Reduction mechanism of surface oxide films and characterization of formations on pulse electric-current sintered Al Mg alloy powders

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Song, Minghui; Mitsuishi, Kazutaka; Furuya, Kazuo

2005-02-01

The microstructure of interfaces between powder particles in Al-Mg alloy specimens sintered by pulse electric-current sintering (PECS) process was characterized using high resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDS). The crystalline precipitates with nano-size in the interface were observed in all of Al-Mg alloy specimens. The composition was determined to be MgAl 2O 4 or MgO, or both of them, which depended on Mg content in alloy powder and sintering temperature. The precipitates were suggested to contribute to reduction reaction of Mg with oxide films originally covered at powder particles surface.

Purification processes of xenogeneic bone substitutes and their impact on tissue reactions and regeneration.

PubMed

Perić Kačarević, Zeljka; Kavehei, Faraz; Houshmand, Alireza; Franke, Jörg; Smeets, Ralf; Rimashevskiy, Denis; Wenisch, Sabine; Schnettler, Reinhard; Jung, Ole; Barbeck, Mike

2018-04-01

Xenogeneic bone substitute materials are widely used in oral implantology. Prior to their clinical use, purification of the former bone tissue has to be conducted to ensure the removal of immunogenic components and pathogens. Different physicochemical methods are applied for purification of the donor tissue, and temperature treatment is one of these methods. Differences in these methods and especially the application of different temperatures for purification may lead to different material characteristics, which may influence the tissue reactions to these materials and the related (bone) healing process. However, little is known about the different material characteristics and their influences on the healing process. Thus, the aim of this mini-review is to summarize the preparation processes and the related material characteristics, safety aspects, tissue reactions, resorbability and preclinical and clinical data of two widely used xenogeneic bone substitutes that mainly differ in the temperature treatment: sintered (cerabone ® ) and non-sintered (Bio-Oss ® ) bovine-bone materials. Based on the summarized data from the literature, a connection between the material-induced tissue reactions and the consequences for the healing processes are presented with the aim of translation into their clinical application.

Mechanism research on arsenic removal from arsenopyrite ore during a sintering process

NASA Astrophysics Data System (ADS)

Cheng, Ri-jin; Ni, Hong-wei; Zhang, Hua; Zhang, Xiao-kun; Bai, Si-cheng

2017-04-01

The mechanism of arsenic removal during a sintering process was investigated through experiments with a sintering pot and arsenic-bearing iron ore containing arsenopyrite; the corresponding chemical properties of the sinter were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES), X-ray diffraction (XRD), and scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS). The experimental results revealed that the reaction of arsenic removal is mainly related to the oxygen atmosphere and temperature. During the sintering process, arsenic could be removed in the ignition layer, the sinter layer, and the combustion zone. A portion of FeAsS reacted with excess oxygen to generate FeAsO4, and the rest of the FeAsS reacted with oxygen to generate As2O3(g) and SO2(g). A portion of As2O3(g) mixed with Al2O3 or CaO, which resulted in the formation of arsenates such as AlAsO4 and Ca3(AsO4)2, leading to arsenic residues in sintering products. The FeAsS component in the blending ore was difficult to decompose in the preliminary heating zone, the dry zone, or the bottom layer because of the relatively low temperatures; however, As2O3(g) that originated from the high-temperature zone could react with metal oxides, resulting in the formation of arsenate residues.

Synthesis of Y1BaCu3O(x) superconducting powders by intermediate phase reactions

NASA Technical Reports Server (NTRS)

Moure, C.; Fernandez, J. F.; Tartaj, J.; Recio, P.; Duran, P.

1991-01-01

A procedure for synthesizing Y1Ba2Cu3O(x) by solid state reactions was developed. The method is based on the use of barium compounds, previously synthesized, as intermediate phases for the process. The reaction kinetics of this procedure were established between 860 C and 920 C. The crystal structure and the presence of second phases were studied by means of XRD. The sintering behavior and ceramic parameters were also determined. The orthorhombic type-I structure was obtained on the synthesized bodies after a cooling cycle in an air atmosphere. Superconducting transition took place at 91 K. Sintering densities higher than 95 percent D sub th were attained at temperatures below 940 C.

Low-Temperature Sintering Behavior (≤ 400°C) of Micro-sized Silver Particles Decorated by Silver Nanoparticles Through Surface Iodination

NASA Astrophysics Data System (ADS)

Zhou, Jian; Tang, Hongbo

2018-05-01

This paper introduces a facile and effective route to decorate micro-sized silver particle surfaces with Ag/AgI nanoclusters through a wet chemical reaction at room temperature using iodine and ethanol as reactant and solvent, respectively. Photosensitivity of AgI is utilized in the route, and AgI decomposes into Ag upon contact with sunshine, forming Ag/AgI nanoclusters. The modified micro-sized Ag particles showed sinterability even at 200°C and formed rigid electrical conductive networks at 350°C. Moreover, sintered film containing the modified Ag particles reached the best conductivity, 9.35 mΩ/sq, after sintering at 350°C for 20 min, while the film with untreated control Ag particles obtained its best conductivity at 400°C. The excellent sinterability should be attributed to the nanoclusters which served as a sintering aid during the heating process. However, increase of sintering temperature and time destroyed densification and conductivity of the sintered film containing the modified particles.

Melt-Infiltration Process For SiC Ceramics And Composites

NASA Technical Reports Server (NTRS)

Behrendt, Donald R.; Singh, Mrityunjay

1994-01-01

Reactive melt infiltration produces silicon carbide-based ceramics and composites faster and more economically than do such processes as chemical vapor infiltration (CVI), reaction sintering, pressureless sintering, hot pressing, and hot isostatic pressing. Process yields dense, strong materials at relatively low cost. Silicon carbide ceramics and composites made by reactive melt infiltration used in combustor liners of jet engines and in nose cones and leading edges of high-speed aircraft and returning spacecraft. In energy industry, materials used in radiant-heater tubes, heat exchangers, heat recuperators, and turbine parts. Materials also well suited to demands of advanced automobile engines.

The effect of preparation conditions on the structure and mechanical properties of reaction-sintered silicon nitride

NASA Technical Reports Server (NTRS)

Heinrich, J.

1980-01-01

The microstructure of reaction sintered silicon nitride (RSSN) was changed over a wide range by varying the grain density, grain size of the silicon starting powder, nitriding conditions, and by introducing artificial pores. The influence of single microstructural parameters on mechanical properties like room temperature strength, creep behavior, and resistance to thermal shock was investigated. The essential factors influencing these properties were found to be total porosity, pore size distribution, and the fractions of alpha and beta Si3N4. In view of high temperature engineering applications of RSSN, potentials for optimizing the material's properties by controlled processing are discussed.

Preparation and Properties of (YCa)(TiMn)O3−δ Ceramics Interconnect of Solid Oxide Fuel Cells

PubMed Central

Liou, Yi-Cheng; Tsai, Wen-Chou; Yen, Hao-Hsuan; Chang, Yung-Chia

2015-01-01

(YCa)(TiMn)O3–δ ceramics prepared using a reaction-sintering process were investigated. Without any calcination involved, the mixture of raw materials was pressed and sintered directly. Y2Ti2O7 instead of YTiO3 formed when a mixture of Y2O3 and TiO2 with Y/Ti ratio 1/1 were sintered in air. Y2Ti2O7, YTiO2.085 and some unknown phases were detected in Y0.6Ca0.4Ti0.6Mn0.4O3–δ. Monophasic Y0.6Ca0.4Ti0.4Mn0.6O3–δ ceramics were obtained after 1400–1500 °C sintering. Dense Y0.6Ca0.4Ti0.4Mn0.6O3–δ with a density 4.69 g/cm3 was observed after 1500 °C/4 h sintering. Log σ for Y0.6Ca0.4Ti0.6Mn0.4O3–δ increased from –3.73 Scm–1 at 350 °C to –2.14 Scm–1 at 700 °C. Log σ for Y0.6Ca0.4Ti0.4Mn0.6O3–δ increased from –2.1 Scm–1 at 350 °C to –1.36 Scm–1 at 700 °C. Increasing Mn content decreased activation energy Ea and increased electrical conductivity. Reaction-sintering process is proved to be a simple and effective method to obtain (YCa)(TiMn)O3–δ ceramics for interconnects in solid oxide fuel cells. PMID:28793436

Effect of microwave-assisted sintering on dielectric properties of CaCu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Rani, Suman; Ahlawat, Neetu; Punia, R.; Kundu, R. S.; Ahlawat, N.

2016-05-01

In this present work, CaCu3Ti4O12 (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It was observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.

Silicon nitride: A ceramic material with outstanding resistance to thermal shock and corrosion

NASA Technical Reports Server (NTRS)

Huebner, K. H.; Saure, F.

1983-01-01

The known physical, mechanical and chemical properties of reaction-sintered silicon nitride are summarized. This material deserves interest especially because of its unusually good resistance to thermal shock and corrosion at high temperatures. Two types are distinguished: reaction-sintered (porous) and hot-pressed (dense) Si3N4. Only the reaction-sintered material which is being produced today in large scale as crucibles, pipes, nozzles and tiles is considered.

Influence of the sintering temperature on the electrical properties of Ce-doped WO3 ceramics prepared from nano-powders

NASA Astrophysics Data System (ADS)

Dong, Liang; Chen, Han-Jun; Wang, Yu; Li, De-Zhu; Li, Tong-Ye; Zhao, Yong

2007-04-01

Using a nm-level powder fabricated by a wet chemical method as precursor, the CeO2-doped WO3 ceramics were prepared by the conventional solid state reaction at sintering temperatures from 600 to 1100 °C. The x-ray diffraction analysis reveals the coexistence of different WO3 phases in the samples sintered at temperatures below 900 °C, whereas a single phase appears in the samples sintered above 1000 °C. No new Ce-W compound appears. As the sintering temperature increases, the electrical properties of the samples display an interesting transformation from linear to nonlinear behaviour. The measurements of scanning electron microscope, complex impedance and electrical stability indicate that a lot of grain boundary regions in the samples sintered at low temperatures strongly influences the electrical transportation. Therefore, the electrical nonlinearity is due to a basic process controlled by the back-to-back Schottky barriers at grain boundaries with suitable thickness as well as the coexistence of phases.

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

PubMed Central

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

Spinel formation for stabilizing simulated nickel-laden sludge with aluminum-rich ceramic precursors.

PubMed

Shih, Kaimin; White, Tim; Leckie, James O

2006-08-15

The feasibility of stabilizing nickel-laden sludge from commonly available Al-rich ceramic precursors was investigated and accomplished with high nickel incorporation efficiency. To simulate the process, nickel oxide was mixed alternatively with gamma-alumina, corundum, kaolinite, and mullite and was sintered from 800 to 1480 degrees C. The nickel aluminate spinel (NiAl2O4) was confirmed as the stabilization phase for nickel and crystallized with efficiencies greater than 90% for all precursors above 1250 degrees C and 3-h sintering. The nickel-incorporation reaction pathways with these precursors were identified, and the microstructure and spinel yield were investigated as a function of sintering temperature with fixed sintering time. This study has demonstrated a promising process for forming nickel spinel to stabilize nickel-laden sludge from a wide range of inexpensive ceramic precursors, which may provide an avenue for economically blending waste metal sludges via the building industry processes to reduce the environmental hazards of toxic metals. The correlation of product textures and nickel incorporation efficiencies through selection of different precursors also provides the option of tailoring property-specific products.

A novel in situ synthesis of SiBCN-Zr composites prepared by a sol-gel process and spark plasma sintering.

PubMed

Miao, Yang; Yang, Zhihua; Liang, Bin; Li, Quan; Chen, Qingqing; Jia, Dechang; Cheng, Yi-Bing; Zhou, Yu

2016-08-09

In the work reported here, SiBCN amorphous powders were first prepared by a mechanical alloying technique, employing cubic silicon, graphite and hexagonal boron nitride powders as raw materials. Zirconia was then introduced via sol-gel methods. The resulting powder composite was then consolidated via SPS sintering. The SPS sintering sample was evaluated using XRD, SEM and TEM. XRD reveals a chemical transformation wherein amorphous BN(C) and ZrO2 form the primary ZrC and ZrB2 phases after SPS processing along with SiC and BN(C). Thereafter ZrC reacts with BN(C) completely to form ZrB2. The reaction starts at the temperature of 1500 °C and is complete at the temperature of 1900 °C. The fracture toughness of the sintered composites reaches 4.9 ± 0.2 MPa m(1/2) due to the presence of the laminated structure of the BN(C) phase.

Characterisation of titanium-titanium boride composites processed by powder metallurgy techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Selva Kumar, M., E-mail: sel_mcet@yahoo.co.in; Chandrasekar, P.; Chandramohan, P.

2012-11-15

In this work, a detailed characterisation of titanium-titanium boride composites processed by three powder metallurgy techniques, namely, hot isostatic pressing, spark plasma sintering and vacuum sintering, was conducted. Two composites with different volume percents of titanium boride reinforcement were used for the investigation. One was titanium with 20% titanium boride, and the other was titanium with 40% titanium boride (by volume). Characterisation was performed using X-ray diffraction, electron probe micro analysis - energy dispersive spectroscopy and wavelength dispersive spectroscopy, image analysis and scanning electron microscopy. The characterisation results confirm the completion of the titanium boride reaction. The results reveal themore » presence of titanium boride reinforcement in different morphologies such as needle-shaped whiskers, short agglomerated whiskers and fine plates. The paper also discusses how mechanical properties such as microhardness, elastic modulus and Poisson's ratio are influenced by the processing techniques as well as the volume fraction of the titanium boride reinforcement. - Highlights: Black-Right-Pointing-Pointer Ti-TiB composites were processed by HIP, SPS and vacuum sintering. Black-Right-Pointing-Pointer The completion of Ti-TiB{sub 2} reaction was confirmed by XRD, SEM and EPMA studies. Black-Right-Pointing-Pointer Hardness and elastic properties of Ti-TiB composites were discussed. Black-Right-Pointing-Pointer Processing techniques were compared with respect to their microstructure.« less

Al{sub 2}O{sub 3} - TiO{sub 2}-A simple sol-gel strategy to the synthesis of low temperature sintered alumina-aluminium titanate composites through a core-shell approach

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jayasankar, M.; Ananthakumar, S.; Mukundan, P.

A simple sol-gel based core-shell approach for the synthesis of alumina-aluminium titanate composite is reported. Alumina is the core and titania is the shell. The coating of titania has been performed in aqueous medium on alumina particle by means of heterocoagulation of titanyl chloride. Further heat treatment results in low temperature formation of aluminium titanate as well as low temperature sintering of alumina-aluminium titanate composites. The lowering of the reaction temperature can be attributed to the maximisation of the contact surface between the reactants due to the core-shell approach involving nanoparticles. The mechanism of formation of aluminium titanate and themore » observations on densification features in the present process are compared with that of mixture of oxides under identical conditions. The sintered alumina-aluminium titanate composite has an average grain size of 2 {mu}m. - Graphical abstract: The article presents a simple sol-gel process through core-shell approach to the synthesis of low temperature sintered alumina-aluminium titanate. The lowering of the reaction temperature can be attributed to the maximisation of the contact surface between the reactant due to the core-shell approach. This material showed the better microstructure control compared to the standard solid-state mixing route.« less

Tracking the shape-dependent sintering of platinum-rhodium model catalysts under operando conditions

NASA Astrophysics Data System (ADS)

Hejral, Uta; Müller, Patrick; Balmes, Olivier; Pontoni, Diego; Stierle, Andreas

2016-03-01

Nanoparticle sintering during catalytic reactions is a major cause for catalyst deactivation. Understanding its atomic-scale processes and finding strategies to reduce it is of paramount scientific and economic interest. Here, we report on the composition-dependent three-dimensional restructuring of epitaxial platinum-rhodium alloy nanoparticles on alumina during carbon monoxide oxidation at 550 K and near-atmospheric pressures employing in situ high-energy grazing incidence x-ray diffraction, online mass spectrometry and a combinatorial sample design. For platinum-rich particles our results disclose a dramatic reaction-induced height increase, accompanied by a corresponding reduction of the total particle surface coverage. We find this restructuring to be progressively reduced for particles with increasing rhodium composition. We explain our observations by a carbon monoxide oxidation promoted non-classical Ostwald ripening process during which smaller particles are destabilized by the heat of reaction. Its driving force lies in the initial particle shape which features for platinum-rich particles a kinetically stabilized, low aspect ratio.

Optimization of the dissolution of molybdenum disks. FY-16 results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tkac, Peter; Rotsch, David A.; Chemerisov, Sergey D.

2016-09-01

Argonne National Laboratory is providing technical development assistance to NorthStar Medical Technologies LLC in its pursuit of two pathways for production of molybdenum-99: the 98Mo(n,γ) 99Mo reaction and the photonuclear reaction, 100Mo(γ,n) 99Mo. Processing of irradiated targets, from either production mode, requires dissolution of the target material in H 2O 2 followed by a concentration step, addition of ferric ion to precipitate impurities, and conversion of the final solution to 5M potassium hydroxide solution of potassium molybdate. Currently, NorthStar is using pressed and sintered Mo disks as targets. Several options are being considered for the design of Mo targets formore » the production of 99Mo using the (γ,n) reaction. In the current design, the target holder contains a series of sintered Mo disks lined up perpendicular to two incident electron beams, one entering from each side of the target stack. In this configuration, the front-most disks absorb most of the heat from the electron beam and need to be thinner to allow for better cooling, while the middle of the target can be thicker. Distribution of the total mass of Mo allows for larger masses of Mo material and thus larger production batches of 99Mo. A limitation of the sintering approach is the production of very thin disks. Recent advances in 3D printing allow for much thinner target components can be achieved than when the traditional press-and-sinter approach is used. We have demonstrated that several factors can play important roles in dissolution behavior: particle size of Mo metal used for production of targets, sintering conditions, degree of open porosity, and thickness of the sintered Mo targets. Here we report experimental results from studies of small-scale dissolution of sintered Mo disks fabricated from various recycled and commercial Mo materials, and dissolution of 3D-printed Mo disks that were fabricated by Oak Ridge National Laboratory (ORNL). We also report on large-scale dissolution studies with 600 g batches of sintered Mo disks.« less

Effect of attrition milling on the reaction sintering of silicon nitride

NASA Technical Reports Server (NTRS)

Herbell, T. P.; Glasgow, T. K.; Yeh, H. C.

