-order function within a synthetic catalyst system presents new opportunities for the discovery and development of biomimetic catalysts.

  19. Physical deoxygenation of graphene oxide paper surface and facile in situ synthesis of graphene based ZnO films

    International Nuclear Information System (INIS)

    Ding, Jijun; Wang, Minqiang; Zhang, Xiangyu; Ran, Chenxin; Shao, Jinyou; Ding, Yucheng

    2014-01-01

    In-situ sputtering ZnO films on graphene oxide (GO) paper are used to fabricate graphene based ZnO films. Crystal structure and surface chemical states are investigated. Results indicated that GO paper can be effectively deoxygenated by in-situ sputtering ZnO on them without adding any reducing agent. Based on the principle of radio frequency magnetron sputtering, we propose that during magnetron sputtering process, plasma streams contain large numbers of electrons. These electrons not only collide with argon atoms to produce secondary electrons but also they are accelerated to bombard the substrates (GO paper) resulting in effective deoxygenation of oxygen-containing functional groups. In-situ sputtering ZnO films on GO paper provide an approach to design graphene-semiconductor nanocomposites

  20. Sintering of anorthite based ceramics prepared from kaolin DD2 and calcite

    Energy Technology Data Exchange (ETDEWEB)

    Zaiou, S.; Harabi, A.; Harabi, E.; Guechi, A.; Karboua, N.; Benhassine, M.-T.; Zouai, S.; Guerfa, F., E-mail: Zaiou_21@yahoo.fr, E-mail: harabi52@gmail.com, E-mail: semouni84@gmail.com, E-mail: guechia@yahoo.fr, E-mail: kanour17@yahoo.fr, E-mail: mtb25dz@gmail.com, E-mail: zouaisouheila@yahoo.fr, E-mail: guerfatiha@gmail.com [Ceramics Lab., Faculty of Exact Science, Physics Department, Mentouri University of Constantine (Algeria)

    2016-10-15

    In this work, the preparation of anorthite based ceramics using a modified milling system and 80 wt% kaolin (DD2 type) and 20 wt% calcium oxide extracted from CaCO{sub 3} is shown. The choice of these raw materials was dictated by their natural abundance. Previous studies have shown that a simple and vibratory multidirectional milling system using a bimodal distribution of highly resistant ceramics can be successfully used for obtaining fine powders. The prepared samples were sintered at different temperatures ranging between 800 and 1100 °C. It has been found that the relative density of samples sintered at 900 °C for 1 h with a heating rate of 5 °C/min was about 96% of the theoretical density of anorthite (2.75 g/cm{sup 3} ). Finally, the prepared samples were also characterized by scanning electron microscopy, X-ray diffraction and Raman spectroscopy. (author)

  1. Sintering of anorthite based ceramics prepared from kaolin DD2 and calcite

    Directory of Open Access Journals (Sweden)

    S. Zaiou

    Full Text Available Abstract In this work, the preparation of anorthite based ceramics using a modified milling system and 80 wt% kaolin (DD2 type and 20 wt% calcium oxide extracted from CaCO3 is shown. The choice of these raw materials was dictated by their natural abundance. Previous studies have shown that a simple and vibratory multidirectional milling system using a bimodal distribution of highly resistant ceramics can be successfully used for obtaining fine powders. The prepared samples were sintered at different temperatures ranging between 800 and 1100 °C. It has been found that the relative density of samples sintered at 900 °C for 1 h with a heating rate of 5 °C/min was about 96% of the theoretical density of anorthite (2.75 g/cm3. Finally, the prepared samples were also characterized by scanning electron microscopy, X-ray diffraction and Raman spectroscopy.

  2. Sintering of anorthite based ceramics prepared from kaolin DD2 and calcite

    International Nuclear Information System (INIS)

    Zaiou, S.; Harabi, A.; Harabi, E.; Guechi, A.; Karboua, N.; Benhassine, M.-T.; Zouai, S.; Guerfa, F.