1978-01-01

Silicon powder was ground in a steel attrition mill under nitrogen. Air exposed powder was compacted, prefired in helium, and reaction sintered in nitrogen-4 v/o hydrogen. For longer grinding times, oxygen content, surface area and compactability of the powder increased; and both alpha/beta ratio and degreee of nitridation during sintering increased. Iron content remained constant.

Effect of attrition milling on the reaction sintering of silicon nitride

NASA Technical Reports Server (NTRS)

Herbell, T. P.; Glasgow, T. K.; Yeh, H. C.

1978-01-01

Silicon powder was ground in a steel attrition mill under nitrogen. Air-exposed powder was compacted, prefired in helium, and reaction-sintered in nitrogen-4 v/o hydrogen. For longer grinding times, oxygen content, surface area and compactability of the powder increased; and both alpha/beta ratio and degree of nitridation during sintering increased. Iron content remained constant.

Enhanced Sintering of TiNi Shape Memory Foams under Mg Vapor Atmosphere

NASA Astrophysics Data System (ADS)

Aydoğmuş, Tarik; Bor, Şakir

2012-12-01

TiNi alloy foams are promising candidates for biomaterials to be used as artificial orthopedic implant materials for bone replacement applications in biomedical sector. However, certain problems exist in their processing routes, such as formation of unwanted secondary intermetallic phases leading to brittleness and deterioration of shape memory and superelasticity characteristics; and the contamination during processing resulting in oxides and carbonitrides which affect mechanical properties negatively. Moreover, the eutectic reaction present in Ti-Ni binary system at 1391 K (1118 °C) prevents employment of higher sintering temperatures (and higher mechanical properties) even when equiatomic prealloyed powders are used because of Ni enrichment of TiNi matrix as a result of oxidation. It is essential to prevent oxidation of TiNi powders during processing for high-temperature (>1391 K i.e., 1118 °C) sintering practices. In the current study, magnesium powders were used as space holder material to produce TiNi foams with the porosities in the range of 40 to 65 pct. It has been found that magnesium prevents secondary phase formation and contamination. It also prevents liquid phase formation while enabling employment of higher sintering temperatures by two-step sintering processing: holding the sample at 1373 K (1100 °C) for 30 minutes, and subsequently sintering at temperatures higher than the eutectic temperature, 1391 K (1118 °C). By this procedure, magnesium may allow sintering up to temperatures close to the melting point of TiNi. TiNi foams produced with porosities in the range of 40 to 55 pct were found to be acceptable as implant materials in the light of their favorable mechanical properties.

Effect of microwave-assisted sintering on dielectric properties of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rani, Suman, E-mail: sumanranigju@gmail.com; Ahlawat, Neetu; Punia, R.

2016-05-23

In this present work, CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It wasmore » observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.« less

Reaction-sintered porous mineral-based mullite ceramic membrane supports made from recycled materials.

PubMed

Dong, Yingchao; Zhou, Jian-Er; Lin, Bin; Wang, Yongqing; Wang, Songlin; Miao, Lifeng; Lang, Ying; Liu, Xingqin; Meng, Guangyao

2009-12-15

Bulk porous mullite supports for ceramic membranes were prepared directly using a mixture of industrial waste fly ash and bauxite by dry-pressing, followed by sintering between 1200 and 1550 degrees C. The effects of sintering temperature on the phase composition and shrinkage percent of porous mullite were studied. The XRD results indicate that secondary mullitization reaction took place above 1200 degrees C, and completed at 1450 degrees C. During sintering, the mixture samples first shrunk, then expanded abnormally between 1326 and 1477 degrees C, and finally shrunk again above 1477 degrees C. This unique volume self-expansion is ascribed to the secondary mullitization reaction between bauxite and fly ash. More especially, the micro-structural variations induced by this self-expansion sintering were verified by SEM, porosity, pore size distribution and nitrogen gas permeation flux. During self-expansion sintering, with increasing temperature, an abnormal increase in both open porosity and pore size is observed, which also results in the increase of nitrogen gas flux. The mineral-based mullite supports with increased open porosity were obtained. Furthermore, the sintered porous mullite membrane supports were characterized in terms of thermal expansion co-efficient and mechanical strength.

Formation of Al3Ti/Mg composite by powder metallurgy of Mg-Al-Ti system.

PubMed

Yang, Zi R; Qi Wang, Shu; Cui, Xiang H; Zhao, Yu T; Gao, Ming J; Wei, Min X

2008-07-01

An in situ titanium trialuminide (Al 3 Ti)-particle-reinforced magnesium matrix composite has been successfully fabricated by the powder metallurgy of a Mg-Al-Ti system. The reaction processes and formation mechanism for synthesizing the composite were studied by differential scanning calorimetry (DSC), x-ray diffractometry (XRD), scanning electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDS). Al 3 Ti particles are found to be synthesized in situ in the Mg alloy matrix. During the reaction sintering of the Mg-Al-Ti system, Al 3 Ti particles are formed through the reaction of liquid Al with as-dissolved Ti around the Ti particles. The formed intermetallic particles accumulate at the original sites of the Ti particles. As sintering time increases, the accumulated intermetallic particles disperse and reach a relatively homogeneous distribution in the matrix. It is found that the reaction process of the Mg-Al-Ti system is almost the same as that of the Al-Ti system. Mg also acts as a catalytic agent and a diluent in the reactions and shifts the reactions of Al and Ti to lower temperatures. An additional amount of Al is required for eliminating residual Ti and solid-solution strengthening of the Mg matrix.

Key parameters governing the densification of cubic-Li7La3Zr2O12 Li+ conductors

NASA Astrophysics Data System (ADS)

Yi, Eongyu; Wang, Weimin; Kieffer, John; Laine, Richard M.

2017-06-01

Cubic-Li7La3Zr2O12 (LLZO) is regarded as one of the most promising solid electrolytes for the construction of inherently safe, next generation all-solid-state Li batteries. Unfortunately, sintering these materials to full density with controlled grain sizes, mechanical and electrochemical properties relies on energy and equipment intensive processes. In this work, we elucidate key parameters dictating LLZO densification by tracing the compositional and structural changes during processing calcined and ball-milled Al3+ doped LLZO powders. We find that the powders undergo ion (Li+/H+) exchange during room temperature processing, such that on heating, the protonated LLZO lattice collapses and crystallizes to its constituent oxides, leading to reaction driven densification at < 1000 °C, prior to sintering of LLZO grains at higher temperatures. It is shown that small particle sizes and protonation cannot be decoupled, and actually aid densification. We conclude that using fully decomposed nanoparticle mixtures, as obtained by liquid-feed flame spray pyrolysis, provides an ideal approach to use high surface and reaction energy to drive densification, resulting in pressureless sintering of Ga3+ doped LLZO thin films (25 μm) at 1130 °C/0.3 h to ideal microstructures (95 ± 1% density, 1.2 ± 0.2 μm average grain size) normally accessible only by pressure-assisted sintering. Such films offer both high ionic conductivity (1.3 ± 0.1 mS cm-1) and record low ionic area specific resistance (2 Ω cm2).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miller, D.J.; Pask, J.A.

The sintering of TiC-Ni particle compacts was studied with specific attention to effects of processing conditions. Densification was progressively inhibited with the increasing additions of free carbon to the system. These results are explained on the basis of changes in the eutectic reactions in the system, reduced solubility of TiC in the Ni-rich liquid, and decreased wetting of the solid by the liquid. Presintering hydrogen heat treatment reduced the carbon content of the TiC-Ni compacts and led to reduction in sintering rates and elevated temperatures of liquid-phase formation. Wetting experiments with hydrogen-treated materials showed a time-dependent wetting angle. These resultsmore » are discussed based on wetting theory and reactions predicted by the equilibrium ternary-phase diagram.« less

Raman and dielectric studies of GdMnO3 bulk ceramics synthesized from nano powders

NASA Astrophysics Data System (ADS)

Samantaray, S.; Mishra, D. K.; Roul, B. K.

2017-05-01

Nanocrystalline GdMnO3 (GMO) powders has been synthesized by a simple chemical route i. e. pyrophoric reaction technique and then sintered in the form of bulk pellet at 850°C for 24 hours by adopting slow step sintering schedule. It is observed that by reducing the particles size, chemical route enhances the mixing process as well as decreasing the sintering temperature to get single phase material system in compared to the polycrystalline sample prepared directly from the micron sized commercial powder. Raman spectroscopic studies confirm that the sample is in single phase without any detectable impurity. Frequency dependent dielectric properties i.e., dielectric constant (K) and dielectric loss (tanδ) of GMO ceramics sintered at 850°C for 24 hours were studied at room temperature. The sample showed high K value (˜2736) in the frequency of 100 Hz at room temperature.

A comparison of ultrasound-augmented and conventional leaching of silver from sintering dust using acidic thiourea.

PubMed

Chang, Jun; Zhang, Er-Dong; Zhang, Li-Bo; Peng, Jin-Hui; Zhou, Jun-Wen; Srinivasakannan, C; Yang, Chang-Jiang

2017-01-01

In the process of steel manufacture, up to ten millions of tons of sintering dust (SD) are produced annually in China, which contain noble metals such as Ag. Therefore, recovery of silver (Ag) from SD could be a potential economic and environmental activity. The purpose of this article is to generate information about reaction kinetics of silver leaching with thiourea from SD, comparing the conventional and ultrasonic-augment leaching. The effects of various control parameters such as the ultrasound power, particle size, leaching temperature and thiourea concentration on leaching rate of silver were studied. The results showed 89% silver recovery for conventional process against 95% for ultrasound assisted leaching. The ultrasonic wave increased the leaching rate and shorten the reaction time. The rate controlling step was analyzed using shrinking core model and the rate controlling step is identified to be the diffusion through the product layer in both conventional and ultrasonic-augment leaching processes. The activation energies were estimated to be 28.01kJ/mol and 18.19kJ/mol, and the reaction order were 0.89 and 0.71, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Catalytic reaction processes revealed by scanning probe microscopy. [corrected].

PubMed

Jiang, Peng; Bao, Xinhe; Salmeron, Miquel

2015-05-19

Heterogeneous catalysis is of great importance for modern society. About 80% of the chemicals are produced by catalytic reactions. Green energy production and utilization as well as environmental protection also need efficient catalysts. Understanding the reaction mechanisms is crucial to improve the existing catalysts and develop new ones with better activity, selectivity, and stability. Three components are involved in one catalytic reaction: reactant, product, and catalyst. The catalytic reaction process consists of a series of elementary steps: adsorption, diffusion, reaction, and desorption. During reaction, the catalyst surface can change at the atomic level, with roughening, sintering, and segregation processes occurring dynamically in response to the reaction conditions. Therefore, it is imperative to obtain atomic-scale information for understanding catalytic reactions. Scanning probe microscopy (SPM) is a very appropriate tool for catalytic research at the atomic scale because of its unique atomic-resolution capability. A distinguishing feature of SPM, compared to other surface characterization techniques, such as X-ray photoelectron spectroscopy, is that there is no intrinsic limitation for SPM to work under realistic reaction conditions (usually high temperature and high pressure). Therefore, since it was introduced in 1981, scanning tunneling microscopy (STM) has been widely used to investigate the adsorption, diffusion, reaction, and desorption processes on solid catalyst surfaces at the atomic level. STM can also monitor dynamic changes of catalyst surfaces during reactions. These invaluable microscopic insights have not only deepened the understanding of catalytic processes, but also provided important guidance for the development of new catalysts. This Account will focus on elementary reaction processes revealed by SPM. First, we will demonstrate the power of SPM to investigate the adsorption and diffusion process of reactants on catalyst surfaces at the atomic level. Then the dynamic processes, including surface reconstruction, roughening, sintering, and phase separation, studied by SPM will be discussed. Furthermore, SPM provides valuable insights toward identifying the active sites and understanding the reaction mechanisms. We also illustrate here how both ultrahigh vacuum STM and high pressure STM provide valuable information, expanding the understanding provided by traditional surface science. We conclude with highlighting remarkable recent progress in noncontact atomic force microscopy (NC-AFM) and inelastic electron tunneling spectroscopy (IETS), and their impact on single-chemical-bond level characterization for catalytic reaction processes in the future.

NT-SiC (new-technology silicon carbide) : Φ 650mm optical space mirror substrate of high-strength reaction-sintered silicon carbide

NASA Astrophysics Data System (ADS)

Suyama, Shoko; Itoh, Yoshiyasu; Tsuno, Katsuhiko; Ohno, Kazuhiko

2005-08-01

Silicon carbide (SiC) is the most advantageous as the material of various telescope mirrors, because of high stiffness, low density, low coefficient of thermal expansion, high thermal conductivity and thermal stability. Newly developed high-strength reaction-sintered silicon carbide (NTSIC), which has two times higher strength than sintered SiC, is one of the most promising candidates for lightweight optical mirror substrate, because of fully dense, lightweight, small sintering shrinkage (+/-1 %), good shape capability and low processing temperature. In this study, 650mm in diameter mirror substrate of NTSIC was developed for space telescope applications. Three developed points describe below. The first point was to realize the lightweight to thin the thickness of green bodies. Ribs down to 3mm thickness can be obtained by strengthen the green body. The second point was to enlarge the mirror size. 650mm in diameter of mirror substrate can be fabricated with enlarging the diameter in order. The final point was to realize the homogeneity of mirror substrate. Some properties, such as density, bending strength, coefficient of thermal expansion, Young's modulus, Poisson's ratio, fracture toughness, were measured by the test pieces cutting from the fabricated mirror substrates.

A Sinter-Resistant Catalytic System Based on Platinum Nanoparticles Supported on TiO2 Nanofibers and Covered by Porous Silica

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dai, Yunqian; Lim, Byungkwon; Yang, Yong

2010-10-25

Platinum is a key catalyst that is invaluable in many important industrial processes such as CO oxidation in catalytic converters, oxidation and reduction reactions in fuel cells, nitric acid production, and petroleum cracking.[1] Many of these applications utilize Pt nanoparticles supported on oxides or porous carbon.[2] However, in practical applications that involve high temperatures (typically higher than 3008C), the Pt nanoparticles tend to lose their specific surface area and thus catalytic activity during operation because of sintering. Recent studies have shown that a porous oxide shell can act as a physical barrier to prevent sintering of unsupported metal nanoparticles and,more » at the same time, provide channels for chemical species to reach the surface of the nanoparticles, thus allowing the catalytic reaction to occur. This concept has been demonstrated in several systems, including Pt@SiO2,[3] Pt@CoO,[4] Pt/CeO2@SiO2,[5] Pd@SiO2,[6] Au@SiO2,[7] Au@SnO2 [8] and Au@ZrO2 [9] core– shell nanostructures. Despite these results, a sinter-resistant system has not been realized in supported Pt nanoparticle catalysts.« less

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

NASA Astrophysics Data System (ADS)

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.

Interfacial characterization in carbon nanotube reinforced aluminum matrix composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Housaer, F., E-mail: francois.housaer@ed.univ-lille1.fr; Beclin, F., E-mail: franck.beclin@univ-lille1.fr; Touzin, M., E-mail: matthieu.touzin@univ-lille1.fr

2015-12-15

In this work, the effects of the sintering parameters, such as temperature and the techniques used (HP and SPS), on CNT/Al composite interfaces are studied. The major role of the native aluminum oxide (Al{sub 2}O{sub 3}) layer covering the aluminum grains is highlighted. It is shown that, for a sintering temperature below 620 °C, the amorphous Al{sub 2}O{sub 3} layer prevents the reaction between aluminum and carbon. For greater sintering temperatures, the breaking of the oxide layer due to its crystallization leads to the formation of aluminum carbide (Al{sub 4}C{sub 3}) by reaction between aluminum and the CNT. The Al{submore » 4}C{sub 3} crystals grow perpendicularly to the matrix grain boundaries by thermally activated diffusion of the carbon atoms coming from the CNT. It is also demonstrated that, by limiting the sintering time, which is the case in SPS, it is possible to limit the growth of the Al{sub 4}C{sub 3} crystals and thus to preserve the CNT. - Highlights: • The high reactivity between CNT and Al matrix, resulting Al{sub 4}C{sub 3} formation during the sintering process is highlighted. • We demonstrate, thanks to in-situ TEM observations, that Al{sub 4}C{sub 3} crystals grow into aluminum grains by carbon diffusion. • The native aluminum oxide around the aluminum particles prevents the diffusion of carbon into the aluminum grains. • We show that the protective layer can be broken because of its crystallization, leading to the formation of Al{sub 4}C{sub 3}. • SPS, by limiting the sintering duration, is an interesting way for preparing CNT/Al composites without carbide formation.« less

Enhancement of thermal shock resistance of reaction sintered mullite–zirconia composites in the presence of lanthanum oxide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, P.; Nath, M.; Ghosh, A.

2015-03-15

Mullite–zirconia composites containing 20 wt.% zirconia were prepared by reaction sintering of zircon flour, sillimanite beach sand and calcined alumina. 0 to 8 mol% of La{sub 2}O{sub 3} with respect to zirconia was used as sintering aid. The effect of additive on the various physical, microstructures, mechanical and thermo-mechanical properties was studied. Quantitative phase analysis shows the change in tetragonal zirconia content with incorporation of lanthanum oxide. La{sub 2}O{sub 3} addition has significantly improved the thermal shock resistance of the samples. Samples without additive retained only 20% of initial flexural strength after 5 cycles, whereas samples containing 5 mol% La{submore » 2}O{sub 3} retained almost 78% of its initial flexural strength even after 15 thermal shock cycles. - Highlights: • Mullite–zirconia composites were prepared by reaction sintering route utilizing zircon and sillimanite beach sand. • Lanthanum oxide was used as sintering aid. • The presence of lanthanum oxide decreased the densification temperature. • Lanthanum oxide significantly improved the thermal shock resistance of the composites.« less

Influence of temperature and aging time on HA synthesized by the hydrothermal method.

PubMed

Kothapalli, C R; Wei, M; Legeros, R Z; Shaw, M T

2005-05-01

The influence of temperature and aging time on the morphology and mechanical properties of nano-sized hydroxyapatite (HA) synthesized by a hydrothermal method is reported here. The pre-mixed reactants were poured into a stirred autoclave and reacted at temperatures between 25-250 degrees C for 2-10 h. HA powders thus obtained were examined using X-ray diffraction (XRD), high-resolution field emission scanning electron microscopy (FESEM) and a particle size analyzer. It was found that the aspect ratio of the particles increased with the reaction temperature. The length of the HA particles increased with the reaction temperature below 170 degrees C, but it decreased when the temperature was raised above 170 degrees C. The agglomerates of HA particles were formed during synthesis, and their sizes were strongly dependent on reaction temperatures. As the reaction temperature increased, the agglomerate size decreased (p = 0.008). The density of the discs pressed from these samples reached 85-90% of the theoretical density after sintering at 1200 degrees C for 1 h. No decomposition to other calcium phosphates was detected at this sintering temperature. A correlation existed (p = 0.05) between the agglomerate sizes of HA particles synthesized at various conditions and their sintered densities. With the increase of the agglomerate size, the sintered density of the HA compact decreased. It was found that both the sintered density and flexural strength increased with increasing aging time and reaction temperature. A maximum flexural strength of 78 MPa was observed for the samples synthesized at 170 degrees C for 5 h with the predicted average at these conditions being 65 MPa. These samples attained an average sintered density of 88%.

An evaluation of UO2-CNT composites made by SPS as an accident tolerant nuclear fuel pellet and the feasibility of SPS as an economical fabrication process for the nuclear fuel cycle

NASA Astrophysics Data System (ADS)

Cartas, Andrew R.

The innovative and advanced purpose of this study is to understand and establish proper sintering procedures for Spark Plasma Sintering process in order to fabricate high density, high thermal conductivity UO2 -CNT pellets. Mixing quality and chemical reactions have been investigated by field emission scanning electron microscopy (FESEM), wavelength dispersive spectroscopy (WDS), and X-ray diffraction (XRD). The effect of various types of CNTs on the mixing and sintering quality of UO2-CNT pellets with SPS processing have been examined. The Archimedes Immersion Method, laser flash method, and FE-SEM will be used to investigate the density, thermal conductivity, grain size, pinning effects, and CNT dispersion of fabricated UO2-CNT pellets. Pre-fabricated CNT's were added to UO 2 powder and dispersed via sonication and/or ball milling and then made into composite nuclear pellets. An investigation of the economic impact of SPS on the nuclear fuel cycle for producing pure and composite UO2 fuels was conducted.

Microalloying of transition metal silicides by mechanical activation and field-activated reaction

DOEpatents

Munir, Zuhair A [Davis, CA; Woolman, Joseph N [Davis, CA; Petrovic, John J [Los Alamos, NM

2003-09-02

Alloys of transition metal suicides that contain one or more alloying elements are fabricated by a two-stage process involving mechanical activation as the first stage and densification and field-activated reaction as the second stage. Mechanical activation, preferably performed by high-energy planetary milling, results in the incorporation of atoms of the alloying element(s) into the crystal lattice of the transition metal, while the densification and field-activated reaction, preferably performed by spark plasma sintering, result in the formation of the alloyed transition metal silicide. Among the many advantages of the process are its ability to accommodate materials that are incompatible in other alloying methods.

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

NASA Astrophysics Data System (ADS)

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.

Copper sludge from printed circuit board production/recycling for ceramic materials: a quantitative analysis of copper transformation and immobilization.

PubMed

Tang, Yuanyuan; Lee, Po-Heng; Shih, Kaimin

2013-08-06

The fast development of electronic industries and stringent requirement of recycling waste electronics have produced a large amount of metal-containing waste sludge. This study developed a waste-to-resource strategy to beneficially use such metal-containing sludge from the production and recycling processes of printed circuit board (PCBs). To observe the metal incorporation mechanisms and phase transformation processes, mixtures of copper industrial waste sludge and kaolinite-based materials (kaolinite and mullite) were fired between 650 and 1250 °C for 3 h. The different copper-hosting phases were identified by powder X-ray diffraction (XRD) in the sintered products, and CuAl2O4 was found to be the predominant hosting phase throughout the reactions, regardless of the strong reduction potential of copper expected at high temperatures. The experimental results indicated that CuAl2O4 was generated more easily and in larger quantities at low-temperature processing when using the kaolinite precursor. Maximum copper transformations reached 86% and 97% for kaolinite and mullite systems, respectively, when sintering at 1000 °C. To monitor the stabilization effect after thermal process, prolonged leaching tests were carried out using acetic acid with an initial pH value of 2.9 to leach the sintered products for 20 days. The results demonstrated the decrease of copper leachability with the formation of CuAl2O4, despite different sintering behavior in kaolinite and mullite systems. This study clearly indicates spinel formation as the most crucial metal stabilization mechanism when sintering copper sludge with aluminosilicate materials, and suggests a promising and reliable technique for reusing metal-containing sludge as ceramic materials.

Cyclic Failure Mechanisms of Thermal and Environmental Barrier Coating Systems Under Thermal Gradient Test Conditions

NASA Technical Reports Server (NTRS)

Zhu, Dongming; Lee, Kang N.; Miller, Robert A.

2002-01-01

Plasma-sprayed ZrO2-8wt%Y2O3 and mullite+BSAS/Si multilayer thermal and environmental barrier coating (TBC-EBC) systems on SiC/SiC ceramic matrix composite (CMC) substrates were thermally cyclic tested under high thermal gradients using a laser high-heat-flux rig in conjunction with furnace exposure in water-vapor environments. Coating sintering and interface damage were assessed by monitoring the real-time thermal conductivity changes during the laser heat-flux tests and by examining the microstructural changes after exposure. Sintering kinetics of the coating systems were also independently characterized using a dilatometer. It was found that the coating failure involved both the time-temperature dependent sintering and the cycle frequency dependent cyclic fatigue processes. The water vapor environments not only facilitated the initial coating conductivity increases due to enhanced sintering and interface reaction, but also promoted later conductivity reductions due to the accelerated coating cracking and delamination. The failure mechanisms of the coating systems are also discussed based on the cyclic test results and are correlated to the sintering and thermal stress behavior under the thermal gradient test conditions.

Microstructural study and densification analysis of hot work tool steel matrix composites reinforced with TiB{sub 2} particles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fedrizzi, A., E-mail: anna.fedrizzi@ing.unitn.it; Pellizzari, M.; Zadra, M.

2013-12-15

Hot work tool steels are characterized by good toughness and high hot hardness but are less wear resistant than other tooling materials, such as high speed steel. Metal matrix composites show improved tribological behavior, but not much work has been done in the field of hot work tool steels. In this paper TiB{sub 2}-reinforced hot work tool steel matrix composites were produced by spark plasma sintering (SPS). Mechanical alloying (MA) was proposed as a suited process to improve the composite microstructure. Density measurements and microstructure confirmed that MA promotes sintering and produces a fine and homogeneous dispersion of reinforcing particles.more » X-ray diffraction patterns of the sintered composites highlighted the formation of equilibrium Fe{sub 2}B and TiC, as predicted by thermodynamic calculations using Thermo-Calc® software. Scanning electron microscopy as well as scanning Kelvin probe force microscopy highlighted the reaction of the steel matrix with TiB{sub 2} particles, showing the formation of a reaction layer at the TiB{sub 2}-steel interface. Phase investigations pointed out that TiB{sub 2} is not chemically stable in steel matrix because of the presence of carbon even during short time SPS. - Highlights: • TiB{sub 2} reinforced steel matrix composites were produced by spark plasma sintering. • TiB{sub 2} was successfully dispersed in the steel matrix by mechanical alloying. • Steel and TiB{sub 2} react during sintering forming equilibrium Fe{sub 2}B and TiC. • The new phases were investigated by means of AFM, Volta potential and XRD analyses.« less

Production of ZrC Matrix for Use in Gas Fast Reactor Composite Fuels

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vasudevamurthy, Gokul; Knight, Travis W.; Roberts, Elwyn

2007-07-01

Zirconium carbide is being considered as a candidate for inert matrix material in composite nuclear fuel for Gas fast reactors due to its favorable characteristics. ZrC can be produced by the direct reaction of pure zirconium and graphite powders. Such a reaction is exothermic in nature. The reaction is self sustaining once initial ignition has been achieved. The heat released during the reaction is high enough to complete the reaction and achieve partial sintering without any external pressure applied. External heat source is required to achieve ignition of the reactants and maintain the temperature close to the adiabatic temperature tomore » achieve higher levels of sintering. External pressure is also a driving force for sintering. In the experiments described, cylindrical compacts of ZrC were produced by direct combustion reaction. External induction heating combined with varying amounts of external applied pressure was employed to achieve varying degrees of density/porosity. The effect of reactant particle size on the product characteristics was also studied. The samples were characterized for density/porosity, composition and microstructure. (authors)« less

Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO₃ Ceramics Fabricated by Spark Plasma Sintering.

PubMed

Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

2017-03-07

Based on precursor powders with a size of 200-300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO₃ ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO₃ ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe 3+ to Fe 2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO₃ ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage.

Effect of milling and leaching on the structure of sintered silicon

NASA Technical Reports Server (NTRS)

Yeh, H. C.; Glascow, T. K.; Herbell, T. P.

1980-01-01

Sintering was performed in He for 16 hours at 1200, 1250, and 1300 C. Compacts of as-received Si did not densify during sintering. Milling reduced the average particle size to below 0.5 micrometer and enhanced densification (1.75 g/cc). Leaching milled Si further enhanced densification (1.90 g/cc max.) and decreased structural coarsening. After sintering, the structure of the milled and leached powder compacts appears favorable for the production of reaction bonded silicon nitride.

Lowering the synthesis temperature of Y3Fe5O12 by surfactant assisted solid state reaction

NASA Astrophysics Data System (ADS)

Xue, Fenghua; Huang, Ju; Li, Tianrui; Wang, Zifan; Zhou, Xiaochao; Wei, Lujun; Gao, Baizhi; Zhai, Ya; Li, Qi; Xu, Qingyu; Du, Jun

2018-01-01

There is an urgent technical requirement of lowering the sintering temperature of Y3Fe5O12 (YIG) for its practical applications. In this paper, a modified solid state reaction method is reported by adding the surfactant of cetyltrimethylammonium bromide (CTAB). A high sintering temperature of 1200 °C is required for the formation of YIG phase without adding CTAB, which is effectively decreased to 1050 °C by adding CTAB. The morphology studies show that the sintering temperature plays the main role in the crystal growth and excludes the possible contribution of CTAB. The prepared YIG ceramic samples show soft ferromagnetic properties, with coercivity of only 21.2 Oe for the sample prepared with CTAB at 1050 °C, which decreases with increasing sintering temperature. The main role of adding CTAB is preventing the agglomeration of ball milled ultrafine source particles, which may facilitate the interdiffusion among them and promote the reaction at lower temperatures. Furthermore, the Gilbert damping constant is significantly reduced for YIG prepared by adding CTAB, which is one order smaller than that without CTAB.

Lightweight Aluminum/Nano composites for Automotive Drive Train Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chelluri, Bhanumathi; Knoth, Edward A.; Schumaker, Edward J.

2012-12-14

During Phase I, we successfully processed air atomized aluminum powders via Dynamic Magnetic Compaction (DMC) pressing and subsequent sintering to produce parts with properties similar to wrought aluminum. We have also showed for the first time that aluminum powders can be processed without lubes via press and sintering to 100 % density. This will preclude a delube cycle in sintering and promote environmentally friendly P/M processing. Processing aluminum powders via press and sintering with minimum shrinkage will enable net shape fabrication. Aluminum powders processed via a conventional powder metallurgy process produce too large a shrinkage. Because of this, sinter partsmore » have to be machined into specific net shape. This results in increased scrap and cost. Fully sintered aluminum alloy under this Phase I project has shown good particle-to-particle bonding and mechanical properties. We have also shown the feasibility of preparing nano composite powders and processing via pressing and sintering. This was accomplished by dispersing nano silicon carbide (SiC) powders into aluminum matrix comprising micron-sized powders (<100 microns) using a proprietary process. These composite powders of Al with nano SiC were processed using DMC press and sinter process to sinter density of 85-90%. The process optimization along with sintering needs to be carried out to produce full density composites.« less

Recent Advances and Research Status in Energy Conservation of Iron Ore Sintering in China

NASA Astrophysics Data System (ADS)

Wang, Yao-Zu; Zhang, Jian-Liang; Liu, Zheng-Jian; Du, Cheng-Bo

2017-11-01

For the ferrous burden of blast furnaces in China, sinter generally accounts for more than 70% and the sintering process accounts for approximately 6-10% of the total energy consumption of the iron and steel enterprise. Therefore, saving energy during the sintering process is important to reduce the energy consumption in the iron and steel industry. This paper aims to illustrate recent advances and the research status of energy conservation of iron ore sintering in China. It focuses on the development and application of energy-saving technologies such as the composite agglomeration process, sintering with high-proportion flue gas recirculation sintering, recovery of sensible heat from the sinter cooling process, homogeneous deep-bed sintering technology, and comprehensive treatment technology of leakage of sintering. Moreover, some suggestions for the future development of energy-saving technologies are put forward.

Study of phenomena related to the sintering process of silicon nitride at atmospheric pressure

NASA Technical Reports Server (NTRS)

Bertani, A.

1982-01-01

A procedure was perfected for the production of components used in engineering applications of silicon nitride. Particles of complex geometry that combine remarkable mechanical properties with a high density are obtained. The process developed, in contrast to the "hot pressing" method, does not use external pressures, and in contrast to the reaction bonding method, final densities close to the theoretical value are obtained.

Development of a statistically proven injection molding method for reaction bonded silicon nitride, sintering reaction bonded silicon nitride, and sintered silicon nitride

NASA Astrophysics Data System (ADS)

Steiner, Matthias

A statistically proven, series injection molding technique for ceramic components was developed for the construction of engines and gas turbines. The flow behavior of silicon injection-molding materials was characterized and improved. Hot-isostatic-pressing reaction bonded silicon nitride (HIPRBSN) was developed. A nondestructive component evaluation method was developed. An injection molding line for HIPRBSN engine components precombustion chamber, flame spreader, and valve guide was developed. This line allows the production of small series for engine tests.

Porous-electrode preparation method

DOEpatents

Arons, R.M.; Dusek, J.T.

1981-09-17

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity.

Porous electrode preparation method

DOEpatents

Arons, Richard M.; Dusek, Joseph T.

1983-01-01

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder of such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity.

Porous electrode preparation method

DOEpatents

Arons, R.M.; Dusek, J.T.

1983-10-18

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder of such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity. 2 figs.

Effect of milling and leaching on the structure of sintered silicon

NASA Technical Reports Server (NTRS)

Yeh, H. C.; Glasgow, T. K.; Herbell, T. P.

1980-01-01

The effects of attrition milling and acid leaching on the sintering behavior and the resultant structures of two commercial silicon powders were investigated. Sintering was performed in He for 16 hours at 1200, 1250, and 1300 C. Compacts of as-received Si did not densify during sintering. Milling reduced the average particle size to below 0.5 microns and enhanced densification (1.75 g/cc). Leaching milled Si further enhanced densification (1.90 g/cc max.) and decreased structural coarsening. After sintering, the structure of the milled and leached powder compacts appears favorable for the production of reaction bonded silicon nitride.

Nitrogen Ceramics Meeting in France

DTIC Science & Technology

1988-01-21

100 and Mocellin (Ecole Polytechnique de Laus- 300*C. Other semiconductors are sensi- anne, Switzerland); this reaction is ob- tive to a very large...number of gases, but served when sintering powder mixtures at only NH3 affects the electrical resistiv- 1400-1600*C ( Mocellin , 1986). Mocellin ity of...isostatic pressure sintering; pres- Mocellin , A., Revue de Chime Mingrale, sure sintering after a preliminary heat 23 (1986), 80. 3

Microwave processing of a dental ceramic used in computer-aided design/computer-aided manufacturing.