    2016-01-01

    In this work, the preparation of anorthite based ceramics using a modified milling system and 80 wt% kaolin (DD2 type) and 20 wt% calcium oxide extracted from CaCO 3 is shown. The choice of these raw materials was dictated by their natural abundance. Previous studies have shown that a simple and vibratory multidirectional milling system using a bimodal distribution of highly resistant ceramics can be successfully used for obtaining fine powders. The prepared samples were sintered at different temperatures ranging between 800 and 1100 °C. It has been found that the relative density of samples sintered at 900 °C for 1 h with a heating rate of 5 °C/min was about 96% of the theoretical density of anorthite (2.75 g/cm 3 ). Finally, the prepared samples were also characterized by scanning electron microscopy, X-ray diffraction and Raman spectroscopy. (author)

  3. Development of iodine waste forms using low-temperature sintering glass

    International Nuclear Information System (INIS)

    Krumhansl, James Lee; Nenoff, Tina Maria; Garino, Terry J.; Rademacher, David

    2010-01-01

    This presentation will describe our recent work on the use of low temperature-sintering glass powders mixed with either AgI or AgI-zeolite to produce a stable waste form. Radioactive iodine ( 129 I, half-life of 1.6 x 10 7 years) is generated in the nuclear fuel cycle and is of particular concern due to its extremely long half-life and its effects on human health. As part of the DOE/NE Advanced Fuel Cycle Initiative (AFCI), the separation of 129 I from spent fuel during fuel reprocessing is being studied. In the spent fuel reprocessing scheme under consideration, the iodine is released in gaseous form and collected using Ag-loaded zeolites, to form AgI. Although AgI has extremely low solubility in water, it has a relatively high vapor pressure at moderate temperatures (>550 C), thus limiting the thermal processing. Because of this, immobilization using borosilicate glass is not feasible. Therefore, a bismuth oxide-based glasses are being studied due to the low solubility of bismuth oxide in aqueous solution at pH > 7. These waste forms were processed at 500 C, where AgI volatility is low but the glass powder is able to first densify by viscous sintering and then crystallize. Since the glass is not melted, a more chemically stable glass can be used. The AgI-glass mixture was found to have high iodine leach resistance in these initial studies.

  4. Enhanced performance of biodegradable poly(butylene succinate)/graphene oxide nanocomposites via in situ polymerization.

    Science.gov (United States)

    Wang, X W; Zhang, C-A; Wang, P L; Zhao, J; Zhang, W; Ji, J H; Hua, K; Zhou, J; Yang, X B; Li, X P

    2012-05-08

    Poly(butylene succinate) (PBS)/graphene oxide (GO) nanocomposites were facilely prepared via in situ polymerization. The properties of the nanocomposites were studied using FTIR, XRD, and (1)H NMR, and the state of dispersion of GO in the PBS matrix was examined by SEM. The crystallization and melting behavior of the PBS matrix in the presence of dispersed GO nanosheets have been studied by DSC and polarized optical microscopy. Through the mechnical testing machine and DMA, PBS/GO nanocomposites with 3% GO have shown a 43% increase in tensile strength and a 45% improvement in storage modulus. This high performance of the nanocomposites is mainly attributed to the high strength of graphene oxide combined with the strong interfacial interactions in the uniformly dispersed PBS/GO nanocomposites.

  5. Mechanistic studies of chemical looping desulfurization of Mn-based oxides using in situ X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    König, C.F.J.; Nachtegaal, M.; Seemann, M.; Clemens, F.; Garderen, N. van; Biollaz, S.M.A.; Schildhauer, T.J.