PubMed

Pendola, Martin; Saha, Subrata

2015-01-01

Because of their favorable mechanical properties and natural esthetics, ceramics are widely used in restorative dentistry. The conventional ceramic sintering process required for their use is usually slow, however, and the equipment has an elevated energy consumption. Sintering processes that use microwaves have several advantages compared to regular sintering: shorter processing times, lower energy consumption, and the capacity for volumetric heating. The objective of this study was to test the mechanical properties of a dental ceramic used in computer-aided design/computer-aided manufacturing (CAD/CAM) after the specimens were processed with microwave hybrid sintering. Density, hardness, and bending strength were measured. When ceramic specimens were sintered with microwaves, the processing times were reduced and protocols were simplified. Hardness was improved almost 20% compared to regular sintering, and flexural strength measurements suggested that specimens were approximately 50% stronger than specimens sintered in a conventional system. Microwave hybrid sintering may preserve or improve the mechanical properties of dental ceramics designed for CAD/CAM processing systems, reducing processing and waiting times.

Improved performance of silicon nitride-based high temperature ceramics

NASA Technical Reports Server (NTRS)

Ashbrook, R. L.

1977-01-01

Recent progress in the production of Si3N4 based ceramics is reviewed: (1) high temperature strength and toughness of hot pressed Si3N4 were improved by using high purity powder and a stabilized ZrO2 additive, (2) impact resistance of hot pressed Si3N4 was increased by the use of a crushable energy absorbing layer, (3) the oxidation resistance and strength of reaction sintered Si3N4 were increased by impregnating reaction sintered silicon nitride with solutions that oxidize to Al2O3 or ZrO2, (4) beta prime SiA1ON compositions and sintering aids were developed for improved oxidation resistance or improved high temperature strength.

Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO3 Ceramics Fabricated by Spark Plasma Sintering

PubMed Central

Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

2017-01-01

Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO3 ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO3 ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe3+ to Fe2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO3 ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage. PMID:28772626

An Investigation of Sintering Parameters on Titanium Powder for Electron Beam Melting Processing Optimization.

PubMed

Drescher, Philipp; Sarhan, Mohamed; Seitz, Hermann

2016-12-01

Selective electron beam melting (SEBM) is a relatively new additive manufacturing technology for metallic materials. Specific to this technology is the sintering of the metal powder prior to the melting process. The sintering process has disadvantages for post-processing. The post-processing of parts produced by SEBM typically involves the removal of semi-sintered powder through the use of a powder blasting system. Furthermore, the sintering of large areas before melting decreases productivity. Current investigations are aimed at improving the sintering process in order to achieve better productivity, geometric accuracy, and resolution. In this study, the focus lies on the modification of the sintering process. In order to investigate and improve the sintering process, highly porous titanium test specimens with various scan speeds were built. The aim of this study was to decrease build time with comparable mechanical properties of the components and to remove the residual powder more easily after a build. By only sintering the area in which the melt pool for the components is created, an average productivity improvement of approx. 20% was achieved. Tensile tests were carried out, and the measured mechanical properties show comparatively or slightly improved values compared with the reference.

The study of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites

NASA Astrophysics Data System (ADS)

Yu, Peng

Aluminum-based metal matrix composites (MMCs) have been widely used as structural materials in the automobile and aerospace industry due to their specific properties. In this thesis, we report the fabrication of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites by the displacement reactions between Al and selected metal oxides (NiO, CuO and ZnO). These MMCs were produced when the Al-20wt% NiO, Al-20wt% CuO and Al-10wt% ZnO green compacts were reaction sintered in the tube furnaces. In this work, differential thermal analysis (DTA) was performed on the green samples. The green samples were then sintered separately in different tube furnaces for 30 minutes. In order to study the reaction mechanisms, the x-ray diffractometry (XRD) was used to obtain diffraction patterns of these sintered samples, the scanning electron microscope (SEM) and transmission electron microscope (TEM) were used to study the microstructures of these samples. The elemental quantitative compositions of samples were determined by the energy dispersive x-ray spectrometry (EDX). In order to study the effect of cooling rate on the samples, the green samples were further sintered to 1000°C and cooled down to room temperature in different conditions: by furnace-cooling, air-quenching, oil-quenching or NaCl-solution-quenching. The SEM, TEM and atomic force microscopy (AFM) were conducted to investigate their microstructures. A microhardness tester was used to measure the hardness values of these samples. It was found that during sintering of the Al-20wt% NiO green sample, displacement reaction between Al and NiO initially occurred in solid-solid form and was soon halted by its products that separated the NiO particles from the Al matrix. The reaction then resumed in solid-liquid form as the temperature increased to the eutectic temperature of Al3Ni-Al when liquid (Al, Ni) phase appeared in the sample. After cooling, Al2O 3 particles, Al3Ni proeutectic phase and fiber-like Al 3Ni-Al eutectic were found in the sintered Al-MMC sample. (Abstract shortened by UMI.)

40 CFR 63.1543 - Standards for process and process fugitive sources.

Code of Federal Regulations, 2011 CFR

2011-07-01

... section. (1) Sinter machine; (2) Blast furnace; (3) Dross furnace; (4) Dross furnace charging location; (5) Blast furnace and dross furnace tapping location; (6) Sinter machine charging location; (7) Sinter machine discharge end; (8) Sinter crushing and sizing equipment; and (9) Sinter machine area. (b) The...

One step sintering of homogenized bauxite raw material and kinetic study

NASA Astrophysics Data System (ADS)

Gao, Chang-he; Jiang, Peng; Li, Yong; Sun, Jia-lin; Zhang, Jun-jie; Yang, Huan-ying

2016-10-01

A one-step sintering process of bauxite raw material from direct mining was completed, and the kinetics of this process was analyzed thoroughly. The results show that the sintering kinetics of bauxite raw material exhibits the liquid-phase sintering behavior. A small portion of impurities existed in the raw material act as a liquid phase. After X-ray diffraction analyses, scanning electron microscopy observations, and kinetics calculations, sintering temperature and heating duration were determined as the two major factors contributing to the sintering process and densification of bauxite ore. An elevated heating temperature and longer duration favor the densification process. The major obstacle for the densification of bauxite material is attributed to the formation of the enclosed blowhole during liquid-phase sintering.

SPS-RS technique for solid-phase “in situ” synthesis of biocompatible ZrO2 porous ceramics

NASA Astrophysics Data System (ADS)

Shichalin, O. O.; Medkov, M. A.; Grishchenko, D. N.; Mayorov, V. Yu; Fedorets, A. N.; Belov, A. A.; Golub, A. V.; Gridasova, E. A.; Papynov, E. K.

2018-02-01

The prospective method of spark plasma sintering-reaction synthesis (SPS-RS) for fabrication of ceramics based on ZrO2 and biocompatible with living tissue is presented. Nanostructured ceramics has high mechanical strength (more than 400 MPa) and controlled porosity depending on specified sintering conditions. Biocompatible phases Ca10(PO4)6(OH)2 are formed “in situ” during SPS sintering of ZrO2 powder due to chemical interaction of phosphate precursors preliminary introduced into the mixture. The effective method to improve (to develop) porous structure of bioceramics obtained by SPS or SPS-RS techniques using poreforming agent (carbon black) is proposed. Suggested original SPS-RS “in situ” technique provides fabrication of new ZrO2 ceramics containing biocompatible phosphate components and possessing unique structural and mechanical characteristics. Such ceramics is indispensable for bone-ceramic implants that are able to activate processes of osteogenesis during bone tissue recovery.

Glass composite waste forms for iodine confined in bismuth-embedded SBA-15

NASA Astrophysics Data System (ADS)

Yang, Jae Hwan; Park, Hwan Seo; Ahn, Do-Hee; Yim, Man-Sung

2016-11-01

The aim of this study was to stabilize bismuth-embedded SBA-15 that captured iodine gas by fabrication of monolithic waste forms. The iodine containing waste was mixed with Bi2O3 (a stabilizing additive) and low-temperature sintering glass followed by pelletizing and the sintering process to produce glass composite materials. Iodine volatility during the sintering process was significantly affected by the ratio of Bi2O3 and the glass composition. It was confirmed that BiI3, the main iodine phase within bismuth-embedded SBA-15, was effectively transformed to the mixed phases of Bi5O7I and BiOI. The initial leaching rates of iodine from the glass composite waste forms ranged 10-3-10-2 g/m2 day, showing the stability of the iodine phases encapsulated by the glassy networks. It was also observed that common groundwater anions (e.g., chloride, carbonate, sulfite, and fluoride) elevated the iodine leaching rate by anion exchange reactions. The present results suggest that the glass composite waste form of bismuth-embedded SBA-15 could be a candidate material for stable storage of 129I.

In-situ DRIFTS investigation on the selective catalytic reduction of NO with NH3 over the sintered ore catalyst

NASA Astrophysics Data System (ADS)

Chen, Wangsheng; Li, Ze; Hu, Fali; Qin, Linbo; Han, Jun; Wu, Gaoming

2018-05-01

In this study, the sintered ore used as catalysts for the selective catalytic reduction (SCR) of NOX with NH3 from the sintering flue gas was investigated. The experimental results demonstrated that the maximum denitration efficiency, about 61.64%, occurred at 300 °C, 1.0 NH3/NO ratio, and 1000 h-1 gas hourly space velocity (GHSV). In order to understand the SCR denitration mechanism, the catalyst was characterized by DRIFTS, XPS, H2-TPR, BET and ICP-MS. It was found that there were Lewis and Brønsted acid sites at the surface of the sintered ore, which lead to the appearance of amide species (sbnd NH2), NH4+ intermediates, gaseous or weakly adsorbed NO2 and nitrite species. Hence, it was concluded that the reaction of the amide species (sbnd NH2) with gaseous NO (E-R mechanism) and the reaction of absorbed NO2 with the coordinated ammonia (L-H mechanism) were attributed to NOx reduction.

Sintering behavior of ultrafine silicon carbide powders obtained by vapor phase reaction

NASA Technical Reports Server (NTRS)

Okabe, Y.; Miyachi, K.; Hojo, J.; Kato, A.

1984-01-01

The sintering behavior of ultrafine SiC powder with average particle size of about 0.01-0.06 microns produced by a vapor phase reaction of the Me4Si-H2 system was studied at the temperature range of 1400-2050 deg. It was found that the homogeneous dispersion of C on SiC particles is important to remove the surface oxide layer effectively. B and C and inhibitive effect on SiC grain growth.

Microstructure and Mechanical Behaviors of Titanium Matrix Composites Containing In Situ Whiskers Synthesized via Plasma Activated Sintering.

PubMed

Sun, Yi; Zhang, Jian; Luo, Guoqiang; Shen, Qiang; Zhang, Lianmeng

2018-04-02

In this paper, titanium matrix composites with in situ TiB whiskers were synthesized by the plasma activated sintering technique; crystalline boron and amorphous boron were used as reactants for in situ reactions, respectively. The influence of the sintering process and the crystallography type of boron on the microstructure and mechanical properties of composites were studied and compared. The densities were evaluated using Archimedes' principle. The microstructure and mechanical properties were characterized by SEM, XRD, EBSD, TEM, a universal testing machine, and a Vickers hardness tester. The prepared composite material showed a high density and excellent comprehensive performance under the PAS condition of 20 MPa at 1000 °C for 3 min. Amorphous boron had a higher reaction efficiency than crystalline boron, and it completely reacted with the titanium matrix to generate TiB whiskers, while there was still a certain amount of residual crystalline boron combining well with the titanium matrix at 1100 °C. The composite samples with a relative density of 98.33%, Vickers hardness of 389.75 HV, compression yield strength of up to 1190 MPa, and an ultimate compressive strength of up to 1710 MPa were obtained. Compared with the matrix material, the compressive strength of TC4 titanium alloy containing crystalline boron and amorphous boron was increased by 7.64% and 15.50%, respectively.

Microstructure and Mechanical Behaviors of Titanium Matrix Composites Containing In Situ Whiskers Synthesized via Plasma Activated Sintering

PubMed Central

Luo, Guoqiang; Shen, Qiang; Zhang, Lianmeng

2018-01-01

In this paper, titanium matrix composites with in situ TiB whiskers were synthesized by the plasma activated sintering technique; crystalline boron and amorphous boron were used as reactants for in situ reactions, respectively. The influence of the sintering process and the crystallography type of boron on the microstructure and mechanical properties of composites were studied and compared. The densities were evaluated using Archimedes’ principle. The microstructure and mechanical properties were characterized by SEM, XRD, EBSD, TEM, a universal testing machine, and a Vickers hardness tester. The prepared composite material showed a high density and excellent comprehensive performance under the PAS condition of 20 MPa at 1000 °C for 3 min. Amorphous boron had a higher reaction efficiency than crystalline boron, and it completely reacted with the titanium matrix to generate TiB whiskers, while there was still a certain amount of residual crystalline boron combining well with the titanium matrix at 1100 °C. The composite samples with a relative density of 98.33%, Vickers hardness of 389.75 HV, compression yield strength of up to 1190 MPa, and an ultimate compressive strength of up to 1710 MPa were obtained. Compared with the matrix material, the compressive strength of TC4 titanium alloy containing crystalline boron and amorphous boron was increased by 7.64% and 15.50%, respectively. PMID:29614842

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

NASA Astrophysics Data System (ADS)

Potanina, Ekaterina; Golovkina, Ludmila; Orlova, Albina; Nokhrin, Aleksey; Boldin, Maksim; Sakharov, Nikita

2016-05-01

Complex oxide Y2.5Nd0.5Al5O12 with garnet structure and phosphates NdPO4 and GdPO4 with monazite structure were obtained by using precipitation methods. Ceramics Y2.5Nd0.5Al5O12 and NdPO4 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 10-6-10-7 g/(cm2 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.

Process Development and Property Evaluation of Organosilicon Infiltrated Reaction Sintered Silicon Nitride (RSSN).

DTIC Science & Technology

1982-01-01

Battelle) (5) Prepolymer based on methyltrichlorosilane and ammonia (Battelle) (6) Polysilastyrene (Professor West, University of Wisconsin) (7...These types of materials are not commercially available, but are produced from commercial intermediates (methyldichlorosilane and ammonia ) and have been...methyltrichlorosilane and ammonia is a low melting, solid resin which has been shown to yield 72 percent residue by thermogravimetric analysis (TGA) in our work

Effects of Molar Ratios and Sintering Times on Crystal Structures and Surface Morphology of Nd1+xFeO3 Oxide Alloy Prepared by using Solid Reaction Method

NASA Astrophysics Data System (ADS)

Sujiono, E. H.; Agus, J.; Samnur, S.; Triyana, K.

2018-05-01

The effects of molar ratios and sintering times on crystal structures and surface morphology on NdFeO3 oxide alloy have been studied. NdFeO3 oxide alloy formed by chemical preparation with solid reaction method using raw oxide Fe2O3 (99.9 %) and Nd2O3 (99.9 %) powders. In this article we reported the effects of molar ratios x = (–0.1, –0.2 and –0.3) and sintering times for 15 h and 20 h on crystal structures and surface morphology of Nd1+xFeO3 synthesized by solid-state reaction method. The results indicate that variation of molar ratio and sintering time has influenced the FWHM, crystalline size and grain size. The Nd1+xFeO3 have a major phase is NdFeO3, and other minor phases are Fe2O3, Nd2O3 and Nd(OH)3. The dominant intensity of hkl (121) with a value in FWHM, crystallite size, and grain size an indication the results will be applied as a gas sensor material as the focus of the further study.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Faisal, Heny, E-mail: faisal@physics.its.ac.id; Darminto,; Triwikantoro,

2016-04-19

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

Densification and Electrical Properties of Zinc Oxide Varistors Microwave-Sintered Under Different Oxygen Partial Pressures

NASA Astrophysics Data System (ADS)

Lin, Cong; Wang, Bo; Xu, Zheng; Peng, Hu

2012-11-01

ZnO varistors were prepared by microwave sintering under different oxygen partial pressures. The temperature profile and the densification behavior in different atmospheres were investigated. It was found that the density of ZnO varistors during sintering was the key factor affecting the absorption of microwave energy. The electrical properties, including the nonlinear properties and capacitance-voltage ( C- V) characteristics, were also carefully studied. The results showed that the oxygen partial pressure has significant effects on the electrical properties of ZnO varistors by changing the concentration of defects through a series of reactions involving oxygen during sintering.

The interaction of small particles and thin films of metals with gases. I - A brief review of the early stages of oxide formation

NASA Technical Reports Server (NTRS)

Poppa, H.

1976-01-01

Existing work on gas-solid reactions making use of thin film technologies is reviewed. The discussion concentrates on two major areas of gas-metal interactions: chemisorption and the early stages of oxidation of metals (characterized by a non-volatile reaction product) and catalytic surface reactions (featuring volatile reaction products). A brief survey of oxide formation on metals is presented. Here it is of importance to distinguish between reactions on continuous thin film substrates and reactions on particulate deposits. Small particle-gas interactions also affect the nucleation, growth and sintering processes of thin films. It is shown that various combinations of UHV and high resolution electron microscopy techniques, which include in situ experimentation, can provide the appropriate tools for studying angstrom particle chemistry.

Hardness of pulsed electric current sintered and hot isostatically pressed Mo(Si,Al)2

NASA Astrophysics Data System (ADS)

Tanabe, Jun

2005-05-01

We improved the reactivity and mechanical characteristics of Mo(Si,Al)2 by pulsed electric current sintering (PECS) and hot isostatic pressing (HIP), and evaluated its reaction state and mechanical characteristics using energy dispersive spectroscopy (EDS), X-ray diffraction, and a hardness test. Mo(Si,Al)2 was generated by pretreatment using a furnace, and the application of the PECS and HIP treatments further densified the sintered body, resulting in an increase in the hardness.

Behavior of New Zealand Ironsand During Iron Ore Sintering

NASA Astrophysics Data System (ADS)

Wang, Zhe; Pinson, David; Chew, Sheng; Rogers, Harold; Monaghan, Brian J.; Pownceby, Mark I.; Webster, Nathan A. S.; Zhang, Guangqing

2016-02-01

A New Zealand ironsand sample was characterized by scanning electron microscopy (SEM), X-ray fluorescence spectroscopy, qualitative and quantitative X-ray diffraction, and electron probe microanalysis. The titanomagnetite-rich ironsand was added into an industrial sinter blend in the proportion of 5 wt pct, and the mixture was uniaxially pressed into cylindrical tablets and sintered in a tube furnace under flowing gas with various oxygen potentials and temperatures to develop knowledge and understanding of the behavior of titanium during sintering. An industrial sinter with the addition of 3 wt pct ironsand was also examined. Both the laboratory and industrial sinters were characterized by optical and SEM. Various morphologies of relict ironsand particles were present in the industrial sinter due to the heterogeneity of sintering conditions, which could be well simulated by the bench-scale sintering experiments. The assimilation of ironsand during sintering in a reducing atmosphere started with the diffusion of calcium into the lattice of the ironsand matrix, and a reaction zone was formed near the boundary within individual ironsand particles where a perovskite phase was generated. With increasing sintering temperature, in a reducing atmosphere, ironsand particles underwent further assimilation and most of the titanium moved from the ironsand particles into a glass phase. In comparison, more titanium remained in the original ironsand particles when sintered in air. Ironsand particles are more resistant to assimilation in an oxidizing atmosphere.

Production of superconductor/carbon bicomponent fibers

NASA Technical Reports Server (NTRS)

Wise, S. A.; Fain, C. C.; Leigh, H. D.

1991-01-01

Certain materials are unable to be drawn or spun into fiber form due to their improper melting characteristics or brittleness. However, fibrous samples of such materials are often necessary for the fabrication of intricate shapes and composites. In response to this problem, a unique process, referred to as the piggyback process, was developed to prepare fibrous samples of a variety of nonspinnable ceramics. In this technique, specially produced C shaped carbon fibers serve as micromolds to hold the desired materials prior to sintering. Depending on the sintering atmosphere used, bicomponent or single component fibers result. While much has been shown worldwide concerning the YBa2Cu3O(7-x) superconductor, fabrication into unique forms has proven quite difficult. However, a variety of intricate shapes are necessary for rapid commercialization of the superconducting materials. The potential for producing fibrous samples of the YBa2Cu3O(7-x) compound by the piggyback process is being studied. Various organic and acrylic materials were studied to determine suspending ability, reactivity with the YBa2Cu3O(7-x) compound during long term storage, and burn out characteristics. While many questions were answered with respect to the interfacial reactions between YBa2Cu3O(7-x) and carbon, much work is still necessary to improve the quality of the sintered material if the fibers produced are to be incorporated into useful composite or cables.

Fabrication of piezoelectric ceramic fibers by extrusion of PZT powder and PZT sol mixture

NASA Astrophysics Data System (ADS)

Kobayashi, Yoshimasa; Um, Tae Y.; Qiu, Jinhao; Tani, Junji; Takahashi, Hirofumi

2001-07-01

This study aims to fabricate Pb(Zr,Ti)O3 (PZT) piezoelectric ceramic fibers by extrusion with mixture of PZT powder and PZT sol. The added PZT sol in this study played a role as a binder; the sol changed into PZT crystalline during sintering, and removal process of additives before sintering was not required. To obtain PZT fibers, the condition of sol viscosity adjustment, the mixture ratio of powder and sol for fiber extrusion, and the sintering condition for obtaining polycrystalline fibers were investigated. PZT precursor solution was synthesized from lead acetate trihydrate, zirconium n-propoxide and titanium isopropoxide by reflux at 120 degree(s)C for 3 hours with 2-methoxyethanol. The appropriate adjustment of spinnable sol was achieved by the addition of acetic acid for suppressing the hydrolysis reaction and the curing sol at 80 degree(s)C for promoting the condensation of sol. Green fibers with diameter of about 300micrometers were successfully extruded from the mixture of PZT powder and sol. The extruded fibers sintered at 1200 degree(s)C had the microstructure with 2-6micrometers grains and had no pores or cracks. From the result of displacement behavior measurement, PZT fibers fabricated by firing at 1200 degree(s)C in this study were considered to have desired piezoelectric properties.

Numerical Simulation of Sintering Process in Ceramic Powder Injection Moulded Components

NASA Astrophysics Data System (ADS)

Song, J.; Barriere, T.; Liu, B.; Gelin, J. C.

2007-05-01

A phenomenological model based on viscoplastic constitutive law is presented to describe the sintering process of ceramic components obtained by powder injection moulding. The parameters entering in the model are identified through sintering experiments in dilatometer with the proposed optimization method. The finite element simulations are carried out to predict the density variations and dimensional changes of the components during sintering. A simulation example on the sintering process of hip implant in alumina has been conducted. The simulation results have been compared with the experimental ones. A good agreement is obtained.

Fabrication Processes and Mechanical Behavior of CNT/Metal Nanocomposites

DTIC Science & Technology

2013-12-01

process, were investigated and applied for fabrication of CNT/Cu and CNT/Ni nanocomposite powders. The spark plasma sintering process was applied... spark plasma sintering process to fabricate CNT/NiTi and CNT/Al-Cu nanocomposites. It is confirmed that the CNTs were homogeneously dispersed in NiTi...can be seen in Figure 1-1. The CNT/NiTi composite powders were consolidated by spark plasma sintering (SPS, Dr. Sinter Lab., Sumitomo). The CNT/NiTi

Post-Plasma SiOx Coatings of Metal and Metal Oxide Nanoparticles for Enhanced Thermal Stability and Tunable Photoactivity Applications

PubMed Central

Post, Patrick; Jidenko, Nicolas; Weber, Alfred P.; Borra, Jean-Pascal

2016-01-01

The plasma-based aerosol process developed for the direct coating of particles in gases with silicon oxide in a continuous chemical vapor deposition (CVD) process is presented. It is shown that non-thermal plasma filaments induced in a dielectric barrier discharge (DBD) at atmospheric pressure trigger post-DBD gas phase reactions. DBD operating conditions are first scanned to produce ozone and dinitrogen pentoxide. In the selected conditions, these plasma species react with gaseous tetraethyl orthosilicate (TEOS) precursor downstream of the DBD. The gaseous intermediates then condense on the surface of nanoparticles and self-reactions lead to homogeneous solid SiOx coatings, with thickness from nanometer to micrometer. This confirms the interest of post-DBD injection of the organo-silicon precursor to achieve stable production of actives species with subsequent controlled thickness of SiOx coatings. SiOx coatings of spherical and agglomerated metal and metal oxide nanoparticles (Pt, CuO, TiO2) are achieved. In the selected DBD operating conditions, the thickness of homogeneous nanometer sized coatings of spherical nanoparticles depends on the reaction duration and on the precursor concentration. For agglomerates, operating conditions can be tuned to cover preferentially the interparticle contact zones between primary particles, shifting the sintering of platinum agglomerates to much higher temperatures than the usual sintering temperature. Potential applications for enhanced thermal stability and tunable photoactivity of coated agglomerates are presented. PMID:28335219

Flash sintering of ceramic materials

NASA Astrophysics Data System (ADS)

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.

Densification of LSGM electrolytes using activated microwave sintering

NASA Astrophysics Data System (ADS)

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).

Improving the Thermochemical Energy Storage Performance of the Mn2 O3 /Mn3 O4 Redox Couple by the Incorporation of Iron.

PubMed

Carrillo, Alfonso J; Serrano, David P; Pizarro, Patricia; Coronado, Juan M

2015-06-08

Redox cycles of manganese oxides (Mn2 O3 /Mn3 O4 ) are a promising alternative for thermochemical heat storage systems coupled to concentrated solar power plants as manganese oxides are abundant and inexpensive materials. Although their cyclability for such a purpose has been proved, sintering processes, related to the high-temperature conditions at which charge-discharge cycles are performed, generally cause a cycle-to-cycle decrease in the oxidation rate of Mn3 O4 . To guarantee proper operation, both reactions should present stable reaction rates. In this study, it has been demonstrated that the incorporation of Fe, which is also an abundant material, into the manganese oxides improves the redox performance of this system by increasing the heat storage density, narrowing the redox thermal hysteresis, and, above all, stabilizing and enhancing the oxidation rate over long-term operation, which counteracts the negative effects caused by sintering, although its presence is not avoided. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dissolution-precipitation reactions and permeability evolution from reactions of CO2-rich aqueous solutions with fractured basalt

NASA Astrophysics Data System (ADS)

Wells, R. K.; Xiong, W.; Bae, Y.; Sesti, E.; Skemer, P. A.; Giammar, D.; Conradi, M.; Ellis, B. R.; Hayes, S. E.

2015-12-01

The injection of CO2 into fractured basalts is one of several possible solutions to mitigate global climate change; however, research on carbonation in natural basalts in relation to carbon sequestration is limited, which impedes our understanding of the processes that may influence the viability of this strategy. We are conducting bench-scale experiments to characterize the mineral dissolution and precipitation and the evolution of permeability in synthetic and natural basalts exposed to CO2-rich fluids. Analytical methods include optical and electron microscopy, electron microprobe, Raman spectroscopy, nuclear magnetic resonance (NMR), and micro X-ray computed tomography (μCT) with variable flow rates. Reactive rock and mineral samples consist of 1) packed powders of olivine or natural basalt, and 2) sintered cores of olivine or a synthetic basalt mixture. Each sample was reacted in a batch reactor at 100 °C, and 100 bars CO2. Magnesite is detected within one day in olivine packed beds, and within 15 days in olivine sintered cores. Forsterite and synthetic basalt sinters were also reacted in an NMR apparatus at 102 °C and 65 bars CO2. Carbonate signatures are observed within 72 days of reaction. Longer reaction times are needed for carbonate precipitation in natural basalt samples. Cores from the Columbia River flood basalt flows that contain Mg-rich olivine and a serpentinized basalt from Colorado were cut lengthwise, the interface mechanically roughened or milled, and edges sealed with epoxy to simulate a fractured interface. The cores were reacted in a batch reactor at 50-150 °C and 100 bars CO2. At lower temperatures, calcite precipitation is rare within the fracture after 4 weeks. At higher temperatures, numerous calcite and aragonite crystals are observed within 1 mm of the fracture entrance along the roughened fracture surface. In flow-through experiments, permeability decreased along the fracture paths within a few hours to several days of flow.

Mechanism analysis on finishing of reaction-sintered silicon carbide by combination of water vapor plasma oxidation and ceria slurry polishing

NASA Astrophysics Data System (ADS)

Shen, Xinmin; Tu, Qunzhang; Deng, Hui; Jiang, Guoliang; Yamamura, Kazuya

2015-05-01

Reaction-sintered silicon carbide (RS-SiC), which is considered as a promising mirror material for space telescope systems, requires a high surface property. An ultrasmooth surface with a Ra surface roughness of 0.480 nm was obtained after water vapor plasma oxidation for 90 min followed by ceria slurry polishing for 40 min. The oxidation process of RS-SiC by water vapor plasma was analyzed based on the Deal-Grove model, and the theoretical calculation results are consistent with the measured data obtained by scanning white light interferometer (SWLI), scanning electron microscopy/energy-dispersive x-ray, and atomic force microscope. The polishing process of oxidized RS-SiC by ceria slurry was investigated according to the Preston equation, which would theoretically forecast the evolutions of RS-SiC surfaces along with the increasing of polishing time, and it was experimentally verified by comparing the surface roughnesses obtained by SWLI and the surface morphologies obtained by SEM. The mechanism analysis on the finishing of RS-SiC would be effective for the optimization of water vapor plasma oxidation parameters and ceria slurry polishing parameters, which will promote the application of RS-SiC substrates by improving the surface property obtained by the oxidation-assisted polishing method.

40 CFR 63.1543 - Standards for process and process fugitive sources.

Code of Federal Regulations, 2012 CFR

2012-07-01

... paragraphs (a)(1) through (9) of this section. (1) Sinter machine; (2) Blast furnace; (3) Dross furnace; (4... machine charging location; (7) Sinter machine discharge end; (8) Sinter crushing and sizing equipment; and (9) Sinter machine area. (b) No owner or operator of any existing, new, or reconstructed primary lead...

40 CFR 63.1543 - Standards for process and process fugitive sources.

Code of Federal Regulations, 2014 CFR

2014-07-01

... paragraphs (a)(1) through (9) of this section. (1) Sinter machine; (2) Blast furnace; (3) Dross furnace; (4... machine charging location; (7) Sinter machine discharge end; (8) Sinter crushing and sizing equipment; and (9) Sinter machine area. (b) No owner or operator of any existing, new, or reconstructed primary lead...

40 CFR 63.1543 - Standards for process and process fugitive sources.

Code of Federal Regulations, 2013 CFR

2013-07-01

... paragraphs (a)(1) through (9) of this section. (1) Sinter machine; (2) Blast furnace; (3) Dross furnace; (4... machine charging location; (7) Sinter machine discharge end; (8) Sinter crushing and sizing equipment; and (9) Sinter machine area. (b) No owner or operator of any existing, new, or reconstructed primary lead...

Microwave sintering of Ag-nanoparticle thin films on a polyimide substrate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fujii, S., E-mail: fujii.s.ap@m.titech.ac.jp; Department of Information and Communication System Engineering, National Institute of Technology, Okinawa College, Nago, Okinawa 905-2192; Kawamura, S.

2015-12-15

Ag-nanoparticle thin films on a polyimide substrate were subjected to microwave sintering by use of a single-mode waveguide applicator. A two-step sintering process was employed. First, at low conductivities of the film, the film sample was placed at the site of the maximum electric field and subjected to microwave irradiation. Second, when the conductivity of the film increased, the film sample was placed at the site of the maximum magnetic field and again subjected to microwave irradiation. The microwave sintering process was completed within 1.5 min, which is significantly lower than the time required for the oven heating process. Themore » resulting conductivity of the film, albeit only 30% of that of the bulk material, was seven times that of a film annealed at the same temperature in a furnace. Scanning electron microscopy images revealed that the nanoparticles underwent both grain necking and grain growth during microwave sintering. In addition, this sintering process was equivalent to the oven heating process performed at a 50 °C higher annealing temperature. An electromagnetic wave simulation and a heat transfer simulation of the microwave sintering process were performed to gain a thorough understanding of the process.« less

Experimental and simulation studies on grain growth in TiC and WC-based cermets during liquid phase sintering

NASA Astrophysics Data System (ADS)

Shin, Soon-Gi

2000-06-01

The grain growth behaviors of TiC and WC particles in TiC-Ni, TiC-Mo2C-Ni, WC-Co and WC-VC-Co alloys during liquid phase sintering were investigated for different Ni or Co contents and compared with the results of Monte Carlo simulations. In the experimental study, TiC-Ni and WC-Co alloys had a maximum grain size at a certain liquid volume fraction, while the grain size in TiC-Mo2C-Ni and WC-VC-Co alloys increased monotonically with an increasing liquid volume fraction. These results mean that the grain growth of these alloys cannot be explained by the conventional mechanisms for Ostwald ripening, namely diffusion or reaction controlled processes. Monte Carlo simulations with different energy relationships between solidliquid interfaces predicted the effect of the liquid volume fraction on grain size similar to the experimental results. The contiguous boundaries between solid (carbide) particles appear to influence the grain growth behavior in TiC- and WC-based alloys during liquid phase sintering.

Effect of sintering process on the magnetic and mechanical properties of sintered Nd-Fe-B magnets

NASA Astrophysics Data System (ADS)

Hu, Z. H.; Qu, H. J.; Zhao, J. Q.; Yan, C. J.; Liu, X. M.

2014-11-01

The magnetic and mechanical properties of sintered Nd-Fe-B magnets prepared by different sintering processes were investigated. The results showed that the intrinsic coercivity and fracture toughness of sintered Nd-Fe-B magnets first increased, and then declined with increasing annealing temperature. The optimum magnetic properties and fracture toughness of sintered Nd-Fe-B magnets were obtained at the annealing temperature of 540 °C. Sintering temperature increasing from 1047 °C to 1071 °C had hardly effect on the magnetic properties of sintered Nd-Fe-B magnets. The variation of Vickers hardness and fracture toughness was not the same with increasing sintering temperature, and the effect of sintering temperature on the mechanical properties was complex and irregular. The reasons for the variation on magnetic and mechanical properties were analyzed, and we presumed that the effect of microstructure on the mechanical properties was more sensitive than the magnetic properties through analyzing the microstructure of sintered Nd-Fe-B magnets.

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

NASA Astrophysics Data System (ADS)

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.

Debinding and Sintering of an Injection-Moulded Hypereutectic Al⁻Si Alloy.