    2014-01-01

    Highlights: • Mn sorbents remove H 2 S from hot syngas in chemical looping desulfurization process. • State of Mn followed by in situ X-ray absorption spectroscopy and mass spectrometry. • Two-step mechanism explains the formation of SO 2 under reducing conditions. - Abstract: Cleaning of producer gas from biomass gasification is required for further processing, e.g. to avoid catalyst poisoning in subsequent conversion steps. High-temperature gas cleaning, of which sulfur removal is an important part, is a promising way to improve the overall efficiency of biomass conversion. In a high temperature “chemical looping desulfurization” process, a sorbent material, here manganese oxide, is cycled between producer gas from the gasifier to remove sulfur species, and an oxidizing atmosphere, in which the sulfur species are released as SO 2 . Alternatively, the use of such material as reactive bed material could be integrated into an allothermal dual fluidized bed gasifier. In a laboratory reactor, we subjected manganese-based materials to a periodically changing gas atmosphere, simulating a “chemical looping desulfurization” reactor. The “fuel reactor” gas contained H 2 , CO, CH 4 and H 2 S, similar as in the producer gas, and the “oxidizing reactor” contained diluted O 2 . Mass spectrometry showed that most of the H 2 S is taken up by the sample in the “fuel reactor” part, while also some unwanted SO 2 is generated in the “fuel reactor” part. Most of the sulfur is released in the oxidizing reactor. Simultaneous in situ X-ray absorption spectroscopy (XAS) of the Mn materials during different stages of the chemical looping desulfurization process showed that the initial Mn 3 O 4 is transformed in the presence of H 2 S to MnS via a MnO intermediate in the fuel reactor. Oxygen from the reduction of Mn 3 O 4 oxidizes some H 2 S to the undesired SO 2 in the fuel reactor. Upon exposure to O 2 , MnS is again oxidized to Mn 3 O 4 via MnO, releasing SO

  6. SINTERING EFFECTS ON THE DENSIFICATION OF NANOCRYSTALLINE HYDROXYAPATITE

    Directory of Open Access Journals (Sweden)

    M. Amiriyan

    2011-06-01

    Full Text Available The effects of sintering profiles on the densification behaviour of synthesized nanocrystalline hydroxyapatite (HA powder were investigated in terms of phase stability and mechanical properties. A wet chemical precipitation method was successfully employed to synthesize a high purity and single phase HA powder. Green HA compacts were prepared and subjected to sintering in air atmosphere over a temperature range of 700° C to 1300° C. In this study two different holding times were compared, i.e. 1 minute versus the standard 120 minutes. The results revealed that the 1 minute holding time sintering profile was indeed effective in producing a HA body with high density of 98% theoretical when sintered at 1200° C. High mechanical properties such as fracture toughness of 1.41 MPa.m1/2 and hardness of 9.5 GPa were also measured for HA samples sintered under this profile. Additionally, XRD analysis indicated that decomposition of the HA phase during sintering at high temperatures was suppressed.

  7. Improvement of mechanical strength of sintered Mo alloyed steel by optimization of sintering and cold-forging processes with densification

    Science.gov (United States)

    Kamakoshi, Y.; Shohji, I.; Inoue, Y.; Fukuda, S.

    2017-10-01

    Powder metallurgy (P/M) materials have been expected to be spread in automotive industry. Generally, since sintered materials using P/M ones contain many pores and voids, mechanical properties of them are inferior to those of conventional wrought materials. To improve mechanical properties of the sintered materials, densification is effective. The aim of this study is to improve mechanical strength of sintered Mo-alloyed steel by optimizing conditions in sintering and cold-forging processes. Mo-alloyed steel powder was compacted. Then, pre-sintering (PS) using a vacuum sintering furnace was conducted. Subsequently, coldforging (CF) by a backward extrusion method was conducted to the pre-sintered specimen. Moreover, the cold-forged specimen was heat treated by carburizing, tempering and quenching (CQT). Afterwards, mechanical properties were investigated. As a result, it was found that the density of the PS specimen is required to be more than 7.4 Mg/m3 to strengthen the specimen by heat treatment after CF. Furthermore, density and the microstructure of the PS specimen are most important factors to make the high density and strength material by CF. At the CF load of 1200 kN, the maximum density ratio reached approximately 99% by the use of the PS specimen with proper density and microstructure. At the CF load of 900 kN, although density ratio was high like more than 97.8%, transverse rupture strength decreased sharply. Since densification caused high shear stress and stress concentration in the surface layer, microcracks occurred by the damages of inter-particle sintered connection of the surface layer. On the contrary, in case of the CF load of 1200 kN, ultra-densification of the surface layer occurred by a sufficient plastic flow. Such sufficient compressed specimens regenerated the sintered connections by high temperature heat treatment and thus the high strength densified material was obtained. These processes can be applicable to near net shape manufacturing