PubMed

Ni, Jiaqi; Yu, Muhuo; Han, Keqing

2018-05-16

Hypereutectic Al⁻Si (20 wt.%) alloy parts were fabricated by employing a powder injection moulding (PIM) technique with a developed multi-component binder system composed of high-density polyethylene (35 wt.%), carnauba wax (62 wt.%) and stearic acid (3 wt.%). The feedstocks contained 83 wt.% metal powders. The debinding process was carried out by a combination of solvent extraction and thermal decomposition. The effects of solvent debinding variables such as kind of solvents, debinding temperatures and time, and the bulk surface area to volume ratios on the debinding process were investigated. Thermal debinding and the subsequent sintering process were carried out in a heating sequence under a nitrogen atmosphere. The influences of sintering temperature and sintering time on the mechanical properties and structure were considered. Under the optimal sintering condition, sintering at 550 °C for 3 h, the final sintering parts were free of distortion and exhibited good mechanical properties. Relative sintered density, Brinell hardness, and tensile strength were ~95.5%, 58 HBW and ~154, respectively.

Effect of starting powders on the sintering of nanostructured ZrO2 ceramics by colloidal processing

NASA Astrophysics Data System (ADS)

Suárez, Gustavo; Sakka, Yoshio; Suzuki, Tohru S.; Uchikoshi, Tetsuo; Zhu, Xinwen; Aglietti, Esteban F.

2009-04-01

The effect of starting powders on the sintering of nanostructured tetragonal zirconia was evaluated. Suspensions were prepared with a concentration of 10 vol.% by mixing a bicomponent mixture of commercial powders (97 mol.% monoclinic zirconia with 3 mol.% yttria) and by dispersing commercially available tetragonal zirconia (3YTZ, Tosoh). The preparation of the slurry by bead-milling was optimized. Colloidal processing using 50 μm zirconia beads at 4000 rpm generated a fully deagglomerated suspension leading to the formation of high-density consolidated compacts (62% of the theoretical density (TD) for the bicomponent suspension). Optimum colloidal processing of the bicomponent suspension followed by the sintering of yttria and zirconia allowed us to obtain nanostructured tetragonal zirconia. Three different sintering techniques were investigated: normal sintering, two-step sintering and spark plasma sintering. The inhibition of grain growth in the bicomponent mixed powders in comparison with 3YTZ was demonstrated. The inhibition of the grain growth may have been caused by inter-diffusion of cations during the sintering.

Enhanced Multiferroic Properties of YMnO3 Ceramics Fabricated by Spark Plasma Sintering Along with Low-Temperature Solid-State Reaction

PubMed Central

Wang, Meng; Wang, Ting; Song, Shenhua; Ravi, Muchakayala; Liu, Renchen; Ji, Shishan

2017-01-01

Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid-state reaction method, phase-pure YMnO3 ceramics are fabricated using spark plasma sintering (SPS). X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YMnO3 ceramics can be prepared by SPS at 1000 °C for 5 minutes with annealing at 800 °C for 2 h. The relative density of the sample is as high as 97%, which is much higher than those of the samples sintered by other methods. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods and SPS with ball-milling precursors, and the ferroelectric loops at room temperature can be detected. These findings indicate that the YMnO3 ceramics prepared by the low temperature solid reaction method and SPS possess excellent dielectric lossy ferroelectric properties at room temperature, and magnetic properties at low temperature (10 K), making them suitable for potential multiferroic applications. PMID:28772832

Phase transformations in the reaction cell of TiNi-based sintered systems

NASA Astrophysics Data System (ADS)

Artyukhova, Nadezhda; Anikeev, Sergey; Yasenchuk, Yuriy; Chekalkin, Timofey; Gunther, Victor; Kaftaranova, Maria; Kang, Ji-Hoon; Kim, Ji-Soon

2018-05-01

The present work addresses the structural-phase state changes of porous TiNi-based compounds fabricated by reaction sintering (RS) of Ti and Ni powders with Co, Mo, and no additives introduced. The study also emphasizes the features of a reaction cell (RC) during the transition from the solid- to liquid-phase sintering. Mechanisms of phase transformations occurring in the solid phase, involving the low-melting Ti2Ni phase within the RC, have been highlighted. Also, the intermediate Ti2Ni phase had a crucial role to provide both the required RS behavior and modified phase composition of RS samples, and besides, it is found to be responsible for the near-equiatomic TiNi saturation of the melt. Both cobalt and molybdenum additives are shown to cause additional structuring of the transition zone (TZ) at the Ti2Ni‑TiNi interface and broadening of this zone. The impact of Co and Mo on the Ti2Ni phase is evident through fissuring of this phase layer, which is referred to solidified stresses increased in the layer due to post-alloying defects in the structure.

A mechanistic study on the synthesis of β-Sialon whiskers from coal fly ash

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, H.; Wang, P.Y.; Yu, J.L., E-mail: jianglong.yu@newcastle.edu.au

2015-05-15

Graphical abstract: The appearance of bead-like whiskers indicated that the growth mechanism of the β-Sialon whiskers was different from the conventional one, in which a chain of droplets were formed and then consumed to participate in the formation of the whiskers. - Highlights: • β-Sialon whiskers were synthesized using waste fly ash by carbothemal reduction reaction under nitrogen atmosphere. • Rod-like β-Sialon whiskers with a diameter of 100–500 nm were formed. • Bead-like whiskers as intermediate morphology of the growing β-Sialon whiskers were found with increasing sintering time. • The growth mechanism of β-Sialon whiskers was different from the conventionalmore » VLS mechanism. • A chain of droplets were formed and participated in the formation of the whiskers. - Abstract: β-Sialon whiskers were produced at 1420 °C through carbothemal reduction reaction under nitrogen atmosphere using fly ash from coal-fired power plants. The effects of sintering time on the phase formation and morphology of the products were investigated by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectrometer (EDS) techniques. Rod-like β-Sialon whiskers with the diameter of 100–500 nm were successfully formed. With increasing sintering time, bead-like morphology during the growth process of the whiskers was found, and growth mechanism of β-Sialon whiskers was also discussed in detail. The growth mechanism proposed in this study was different from the conventional vapor–liquid–solid (VLS) mechanism.« less

Effect of sintering temperature on the electrolysis of TiO2

NASA Astrophysics Data System (ADS)

Li, Ze-quan; Ru, Li-yue; Bai, Cheng-guang; Zhang, Na; Wang, Hai-hua

2012-07-01

The effects of sintering temperature on the microstructure and the conductivity of TiO2 cathodes were studied by examining the phase composition, microstructure, and element contents of the sintered cathodes and the cathodic products using X-ray diffraction and scanning electronic microscopy-energy dispersive spectrometry. The oxygen vacancy, conductivity, average pore diameter, and specific surface area of the sintered cathodes were detected by X-ray photoelectron spectroscopy, four-point probe, and ASPA 2010. The results showed that TiO2 phase transformations occurred, and oxygen vacancies formed with the increase of sintering temperature. The cathodic conductivity improved, but the average pore diameter and the effective response area of the TiO2 cathode were reduced when the sintering temperature increased. These phenomena could weaken the contact between reaction ions and electrons and also had the same effect on the cathodes and the molten salt. Moreover, they were disadvantageous to ion migration, so a lower sintering temperature was favorable for the microstructure of electrolysis. Consequently, the cathodic conductivity may be improved, but the microstructure became compact with the increase of sintering temperature. The cathodic products at different temperatures indicated that the cathodic conductivity was more important for electrolysis.

Sintering Kinetics of Inkjet Printed Conductive Silver Lines on Insulating Plastic Substrate

DOE PAGES

Zhou, Wenchao; List, III, Frederick Alyious; Duty, Chad E; ...

2015-01-24

This paper focuses on sintering kinetics of inkjet printed lines containing silver nanoparticles deposited on a plastic substrate. Upon heat treatment, the change of resistance in the printed lines was measured as a function of time and sintering temperatures from 150 to 200 C. A critical temperature was observed for the sintering process, beyond which there was no further reduction in resistance. Analysis shows the critical temperature correlates to the boiling point of the solvent, which is attributed to a liquid-mediated sintering mechanism. It is demonstrated that the sintering process shuts down after the solvent has completely evaporated.

Pressureless sintered beta prime-Si3N4 solid solution: Fabrication, microstructure, and strength

NASA Technical Reports Server (NTRS)

Dutta, S.

1977-01-01

Si3N4, AlN, and Al2O3 were used as basic constituents in a study of the pressureless sintering of beta prime-Si3N4 solid solution as a function of temperature. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 MPa were achieved at moderate temperature (1000 C), but decreased to 228 MPa at 1380 C. This substantial strength loss was attributed to a glassy grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Design of Nanomaterial Synthesis by Aerosol Processes

PubMed Central

Buesser, Beat; Pratsinis, Sotiris E.

2013-01-01

Aerosol synthesis of materials is a vibrant field of particle technology and chemical reaction engineering. Examples include the manufacture of carbon blacks, fumed SiO2, pigmentary TiO2, ZnO vulcanizing catalysts, filamentary Ni, and optical fibers, materials that impact transportation, construction, pharmaceuticals, energy, and communications. Parallel to this, development of novel, scalable aerosol processes has enabled synthesis of new functional nanomaterials (e.g., catalysts, biomaterials, electroceramics) and devices (e.g., gas sensors). This review provides an access point for engineers to the multiscale design of aerosol reactors for the synthesis of nanomaterials using continuum, mesoscale, molecular dynamics, and quantum mechanics models spanning 10 and 15 orders of magnitude in length and time, respectively. Key design features are the rapid chemistry; the high particle concentrations but low volume fractions; the attainment of a self-preserving particle size distribution by coagulation; the ratio of the characteristic times of coagulation and sintering, which controls the extent of particle aggregation; and the narrowing of the aggregate primary particle size distribution by sintering. PMID:22468598

Design of nanomaterial synthesis by aerosol processes.

PubMed

Buesser, Beat; Pratsinis, Sotiris E

2012-01-01

Aerosol synthesis of materials is a vibrant field of particle technology and chemical reaction engineering. Examples include the manufacture of carbon blacks, fumed SiO(2), pigmentary TiO(2), ZnO vulcanizing catalysts, filamentary Ni, and optical fibers, materials that impact transportation, construction, pharmaceuticals, energy, and communications. Parallel to this, development of novel, scalable aerosol processes has enabled synthesis of new functional nanomaterials (e.g., catalysts, biomaterials, electroceramics) and devices (e.g., gas sensors). This review provides an access point for engineers to the multiscale design of aerosol reactors for the synthesis of nanomaterials using continuum, mesoscale, molecular dynamics, and quantum mechanics models spanning 10 and 15 orders of magnitude in length and time, respectively. Key design features are the rapid chemistry; the high particle concentrations but low volume fractions; the attainment of a self-preserving particle size distribution by coagulation; the ratio of the characteristic times of coagulation and sintering, which controls the extent of particle aggregation; and the narrowing of the aggregate primary particle size distribution by sintering.

Electrochemical Synthesis of Core-Shell-Structured NbC-Fe Composite Powder for Enforcement in Low-Carbon Steel.

PubMed

Li, Hongmei; Song, Qiushi; Xu, Qian; Chen, Ying; Xu, Liang; Man, Tiannan

2017-11-01

An NbC-Fe composite powder was synthesized from an Nb₂O₅/Fe/C mixture by electrochemical reduction and subsequent carbonization in molten CaCl₂-NaCl. The composite has a core-shell structure, in which NbC acts as the cores distributing in the Fe matrix. A strong bonding between NbC and Fe is benefit from the core-shell structure. The sintering and electrochemical reduction processes were investigated to probe the mechanism for the reactions. The results show that NbC particles about several nanometers were embraced by the Fe shell to form a composite about 100 nm in size. This featured structure can feasibly improve the wettability and sinterability of NbC as well as the uniform distribution of the carbide in the cast steel. By adding the composite into steel in the casting process, the grain size of the casted steel was markedly deceased from 1 mm to 500 μm on average, favoring the hardening of the casted steel.

Microstructural development of cobalt ferrite ceramics and its influence on magnetic properties

NASA Astrophysics Data System (ADS)

Kim, Gi-Yeop; Jeon, Jae-Ho; Kim, Myong-Ho; Suvorov, Danilo; Choi, Si-Young

2013-11-01

The microstructural evolution and its influence on magnetic properties in cobalt ferrite were investigated. The cobalt ferrite powders were prepared via a solid-state reaction route and then sintered at 1200 °C for 1, 2, and 16 h in air. The microstructures from sintered samples represented a bimodal distribution of grain size, which is associated with abnormal grain growth behavior. And thus, with increasing sintering time, the number and size of abnormal grains accordingly increased but the matrix grains were frozen with stagnant grain growth. In the sample sintered for 16 h, all of the matrix grains were consumed and the abnormal grains consequently impinged on each other. With the appearance of abnormal grains, the magnetic coercivity significantly decreased from 586.3 Oe (1 h sintered sample) to 168.3 Oe (16 h sintered sample). This is due to the magnetization in abnormal grains being easily flipped. In order to achieve high magnetic coercivity of cobalt ferrite, it is thus imperative to fabricate the fine and homogeneous microstructure.

Correlation between structural, electrical and magnetic properties of GdMnO3 bulk ceramics

NASA Astrophysics Data System (ADS)

Samantaray, S.; Mishra, D. K.; Pradhan, S. K.; Mishra, P.; Sekhar, B. R.; Behera, Debdhyan; Rout, P. P.; Das, S. K.; Sahu, D. R.; Roul, B. K.

2013-08-01

This paper reports the effect of sintering temperature on ferroelectric properties of GdMnO3 (GMO) bulk ceramics at room temperature prepared by the conventional solid state reaction route following slow step sintering schedule. Ferroelectric hysteresis loop as well as sharp dielectric anomaly in pure (99.999%) GMO sintered ceramics has been clearly observed. Samples sintered at 1350 °C become orthorhombic with Pbnm space group and showed frequency independent sharp dielectric anomalies at 373 K and a square type of novel ferroelectric hysteresis loop was observed at room temperature. Interestingly, dielectric anomalies and ferroelectric behavior were observed to be dependent upon sintering temperature of GdMnO3. Room temperature dielectric constant (ɛr) value at different frequencies is observed to be abnormally high. The magnetic field and temperature dependent magnetization show antiferromagnetic behavior at 40 K for both 1350 °C and 1700 °C sintered GMO. Present findings showed the possibility of application of GdMnO3 at room temperature as multifunctional materials.

Process for the production of metal nitride sintered bodies and resultant silicon nitride and aluminum nitride sintered bodies

NASA Technical Reports Server (NTRS)

Yajima, S.; Omori, M.; Hayashi, J.; Kayano, H.; Hamano, M.

1983-01-01

A process for the manufacture of metal nitride sintered bodies, in particular, a process in which a mixture of metal nitrite powders is shaped and heated together with a binding agent is described. Of the metal nitrides Si3N4 and AIN were used especially frequently because of their excellent properties at high temperatures. The goal is to produce a process for metal nitride sintered bodies with high strength, high corrosion resistance, thermal shock resistance, thermal shock resistance, and avoidance of previously known faults.

3-D laser confocal microscopy study of the oxidation of NdFeB magnets in atmospheric conditions

NASA Astrophysics Data System (ADS)

Meakin, J. P.; Speight, J. D.; Sheridan, R. S.; Bradshaw, A.; Harris, I. R.; Williams, A. J.; Walton, A.

2016-08-01

Neodymium iron boron (NdFeB) magnets are used in a number of important applications, such as generators in gearless wind turbines, motors in electric vehicles and electronic goods (e.g.- computer hard disk drives, HDD). Hydrogen can be used as a processing gas to separate and recycle scrap sintered Nd-Fe-B magnets from end-of-life products to form a powder suitable for recycling. However, the magnets are likely to have been exposed to atmospheric conditions prior to processing, and any oxidation could lead to activation problems for the hydrogen decrepitation reaction. Many previous studies on the oxidation of NdFeB magnets have been performed at elevated temperatures; however, few studies have been formed under atmospheric conditions. In this paper a combination of 3-D laser confocal microscopy and Raman spectroscopy have been used to assess the composition, morphology and rate of oxidation/corrosion on scrap sintered NdFeB magnets. Confocal microscopy has been employed to measure the growth of surface reaction products at room temperature, immediately after exposure to air. The results showed that there was a significant height increase at the triple junctions of the Nd-rich grain boundaries. Using Raman spectroscopy, the product was shown to consist of Nd2O3 and formed only on the Nd-rich triple junctions. The diffusion coefficient of the triple junction reaction product growth at 20 °C was determined to be approximately 4 × 10-13 cm2/sec. This value is several orders of magnitude larger than values derived from the diffusion controlled oxide growth observations at elevated temperatures in the literature. This indicates that the growth of the room temperature oxidation products are likely defect enhanced processes at the NdFeB triple junctions.

Ultrasonic sensor based defect detection and characterisation of ceramics.

PubMed

Kesharaju, Manasa; Nagarajah, Romesh; Zhang, Tonzhua; Crouch, Ian

2014-01-01

Ceramic tiles, used in body armour systems, are currently inspected visually offline using an X-ray technique that is both time consuming and very expensive. The aim of this research is to develop a methodology to detect, locate and classify various manufacturing defects in Reaction Sintered Silicon Carbide (RSSC) ceramic tiles, using an ultrasonic sensing technique. Defects such as free silicon, un-sintered silicon carbide material and conventional porosity are often difficult to detect using conventional X-radiography. An alternative inspection system was developed to detect defects in ceramic components using an Artificial Neural Network (ANN) based signal processing technique. The inspection methodology proposed focuses on pre-processing of signals, de-noising, wavelet decomposition, feature extraction and post-processing of the signals for classification purposes. This research contributes to developing an on-line inspection system that would be far more cost effective than present methods and, moreover, assist manufacturers in checking the location of high density areas, defects and enable real time quality control, including the implementation of accept/reject criteria. Copyright © 2013 Elsevier B.V. All rights reserved.