  8. Tuning the structure of platinum particles on ceria in situ for enhancing the catalytic performance of exhaust gas catalysts

    International Nuclear Information System (INIS)

    Gaenzler, Andreas M.; Casapu, Maria; Grunwaldt, Jan-Dierk; Vernoux, Philippe; Loridant, Stephane; Cadete Santos Aires, Francisco J.; Epicier, Thierry; Betz, Benjamin; Hoyer, Ruediger

    2017-01-01

    A dynamic structural behavior of Pt nanoparticles on the ceria surface under reducing/oxidizing conditions was found at moderate temperatures (<500 C) and exploited to enhance the catalytic activity of Pt/CeO 2 -based exhaust gas catalysts. Redispersion of platinum in an oxidizing atmosphere already occurred at 400 C. A protocol with reducing pulses at 250-400 C was applied in a subsequent step for controlled Pt-particle formation. Operando X-ray absorption spectroscopy unraveled the different extent of reduction and sintering of Pt particles: The choice of the reductant allowed the tuning of the reduction degree/particle size and thus the catalytic activity (CO>H 2 >C 3 H 6 ). This dynamic nature of Pt on ceria at such low temperatures (250-500 C) was additionally confirmed by in situ environmental transmission electron microscopy. A general concept is proposed to adjust the noble metal dispersion (size, structure), for example, during operation of an exhaust gas catalyst. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Tuning the structure of platinum particles on ceria in situ for enhancing the catalytic performance of exhaust gas catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Gaenzler, Andreas M.; Casapu, Maria; Grunwaldt, Jan-Dierk [Institute for Chemical Technology and Polymer Chemistry (ITCP), Karlsruhe Institute of Technology (KIT), Karlsruhe (Germany); Vernoux, Philippe; Loridant, Stephane; Cadete Santos Aires, Francisco J. [Institut de Recherches sur la Catalyse et l' Environnement de Lyon, UMR 5256, CNRS, Universite Claude Bernard Lyon 1, Universite de Lyon, Villeurbanne (France); Epicier, Thierry [Materiaux, Ingenierie et Science, UMR 5510, CNRS, INSA de Lyon, Universite de Lyon, Villeurbanne (France); Betz, Benjamin [Umicore AG and Co. KG, Hanau (Germany); Ernst-Berl Institut, Technische Universitaet Darmstadt (Germany); Hoyer, Ruediger [Umicore AG and Co. KG, Hanau (Germany)

    2017-10-09

    A dynamic structural behavior of Pt nanoparticles on the ceria surface under reducing/oxidizing conditions was found at moderate temperatures (<500 C) and exploited to enhance the catalytic activity of Pt/CeO{sub 2}-based exhaust gas catalysts. Redispersion of platinum in an oxidizing atmosphere already occurred at 400 C. A protocol with reducing pulses at 250-400 C was applied in a subsequent step for controlled Pt-particle formation. Operando X-ray absorption spectroscopy unraveled the different extent of reduction and sintering of Pt particles: The choice of the reductant allowed the tuning of the reduction degree/particle size and thus the catalytic activity (CO>H{sub 2}>C{sub 3}H{sub 6}). This dynamic nature of Pt on ceria at such low temperatures (250-500 C) was additionally confirmed by in situ environmental transmission electron microscopy. A general concept is proposed to adjust the noble metal dispersion (size, structure), for example, during operation of an exhaust gas catalyst. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  10. Sintering Behavior of Spark Plasma Sintered SiC with Si-SiC Composite Nanoparticles Prepared by Thermal DC Plasma Process

    Science.gov (United States)

    Yu, Yeon-Tae; Naik, Gautam Kumar; Lim, Young-Bin; Yoon, Jeong-Mo

    2017-11-01

    The Si-coated SiC (Si-SiC) composite nanoparticle was prepared by non-transferred arc thermal plasma processing of solid-state synthesized SiC powder and was used as a sintering additive for SiC ceramic formation. Sintered SiC pellet was prepared by spark plasma sintering (SPS) process, and the effect of nano-sized Si-SiC composite particles on the sintering behavior of micron-sized SiC powder was investigated. The mixing ratio of Si-SiC composite nanoparticle to micron-sized SiC was optimized to 10 wt%. Vicker's hardness and relative density was increased with increasing sintering temperature and holding time. The relative density and Vicker's hardness was further increased by reaction bonding using additional activated carbon to the mixture of micron-sized SiC and nano-sized Si-SiC. The maximum relative density (97.1%) and Vicker's hardness (31.4 GPa) were recorded at 1800 °C sintering temperature for 1 min holding time, when 0.2 wt% additional activated carbon was added to the mixture of SiC/Si-SiC.

  11. Low temperature sintering of fluorapatite glass-ceramics.

    Science.gov (United States)

    Denry, Isabelle; Holloway, Julie A

    2014-02-01

    Fluorapatite glass-ceramics have been shown to be excellent candidates as scaffold materials for bone grafts, however, scaffold production by sintering is hindered by concurrent crystallization of the glass. Objective, our goal was to investigate the effect of Ca/Al ratio on the sintering behavior of Nb-doped fluorapatite-based glasses in the SiO2-Al2O3-P2O5-MgO-Na2O-K2O-CaO-CaF2 system. Methods, glass compositions with Ca/Al ratio of 1 (A), 2 (B), 4 (C) and 19 (D) were prepared by twice melting at 1525°C for 3h. Glasses were either cast as cylindrical ingots or ground into powders. Disk-shaped specimens were prepared by either sectioning from the ingots or powder-compacting in a mold, followed by heat treatment at temperatures ranging between 700 and 1050°C for 1h. The density was measured on both sintered specimens and heat treated discs as controls. The degree of sintering was determined from these measurements. Results and Significance XRD showed that fluorapatite crystallized in all glass-ceramics. A high degree of sintering was achieved at 775°C for glass-ceramic D (98.99±0.04%), and 900°C for glass-ceramic C (91.31±0.10). Glass-ceramics A or B were only partially sintered at 1000°C (63.6±0.8% and 74.1±1.5%, respectively). SEM revealed a unique microstructure of micron-sized spherulitic fluorapatite crystals in glass-ceramics C and D. Increasing the Ca/Al ratio promoted low temperature sintering of fluorapatite glass-ceramics, which are traditionally difficult to sinter. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  12. Scanning transmission X-ray microscopy probe for in situ mechanism study of graphene-oxide-based resistive random access memory.

    Science.gov (United States)

    Nho, Hyun Woo; Kim, Jong Yun; Wang, Jian; Shin, Hyun-Joon; Choi, Sung-Yool; Yoon, Tae Hyun

    2014-01-01

    Here, an in situ probe for scanning transmission X-ray microscopy (STXM) has been developed and applied to the study of the bipolar resistive switching (BRS) mechanism in an Al/graphene oxide (GO)/Al resistive random access memory (RRAM) device. To perform in situ STXM studies at the C K- and O K-edges, both the RRAM junctions and the I0 junction were fabricated on a single Si3N4 membrane to obtain local XANES spectra at these absorption edges with more delicate I0 normalization. Using this probe combined with the synchrotron-based STXM technique, it was possible to observe unique chemical changes involved in the BRS process of the Al/GO/Al RRAM device. Reversible oxidation and reduction of GO induced by the externally applied bias voltages were observed at the O K-edge XANES feature located at 538.2 eV, which strongly supported the oxygen ion drift model that was recently proposed from ex situ transmission electron microscope studies.

  13. In-situ investigation of the calcination process of mixed oxide xerogels with Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Panitz, J C [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-06-01

    The controlled calcination of materials derived by sol-gel reactions is important for the evolution of the final structure. Raman spectroscopy is an ideal tool for the identification of surface species under in-situ conditions, as demonstrated in the following for the example of a molybdenum oxide-silica xerogel. Raman spectra of this particular sample were recorded at temperatures as high as 1173 K, and compared with those of a reference material.(author) 3 figs., 4 refs.