A Novel Process for Joining Ti Alloy and Al Alloy using Two-Stage Sintering Powder Metallurgy

NASA Astrophysics Data System (ADS)

Long, Luping; Liu, Wensheng; Ma, Yunzhu; Wu, Lei; Liu, Chao

2018-04-01

The major challenges for conventional diffusion bonding of joining Ti alloy and Al alloy are the undesirable interfacial reaction, low matrixes and joint strength. To avoid the problem in diffusion bonding, a novel two-stage sintering powder metallurgy process is developed. In the present work, the interface characterization and joint performance of the bonds obtained by powder metallurgy bonding are investigated and are compared with the diffusion bonded Ti/Al joints obtained with the same and the optimized process parameters. The results show that no intermetallic compound is visible in the Ti/Al joint obtained by powder metallurgy bonding, while a new layer formed at the joint diffusion bonded with the same parameters. The maximum tensile strength of joint obtained by diffusion bonding is 58 MPa, while a higher tensile strength reaching 111 MPa for a bond made by powder metallurgy bonding. Brittle fractures occur at all the bonds. It is shown that the powder metallurgy bonding of Ti/Al is better than diffusion bonding. The results of this study should benefit the bonding quality.

Corrosion Issues for Ceramics in Gas Turbines

NASA Technical Reports Server (NTRS)

Jacobson, Nathan S.; Fox, Dennis S.; Smialek, James L.; Opila, Elizabeth J.; Tortorelli, Peter F.; More, Karren L.; Nickel, Klaus G.; Hirata, Takehiko; Yoshida, Makoto; Yuri, Isao

2000-01-01

The requirements for hot-gas-path materials in gas turbine engines are demanding. These materials must maintain high strength and creep resistance in a particularly aggressive environment. A typical gas turbine environment involves high temperatures, rapid gas flow rates, high pressures, and a complex mixture of aggressive gases. Figure 26.1 illustrates the requirements for components of an aircraft engine and critical issues [1]. Currently, heat engines are constructed of metal alloys, which meet these requirements within strict temperature limits. In order to extend these temperature limits, ceramic materials have been considered as potential engine materials, due to their high melting points and stability at high temperatures. These materials include oxides, carbides, borides, and nitrides. Interest in using these materials in engines appears to have begun in the 1940s with BeO-based porcelains [2]. During the 1950s, the efforts shifted to cermets. These were carbide-based materials intended to exploit the best properties of metals and ceramics. During the 1960s and 1970s, the silicon-based ceramics silicon carbide (SiC) and silicon nitride (Si3N4) were extensively developed. Although the desirable high-temperature properties of SiC and Si3N4 had long been known, consolidation of powders into component-sized bodies required the development of a series of specialized processing routes [3]. For SiC, the major consolidation routes are reaction bonding, hot-pressing, and sintering. The use of boron and carbon as additives which enable sintering was a particularly noteworthy advance [4]. For Si3N4 the major consolidation routes are reaction bonding and hot pressing [5]. Reaction-bonding involves nitridation of silicon powder. Hot pressing involves addition of various refractory oxides, such as magnesia (MgO), alumina (Al2O3), and yttria (y2O3). Variations on these processes include a number of routes including Hot Isostatic Pressing (HIP), gas-pressure sintering, sinter-HIPing, and Encapsulation-HIPing. It is important to note that each process involves the addition of secondary elements, which later were shown to dramatically influence oxidation and corrosion behavior. As dense bodies of silicon-based ceramics became more readily available, their desirable high temperature properties were confirmed. These materials retained strength to very high temperatures (i.e. 1300-1400 C). Further, they were lightweight and made from abundant materials. SiC and Si3N4 therefore emerged as leading ceramic candidates for components in heat engines, designed to operate at higher temperatures for better performance and fuel efficiency. The first US programs for ceramics in heat engines have been reviewed [6]. Selected programs on ceramic engine parts are summarized here in regard to their contributions to understanding the corrosion behavior of a heat engine environment.

A method for phenomenological and chemical kinetics study of autocatalytic reactive dissolution by optical microscopy. The case of uranium dioxide dissolution in nitric acid media

NASA Astrophysics Data System (ADS)

Marc, Philippe; Magnaldo, Alastair; Godard, Jérémy; Schaer, Éric

2018-03-01

Dissolution is a milestone of the head-end of hydrometallurgical processes, as the stabilization rates of the chemical elements determine the process performance and hold-up. This study aims at better understanding the chemical and physico-chemical phenomena of uranium dioxide dissolution reactions in nitric acid media in the Purex process, which separates the reusable materials and the final wastes of the spent nuclear fuels. It has been documented that the attack of sintering-manufactured uranium dioxide solids occurs through preferential attack sites, which leads to the development of cracks in the solids. Optical microscopy observations show that in some cases, the development of these cracks leads to the solid cleavage. It is shown here that the dissolution of the detached fragments is much slower than the process of the complete cleavage of the solid, and occurs with no disturbing phenomena, like gas bubbling. This fact has motivated the measurement of dissolution kinetics using optical microscopy and image processing. By further discriminating between external resistance and chemical reaction, the "true" chemical kinetics of the reaction have been measured, and the highly autocatalytic nature of the reaction confirmed. Based on these results, the constants of the chemical reactions kinetic laws have also been evaluated.

Verification of the Skorohod-Olevsky Viscous Sintering (SOVS) Model

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lester, Brian T.

2017-11-16

Sintering refers to a manufacturing process through which mechanically pressed bodies of ceramic (and sometimes metal) powders are heated to drive densification thereby removing the inherit porosity of green bodies. As the body densifies through the sintering process, the ensuing material flow leads to macroscopic deformations of the specimen and as such the final configuration differs form the initial. Therefore, as with any manufacturing step, there is substantial interest in understanding and being able to model the sintering process to predict deformation and residual stress. Efforts in this regard have been pursued for face seals, gear wheels, and consumer productsmore » like wash-basins. To understand the sintering process, a variety of modeling approaches have been pursued at different scales.« less

Electrical conductivity and molten salt corrosion behavior of spinel nickel ferrite

NASA Astrophysics Data System (ADS)

Liu, Baogang; Zhang, Lei; Zhou, Kechao; Li, Zhiyou; Wang, Hao

2011-08-01

Nickel ferrite was prepared by solid-state reaction at 1300 °C as inert anode for aluminum electrolysis. DC conductivities and molten salt corrosion behavior of the samples were investigated in detail regarding the effects of different sintering atmospheres. X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray analysis were used to analyse the phase compositions and microstructures. The DC conductivities of the samples sintered in nitrogen showed a drastic increase compared to those sintered in air, and at 960 °C they increased from 1.94 S/cm to 22.65 S/cm. The samples sintered in nitrogen showed much better corrosion resistance than those sintered in air, attributing to the formation of the dense protective layers in the anode surfaces during the electrolysis at 960 °C. The conductive mechanism and molten salt corrosion behavior were also discussed.

Ash chemistry and sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skrifvars, B.J.; Backman, R.; Hupa, M.

1996-10-01

The chemistry of a fuel ash is important to consider when ash behavior in combustion or gasification is studied. Four different types of thermal behavior based bed agglomeration and deposit foliation mechanisms have been proposed to be important, (1) partial melting, (2) viscous flow, (3) chemical reaction sintering, and (4) solid state sintering. In this paper we present data from a broader study in which we have quantified the four mechanisms more in detail. The ashes from 10 different types of fuels have been tested for their sintering tendency by a compression strength sintering test. The ashes were also subjectmore » to quantitative wet chemical analyses and combined differential thermal, thermogravimetric (DT/TG) analyses. These thermal behavior predictions were compared with multi-component multi-phase thermodynamic phase equilibrium calculations and further with full scale combustion experience. The results and their relevance to full scale conversion systems are discussed in the paper.« less

Enhanced Densification and Hardness of Titanium Bodies Sintered by Advanced Hydrogen Sintering Process

NASA Astrophysics Data System (ADS)

Oh, Jung-Min; Koo, Ja-Geon; Lim, Jae-Won

2018-05-01

A new sintering technique for enhancing a densification and hardness of sintered titanium body by supplying hydrogen was developed (Hydrogen Sintering Process, HSP). The HSP was developed by only injecting hydrogen into an argon atmosphere during the core time. As a result, sound titanium sintered bodies with high density and hardness were obtained by the HSP. In addition, a pore size and number of the HSP specimens were smaller than those of the argon atmosphere specimen. It was found that the injecting hydrogen into the argon atmosphere by HSP can prevent the formation of oxide layers, resulting in enhanced densification and hardness.

Rapid sintering of anisotropic, nanograined Nd-Fe-B by flash-spark plasma sintering

NASA Astrophysics Data System (ADS)

Castle, Elinor; Sheridan, Richard; Grasso, Salvatore; Walton, Allan; Reece, Mike

2016-11-01

A Spark Plasma Sintering (SPS) furnace was used to Flash-Sinter (FS) Nd-Fe-Dy-Co-B-Ga melt spun permanent magnetic material. During the 10 s "Flash" process (heating rate 2660 K min-1), sample sintering (to theoretical density) and deformation (54% height reduction) occurred. This produced texturing and significant magnetic anisotropy, comparable to conventional die-upset magnets; yet with much greater coercivities (>1600 kA m-1) due to the nanoscale characteristics of the plate-like sintered grains. These preliminary results suggest that Flash-SPS could provide a new processing route for the mass production of highly anisotropic, nanocrystalline magnetic materials with high coercivity.

Solvent/non-solvent sintering: a novel route to create porous microsphere scaffolds for tissue regeneration.

PubMed

Brown, Justin L; Nair, Lakshmi S; Laurencin, Cato T

2008-08-01

Solvent/non-solvent sintering creates porous polymeric microsphere scaffolds suitable for tissue engineering purposes with control over the resulting porosity, average pore diameter, and mechanical properties. Five different biodegradable biocompatible polyphosphazenes exhibiting glass transition temperatures from -8 to 41 degrees C and poly (lactide-co-glycolide), (PLAGA) a degradable polymer used in a number of biomedical settings, were examined to study the versatility of the process and benchmark the process to heat sintering. Parameters such as: solvent/non-solvent sintering solution composition and submersion time effect the sintering process. PLAGA microsphere scaffolds fabricated with solvent/non-solvent sintering exhibited an interconnected porosity and pore size of 31.9% and 179.1 mum, respectively which was analogous to that of conventional heat sintered PLAGA microsphere scaffolds. Biodegradable polyphosphazene microsphere scaffolds exhibited a maximum interconnected porosity of 37.6% and a maximum compressive modulus of 94.3 MPa. Solvent/non-solvent sintering is an effective strategy for sintering polymeric microspheres, with a broad spectrum of glass transition temperatures, under ambient conditions making it an excellent fabrication route for developing tissue engineering scaffolds and drug delivery vehicles. (c) 2007 Wiley Periodicals, Inc.

Solvent/Non-Solvent Sintering: A Novel Route to Create Porous Microsphere Scaffolds For Tissue Regeneration

PubMed Central

Brown, Justin L.; Nair, Lakshmi S.; Laurencin, Cato T.

2009-01-01

Solvent/non-solvent sintering creates porous polymeric microsphere scaffolds suitable for tissue engineering purposes with control over the resulting porosity, average pore diameter and mechanical properties. Five different biodegradable biocompatible polyphosphazenes exhibiting glass transition temperatures from −8°C to 41oC and poly(lactide-co-glycolide), (PLAGA) a degradable polymer used in a number of biomedical settings, were examined to study the versatility of the process and benchmark the process to heat sintering. Parameters such as: solvent/non-solvent sintering solution composition and submersion time effect the sintering process. PLAGA microsphere scaffolds fabricated with solvent/non-solvent sintering exhibited an interconnected porosity and pore size of 31.9% and 179.1µm respectively which was analogous to that of conventional heat sintered PLAGA microsphere scaffolds. Biodegradable polyphosphazene microsphere scaffolds exhibited a maximum interconnected porosity of 37.6% and a maximum compressive modulus of 94.3MPa. Solvent/non-solvent sintering is an effective strategy for sintering polymeric microspheres, with a broad spectrum of glass transition temperatures, under ambient conditions making it an excellent fabrication route for developing tissue engineering scaffolds and drug delivery vehicles. PMID:18161819

Densification behavior of ceramic and crystallizable glass materials constrained on a rigid substrate

NASA Astrophysics Data System (ADS)

Calata, Jesus N.

2005-11-01

Constrained sintering is an important process for many applications. The sintering process almost always involves some form of constraint, both internal and external, such as rigid particles, reinforcing fibers and substrates to which the porous body adheres. The densification behavior of zinc oxide and cordierite-base crystallizable glass constrained on a rigid substrate was studied to add to the understanding of the behavior of various materials undergoing sintering when subjected to external substrate constraint. Porous ZnO films were isothermally sintered at temperatures between 900°C and 1050°C. The results showed that the densification of films constrained on substrates is severely reduced. This was evident in the sintered microstructures where the particles are joined together by narrower necks forming a more open structure, instead of the equiaxed grains with wide grain boundaries observed in the freestanding films. The calculated activation energies of densification were also different. For the density range of 60 to 64%, the constrained film had an activation energy of 391 +/- 34 kJ/mole compared to 242 +/- 21 kJ/mole for the freestanding film, indicating a change in the densification mechanism. In-plane stresses were observed during the sintering of the constrained films. Yielding of the films, in which the stresses dropped slight or remained unchanged, occurred at relative densities below 60% before the stresses climbed linearly with increasing density followed by a gradual relaxation. A substantial amount of the stresses remained after cooling. Free and constrained films of the cordierite-base crystallizable glass (glass-ceramic) were sintered between 900°C and 1000°C. The substrate constraint did not have a significant effect on the densification rate but the constrained films eventually underwent expansion. Calculations of the densification activation energy showed that, on average, it was close to 1077 kJ/mole, the activation energy of the glass, indicating that the prevailing mechanism was still viscous flow. The films expanded earlier and faster with increasing sintering temperature. The expansion was traced to the formation of pores at the interface with the silicon substrate and to a lesser extent on aluminum nitride. It was significantly reduced when the silicon substrate was pre-oxidized at 900°C, leading to the conclusion that the pore formation at the interface was due to poor wetting, which in turn was caused by the loss of the thin oxide layer through a reaction with the glass.

A new ferroelectric solid solution system of LaCrO 3-BiCrO 3

NASA Astrophysics Data System (ADS)

Chen, J. I. L.; Kumar, M. Mahesh; Ye, Z.-G.

2004-04-01

A new perovskite solid solution system of (1- x)LaCrO 3- xBiCrO 3 has been prepared by conventional solid-state reaction and sintering processes at 1200°C in a sealed Pt tube or a Bi 2O 3-rich environment. A clean orthorhombic phase of LaCrO 3-type structure is established at room temperature for compositions with 0⩽ x⩽0.35. The relative density, lattice parameters, sintering mechanism, microstructure and ferroelectricity of the compounds are investigated. The substitution of Bi 2O 3 for La 2O 3 is found to decrease the unit cell volume and increase the grain size of the ceramics. The relative density of the ceramics sintered at 1200°C is significantly improved from 40% for LaCrO 3 up to about 90% for La 0.65Bi 0.35CrO 3 through a liquid phase sintering mechanism. The ferroelectricity is revealed in La 1- xBi xCrO 3 with 0.1⩽ x⩽0.35 by dielectric hysteresis loops displayed at 77 K. The remnant polarization is found to increase with increasing Bi 3+ content. The origin of the ferroelectricity is attributed to the structural distortion induced by the stereochemically active Bi 3+ ion on the A site.

New Polymer Materials for the Laser Sintering Process: Polypropylene and Others

NASA Astrophysics Data System (ADS)

Wegner, Andreas

Laser sintering of polymers gets more and more importance for small series production. However, there is only a little number of materials available for the process. In most cases parts are build up using polyamide 12 or polyamide 11. Reasons for that are high prices, a restricted availability, poor mechanical part properties or an insufficient understanding of the processing of other materials. These problems result from the complex processing conditions in laser sintering with high requirements on the material's characteristics. Within this area, at the chair for manufacturing technology fundamental knowledge was established. Aim of the presented study was to qualify different polymers for the laser sintering process. Polyethylene, polypropylene, polyamide 6, polyoxymethylene as well as polybutylene terephthalate were analyzed. Within the study problems of qualifying new materials are discussed using some examples. Furthermore, the processing conditions as well as mechanical properties of a new polypropylene compound are shown considering also different laser sintering machines.

Mechanochemical stabilization and sintering of nanocrystalline the (ZrO2)0.97 (Y2O3)0.03 solid solution from pure oxides

NASA Astrophysics Data System (ADS)

Rendtorff, N. M.; Suárez, G.; Sakka, Y.; Aglietti, E. F.

2011-10-01

The mechanochemical activation processing has proved to be an effective technique to enhance a solid-state reaction at relatively low temperatures. In such a process, the mechanical effects of milling, such as reduction of particle size and mixture homogenization, are accompanied by chemical effects, such as partial decomposition of salts or hydroxides resulting in very active reactants. The objective of the present work is to obtain (ZrO2)0.97(Y2O3)0.03 nanocrystalline tetragonal solid solution powders directly using a high energy milling on a mixture of the pure oxides. A second objective is to evaluate the efficiency of the processing proposed and to characterize both textural and structural evolution of the mixtures during the milling processes and throughout posterior low temperature treatments. The Textural and structural evolution were studied by XRD analysis, specific area measurements (BET) and SEM. Firstly a decrease of the crystallinity of the reactants was observed, followed by the disappearance of Y2O3 diffraction peaks and the partial appearance of the tetragonal phase at room temperature. The solid solution proportion was increased with the high energy milling time, obtaining complete stabilization of the tetragonal solid solution with long milling treatments (60 min).The obtained powders were uniaxially pressed and sintered at different temperatures (600-1400°C) the influence of the milling time was correlated with the sinterization degree and final crystalline composition of the materials. Finally, fully stabilized nanocrystalline zirconia materials were obtained satisfactorily by the proposed method.