  14. Study of effect of dynamic mill treatment on the compaction and sintering of UO2-5wt%CeO2

    International Nuclear Information System (INIS)

    Na, S. H.; Kim, S. H.; Kim, Y. K.; Lee, Y. W.; Yoo, M. J.

    2002-01-01

    Some properties (apparent density, green density, sintered density and grain size) of the simulated mixed oxide(UO 2 -5wt%CeO 2 ) prepared by using the dynamic mill newly developed were investigated. As the dynamic milling time increases, these properties increase. However, the increases of sintered density and grain size were saturated above 2 hrs and 4 hrs of dynamic milling treatment, respectively. It appeared that the dynamic mill has a similar capability to that of other milling methods, and hence can manufacture the pellets having desired properties by controlling milling time

  15. A study of pressureless microwave sintering, microwave-assisted hot press sintering and conventional hot pressing on properties of aluminium/alumina nanocomposite

    Energy Technology Data Exchange (ETDEWEB)

    Abedinzadeh, Reza; Safavi, Seyed Mohsen; Karimzadeh, Fathallah [Isfahan University, Isfahan (Iran, Islamic Republic of)

    2016-05-15

    Bulk Al/4wt-%Al{sub 2}O{sub 3} nanocomposites were prepared by consolidating nanocomposite powders using pressureless microwave sintering, microwave-assisted hot press sintering and conventional hot pressing techniques. Microstructural observations revealed that the microwave-assisted hot press sintering at different sintering temperatures of 400.deg.C and 500.deg.C resulted in more densification and smaller grain size for Al/Al{sub 2}O{sub 3} nanocomposite as compared with the conventional hot pressing. Moreover, the application of pressure in microwave sintering process led to more densification and grain growth. Mechanical properties resulting from microhardness and nanoindentation tests were also compared between three-method processed samples. It was found that the microwave-assisted hot-pressed sample exhibited higher hardness and elastic modulus in comparison with microwave-sintered and conventional hot-pressed samples. The improvement in the mechanical properties can be ascribed to lower porosity of microwave-assisted hot-pressed sample.

  16. Shape distortion and thermo-mechanical properties of SOFC components from green tape to sintering body

    DEFF Research Database (Denmark)

    Teocoli, Francesca; Ni, De Wei; Tadesse Molla, Tesfaye

    due to binder burn out, differential shrinkage behavior and to a potential interfacial reaction between the two materials. To analyze the phenomena, shrinkage of SOFC components single layers and bilayered samples were measured insitu by optical dilatometer. The densification mismatch stress, due...... to the strain rate difference between materials, was calculated using Cai’s model. Camber (curvature) development for in situ co-firing of a bi-layer ceramic green tape has been investigated. Analysis of shape evolution from green to sintered body can be carried out by the thermo-mechanical analysis techniques....

  17. Heterogeneous burnable poisons. Sinterability study in oxidizing atmosphere of alumina-gadolinia and alumina-boron carbide compounds

    International Nuclear Information System (INIS)

    Agueda, H.C.; Leiva, S.F.; Russo, D.O.

    1990-01-01

    Solid burnable poisons are used in reactors cooled by pressure light water (PLWR) with the purpose of controlling initial reactivity in the first reactor's core. The burnable poisons may be uniformly mixed with the fuel -known as 'homogeneous' poisons-; or constituting separate elements -known as heterogeneous poisons-. The purpose of this work is to present the results of two sinterability studies, performed on Al 2 O 3 -Gd 2 O 3 and Al 2 O 3 -B 4 C, where alumina acts as inert matrix, storing the absorbing elements as Gd 2 O 3 or B 4 C. The elements were sintered at an air atmosphere and additives permitting the obtention of a greater density alumina were tested at lower temperatures than the characteristic for this material, in order to determine its compatibility with the materials dealt with herein. (Author) [es

  18. Effect Of Compaction Pressure And Sintering Temperature On The Liquid Phase Sintering Behavior Of Al-Cu-Zn Alloy

    Directory of Open Access Journals (Sweden)

    Lee S.H.

    2015-06-01

    Full Text Available The liquid phase sintering characteristics of Al-Cu-Zn alloy were investigated with respect to various powder metallurgy processing conditions. Powders of each alloying elements were blended to form Al-6Cu-5Zn composition and compacted with pressures of 200, 400, and 600 MPa. The sintering process was performed at various temperatures of 410, 560, and 615°C in N2 gas atmosphere. Density and micro-Vickers hardness measurements were conducted at different processing stages, and transverse rupture strength of sintered materials was examined for each condition, respectively. The microstructure was characterized using optical microscope and scanning electron microscopy. The effect of Zn addition on the liquid phase sintering behavior during P/M process of the Al-Cu-Zn alloy was also discussed in detail.

  19. High Temperature Oxidation of Spark Plasma Sintered and Thermally Sprayed FeAl-Based Iron Aluminides

    Czech Academy of Sciences Publication Activity Database

    Haušild, P.; Karlík, M.; Skiba, T.; Sajdl, P.; Dubský, Jiří; Palm, M.

    2012-01-01

    Roč. 122, č. 3 (2012), s. 465-468 ISSN 0587-4246. [International Symposium on Physics of Materials (ISPMA)/12./. Prague, 04.09.2011-08.09.2011] Institutional support: RVO:61389021 Keywords : thermal spraying * plasma sintering Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass Impact factor: 0.531, year: 2012

  20. High performance top-gated indium–zinc–oxide thin film transistors with in-situ formed HfO{sub 2} gate insulator

    Energy Technology Data Exchange (ETDEWEB)

    Song, Yang, E-mail: yang_song@brown.edu [Department of Physics, Brown University, 182 Hope Street, Providence, RI 02912 (United States); Zaslavsky, A. [Department of Physics, Brown University, 182 Hope Street, Providence, RI 02912 (United States); School of Engineering, Brown University, 184 Hope Street, Providence, RI 02912 (United States); Paine, D.C. [School of Engineering, Brown University, 184 Hope Street, Providence, RI 02912 (United States)

    2016-09-01

    We report on top-gated indium–zinc–oxide (IZO) thin film transistors (TFTs) with an in-situ formed HfO{sub 2} gate dielectric insulator. Building on our previous demonstration of high-performance IZO TFTs with Al{sub 2}O{sub 3}/HfO{sub 2} gate dielectric, we now report on a one-step process, in which Hf is evaporated onto the 20 nm thick IZO channel, forming a partially oxidized HfO{sub x} layer, without any additional insulator in-between. After annealing in air at 300 °C, the in-situ reaction between partially oxidized Hf and IZO forms a high quality HfO{sub 2} gate insulator with a low interface trapped charge density N{sub TC} ~ 2.3 × 10{sup 11} cm{sup −2} and acceptably low gate leakage < 3 × 10{sup −7} A/cm{sup 2} at gate voltage V{sub G} = 1 V. The annealed TFTs with gate length L{sub G} = 50 μm have high mobility ~ 95 cm{sup 2}/V ∙ s (determined via the Y-function technique), high on/off ratio ~ 10{sup 7}, near-zero threshold voltage V{sub T} = − 0.02 V, and a subthreshold swing of 0.062 V/decade, near the theoretical limit. The on-current of our proof-of-concept TFTs is relatively low, but can be improved by reducing L{sub G}, indicating that high-performance top-gated HfO{sub 2}-isolated IZO TFTs can be fabricated using a single-step in-situ dielectric formation approach. - Highlights: • High-performance indium–zinc–oxide (IZO) thin film transistors (TFTs). • Single-step in-situ dielectric formation approach simplifies fabrication process. • During anneal, reaction between HfO{sub x} and IZO channel forms a high quality HfO{sub 2} layer. • Gate insulator HfO{sub 2} shows low interface trapped charge and small gate leakage. • TFTs have high mobility, near-zero threshold voltage, and a low subthreshold swing.