A study on flash sintering and related phenomena in titania and its composite with alumina

NASA Astrophysics Data System (ADS)

Shikhar

In 2010, Cologna et. al. [1] reported that with a help of small electric field 120 Vcm-1, the sintering temperature of 3 mol % yittria stabilized zirconia could be brought down to 850°C from 1450°C. On top of reducing the temperature requirements, the green sample could be sintered from starting density of 50% to near full density in mere 5 seconds, a sintering rate three orders of magnitude higher than conventional methods. This discovery led to the emergence of a new field of enhanced sintering with electric field, named "Flash Sintering". The objective of this thesis is to understand the phenomenological behavior of flash-sintering and related phenomena on titania and its composites with alumina at elevated temperature. The possible mechanisms to explain flash sintering are discussed: Joule heating and the avalanche of defect generation [2], both induced by the rapid rise in conductivity just before the onset of the flash. Apparently, both mechanisms play a role. The thesis covers the response of pure titania and composites of titania-alumina under flash and compared with conventional sintering. We start with the sintering behavior of pure titania and observe lowering of sintering temperature requirements with higher applied electric field. The conductivity of titania during flash is also measured, and compared with the nominal conductivity of titania at equivalent temperatures. The conductivity during flash is determined to be have a different activation energy. For the composites of titania-alumina, effect of flash on the constrained sintering was studied. It is a known fact that sintering of one component of composite slows down when the other component of a different densification rate is added to it, called constrained sintering. In our case, large inclusions of alumina particles were added to nano-grained titania green compact that hindered its densification. Flash sintering was found to be overcoming this problem and near full densification was achieved. In another experiment, effect of high current density and hold time under flash on the chemical reaction (phase transformation) of titania and alumina to form Al2TiO5 is studied. It was found that not only flash enhances the kinetics of reaction when compared with conventional heating at equivalent temperatures, but also brought down the phase transformation temperature for this spinel formation, as reported by the phase diagram. In-situ X-ray diffraction experiments were performed at the synchrotron facility in Argonne National Laboratory. The specimen temperature were measured during the experiment on the basis of peak shift with temperature and were found to be matching with our predicted values by Black-Body-Radiation model. We also observed the instant evolution of texture in grain orientation of pure titania under flash and their disappearance as the fields were switched off. Study on chemical kinetics between titania and alumina were also performed which supported our findings of in-house experiments.

Energy-Saving Sintering of Electrically Conductive Powders by Modified Pulsed Electric Current Heating Using an Electrically Nonconductive Die

NASA Astrophysics Data System (ADS)

Ito, Mikio; Kawahara, Kenta; Araki, Keita

2014-04-01

Sintering of Cu and thermoelectric Ca3Co4O9 was tried using a modified pulsed electric current sintering (PECS) process, where an electrically nonconductive die was used instead of a conventional graphite die. The pulsed electric current flowed through graphite punches and sample powder, which caused the Joule heating of the powder compact itself, resulting in sintering under smaller power consumption. Especially for the Ca3Co4O9 powder, densification during sintering was also accelerated by this modified PECS process.

Al2O3-TiC Composite Prepared by Spark Plasma Sintering Process: Evaluation of Mechanical and Tribological Properties

NASA Astrophysics Data System (ADS)

Kumar, Rohit; Chaubey, A. K.; Bathula, Sivaiah; Prashanth, K. G.; Dhar, Ajay

2018-03-01

Al2O3-10TiC composites were synthesized by spark plasma sintering (SPS) process. Microstructural and mechanical properties of the composite reveal homogeneous distribution of the fine TiC particles in the matrix. The samples were produced with different sintering temperature, and it shows that the hardness and density gradually increases with increasing sintering temperature. Abrasion wear test result reveals that the composite sintered at 1500 °C shows high abrasion resistance (wt. loss 0.016 g) and the lowest abrasion resistance was observed for the composite sample sintered at 1100 °C (wt. loss 1.459 g). The profilometry surface roughness study shows that sample sintered at 1100 °C shows maximum roughness ( R a = 6.53 µm) compared to the sample sintered at 1500 °C ( R a = 0.66 µm) corroborating the abrasion wear test results.

New materials through a variety of sintering methods

NASA Astrophysics Data System (ADS)

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.

Behavior of Oxide Film at Interface between Particles of Al-Mg Alloy Powder Compacts Prepared by Pulse Electric Current Sintering

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Yamaguchi, Norio; Song, Minghui; Mitsuishi, Kazutaka; Furuya, Kazuo; Noda, Tetsuji

2003-07-01

Al-1.0 mass% Mg alloy powders were sintered using the pulse electric current sintering (PECS) process at various temperatures. The microstructure at the interfaces between powder particles and the effect of sintering temperature on interface characteristics were investigated using transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS). The precipitates were observed at the interfaces between powder particles of the compacts. The amounts of the precipitates increased and the compositions changed with an increase in sintering temperature: MgO for the compact sintered at 613 K, MgAl2O4+MgO for those at 663 K and 713 K, and MgAl2O4 for those above 763 K. Comparing the results obtained by the PECS process with those of diffusion bonding experiments and thermodynamic calculation, it was suggested that the temperature at the interfaces between the particles was higher than that of the particles sintered by the PECS process.

Sintering Theory and Practice

NASA Astrophysics Data System (ADS)

German, Randall M.

1996-01-01

Although sintering is an essential process in the manufacture of ceramics and certain metals, as well as several other industrial operations, until now, no single book has treated both the background theory and the practical application of this complex and often delicate procedure. In Sintering Theory and Practice, leading researcher and materials engineer Randall M. German presents a comprehensive treatment of this subject that will be of great use to manufacturers and scientists alike. This practical guide to sintering considers the fact that while the bonding process improves strength and other engineering properties of the compacted material, inappropriate methods of control may lead to cracking, distortion, and other defects. It provides a working knowledge of sintering, and shows how to avoid problems while accounting for variables such as particle size, maximum temperature, time at that temperature, and other problems that may cause changes in processing. The book describes the fundamental atomic events that govern the transformation from particles to solid, covers all forms of the sintering process, and provides a summary of many actual production cycles. Building from the ground up, it begins with definitions and progresses to measurement techniques, easing the transition, especially for students, into advanced topics such as single-phase solid-state sintering, microstructure changes, the complications of mixed particles, and pressure-assisted sintering. German draws on some six thousand references to provide a coherent and lucid treatment of the subject, making scientific principles and practical applications accessible to both students and professionals. In the process, he also points out and avoids the pitfalls found in various competing theories, concepts, and mathematical disputes within the field. A unique opportunity to discover what sintering is all about--both in theory and in practice What is sintering? We see the end product of this thermal 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.

The thermal stability of hydroxyapatite in biphasic calcium phosphate ceramics.

PubMed

Nilen, R W N; Richter, P W

2008-04-01

Biphasic calcium phosphate ceramics (BCP) comprising a mix of non-resorbable hydroxyapatite (HA) and resorbable beta-tricalcium phosphate (beta-TCP) are particularly suitable materials for synthetic bone substitute applications. In this study, HA synthesised by solid state reaction was mechanically mixed with beta-TCP, then sintered to form a suite of BCP materials with a wide range of HA/beta-TCP phase content ratios. The influence of sintering temperature and composition on the HA thermal stability was quantified by X-ray diffraction (XRD). The pre-sinter beta-TCP content was found to strongly affect the post-sinter HA/beta-TCP ratio by promoting the thermal decomposition of HA to beta-TCP, even at sintering temperatures as low as 850 degrees C. For BCP material with pre-sinter HA/beta-TCP = 40/60 wt%, approximately 80% of the HA decomposed to beta-TCP during sintering at 1000 degrees C. Furthermore, the HA content appeared to influence the reverse transformation of alpha-TCP to beta-TCP expected upon gradual cooling from sintering temperatures greater than 1125 degrees C. Because the HA/beta-TCP ratio dominantly determines the rate and extent of BCP resorption in vivo, the possible thermal decomposition of HA during BCP synthesis must be considered, particularly if high temperature treatments are involved.

Low-Temperature Oxidation-Free Selective Laser Sintering of Cu Nanoparticle Paste on a Polymer Substrate for the Flexible Touch Panel Applications.

PubMed

Kwon, Jinhyeong; Cho, Hyunmin; Eom, Hyeonjin; Lee, Habeom; Suh, Young Duk; Moon, Hyunjin; Shin, Jaeho; Hong, Sukjoon; Ko, Seung Hwan

2016-05-11

Copper nanomaterials suffer from severe oxidation problem despite the huge cost effectiveness. The effect of two different processes for conventional tube furnace heating and selective laser sintering on copper nanoparticle paste is compared in the aspects of chemical, electrical and surface morphology. The thermal behavior of the copper thin films by furnace and laser is compared by SEM, XRD, FT-IR, and XPS analysis. The selective laser sintering process ensures low annealing temperature, fast processing speed with remarkable oxidation suppression even in air environment while conventional tube furnace heating experiences moderate oxidation even in Ar environment. Moreover, the laser-sintered copper nanoparticle thin film shows good electrical property and reduced oxidation than conventional thermal heating process. Consequently, the proposed selective laser sintering process can be compatible with plastic substrate for copper based flexible electronics applications.

Porous single-phase NiTi processed under Ca reducing vapor for use as a bone graft substitute.

PubMed

Bertheville, Bernard

2006-03-01

Porous nickel-titanium alloys (NiTi, nitinol) have recently attracted attention in clinical surgery because they are a very interesting alternative to the more brittle and less machinable conventional porous Ca-based ceramics. The main remaining limitations come from the chemical homogeneity of the as-processed porous nickel-titanium alloys, which always contain undesired secondary Ti- and Ni-rich phases. These are known to weaken the NiTi products, to favor their cavitation corrosion and to decrease their biocompatibility. Elemental nickel must also be avoided because it could give rise to several adverse tissue reactions. Therefore, the synthesis of porous single-phase NiTi alloys by using a basic single-step sintering procedure is an important step towards the processing of safe implant materials. The sintering process used in this work is based on a vapor phase calciothermic reduction operating during the NiTi compound formation. The as-processed porous nickel-titanium microstructure is single-phase and shows a uniformly open pore distribution with porosity of about 53% and pore diameters in the range 20-100 microm. Furthermore, due to the process, fine CaO layers grow on the NiTi outer and inner surfaces, acting as possible promoting agents for the ingrowth of bone cells at the implantation site.

Flash (Ultra-Rapid) Spark-Plasma Sintering of Silicon Carbide

PubMed Central

Olevsky, Eugene A.; Rolfing, Stephen M.; Maximenko, Andrey L.

2016-01-01

A new ultra-rapid process of flash spark plasma sintering is developed. The idea of flash spark plasma sintering (or flash hot pressing - FHP) stems from the conducted theoretical analysis of the role of thermal runaway phenomena for material processing by flash sintering. The major purpose of the present study is to theoretically analyze the thermal runaway nature of flash sintering and to experimentally address the challenge of uncontrollable thermal conditions by the stabilization of the flash sintering process through the application of the external pressure. The effectiveness of the developed FHP technique is demonstrated by the few seconds–long consolidation of SiC powder in an industrial spark plasma sintering device. Specially designed sacrificial dies heat the pre-compacted SiC powder specimens to a critical temperature before applying any voltage to the powder volume and allowing the electrode-punches of the SPS device setup to contact the specimens and pass electric current through them under elevated temperatures. The experimental results demonstrate that flash sintering phenomena can be realized using conventional SPS devices. The usage of hybrid heating SPS devices is pointed out as the mainstream direction for the future studies and utilization of the new flash hot pressing (ultra-rapid spark plasma sintering) technique. PMID:27624641

Flash (Ultra-Rapid) Spark-Plasma Sintering of Silicon Carbide

DOE PAGES

Olevsky, Eugene A.; Rolfing, Stephen M.; Maximenko, Andrey L.

2016-09-14

A new ultra-rapid process of flash spark plasma sintering is developed. The idea of flash spark plasma sintering (or flash hot pressing - FHP) stems from the conducted theoretical analysis of the role of thermal runaway phenomena for material processing by flash sintering. The major purpose of the present study is to theoretically analyze the thermal runaway nature of flash sintering and to experimentally address the challenge of uncontrollable thermal conditions by the stabilization of the flash sintering process through the application of the external pressure. The effectiveness of the developed FHP technique is demonstrated by the few seconds–long consolidationmore » of SiC powder in an industrial spark plasma sintering device. Specially designed sacrificial dies heat the pre-compacted SiC powder specimens to a critical temperature before applying any voltage to the powder volume and allowing the electrode-punches of the SPS device setup to contact the specimens and pass electric current through them under elevated temperatures. The experimental results demonstrate that flash sintering phenomena can be realized using conventional SPS devices. The usage of hybrid heating SPS devices is pointed out as the mainstream direction for the future studies and utilization of the new flash hot pressing (ultra-rapid spark plasma sintering) technique.« less

Superconductivity in BiPbCaSrCuO thin films

NASA Astrophysics Data System (ADS)

Fu, S. M.; Yang, H. C.; Chen, F. C.; Horng, H. E.; Jao, J. C.

1989-12-01

Thin films of BiPbCaSrCuO sample were prepared by RF sputtering from sintered ceramic targets. Single crystal of MgO(100) was selected as substrate. The sputtering was held at room temperature. Different annealing conditions were carried out to obtain optimum conditions. High temperature resistivity was measured in air to study the thermodynamic reaction of the sintered films. An resistivity anomaly was found in the first heating cycle which suggests a thermodynamic reaction. A temperature dependence of I c was measured to study the coupling of grains in the granular films in different temperature ranges and the results will be discussed.

Synthesisofc-lifepo4 composite by solid state reaction method

NASA Astrophysics Data System (ADS)

Rahayu, I.; Hidayat, S.; Noviyanti, A. R.; Rakhmawaty, D.; Ernawati, E.

2017-02-01

In this research, the enhancement of LiFePO4 conductivity was conducted by doping method with carbon materials. Carbon-based materials were obtained from the mixture of sucrose, and the precursor of LiH2PO4 and α-Fe2O3 was synthesized by solid state reaction. Sintering temperature was varied at 700°C, 800°C, 900°C and 1,000°C. The result showed that C-LiFePO4 could be synthesized by using solid state reaction method. Based on the XRD and FTIR spectrums, C-LiFePO4 can be identified as the type of crystal, characterized by the appearance of sharp signal on (011), (211) and typical peak of LiFePO4 materials. The result of conductivity measurement from C-LiFePO4 at sintering temperature of 900°C and 1,000°C was 2×10-4 S/cm and 4×10-4S/cm, respectively. The conductivity value at sintering temperature of 700°C and 800°C was very small (<10-6 S/cm), which cannot be measured by the existing equipment.

Improved Properties of Pb Based BLZT Ferroelectric Ceramics

NASA Astrophysics Data System (ADS)

Kumar, Parveen; Singh, Sangeeta; Juneja, J. K.; Raina, K. K.; Prakash, Chandra

2011-11-01

Present report is concerning with investigation of effect of different sintering profiles on Pb based BLZT ceramics. The material powder of selected composition (Ba0.795La0.005Pb0.20Ti0.90Zr0.10O3) was prepared by solid state reaction route and then powder was compacted in the form of circular discs. The discs were then sintered at different temperatures (1325 °C for 4h, 1325 °C for 15min+1200 °C for 4h). Improved dielectric and ferroelectric properties were observed for samples sintered at 1200 °C. Shifting in Tc to higher temperature could be related to enhanced tetragonality, which was further confirmed by X-ray diffraction analysis. All these improvements evidences that there is less Pb loss in case of modified sintering profile.

Mechanical and microstructural characterization of W–Cu FGM fabricated by one-step sintering method through PM route

NASA Astrophysics Data System (ADS)

Gupta, Rajat; Kumar, Rohit; Chaubey, A. K.; Kanpara, Shailesh; Khirwadkar, S. S.

2018-03-01

Five layer W-Cu functionally graded material (FGM) for components in nuclear fusion application was fabricated by a one-step resistance sintering process, known as spark plasma sintering (SPS). In this study effect of sintering temperature (Ts) on physical, mechanical and surface property was investigated. Detailed microstructural study revealed that the graded structure of the composite layers with varying composition from 0 to 100 wt% W and Cu in opposite directions could be well densified after the SPS process. It also indicates that the fine microstructure within functionally graded layers can be maintained because of short sintering time. The sample sintered at 1050°C shows more than 90% theoretical density, hardness greater than 239±5 Hv and excellent surface scratch resistance. The result demonstrates that SPS is promising and more suitable process for fabrication of W-Cu FGM.

Two-Step Reactive Aid Sintering of BaZr0.8Y0.2O3- δ Proton-Conducting Ceramics

NASA Astrophysics Data System (ADS)

Wang, Siwei; Chen, Yan; Zhang, Lingling; Ren, Cong; Chen, Fanglin; Brinkman, Kyle S.

2015-12-01

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr0.8Y0.2O3- δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. In this paper, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO3 and B2O3-Li2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improved to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. The bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.

Two-Step Reactive Aid Sintering of BaZr 0.8Y 0.2O 3-δ Proton-Conducting Ceramics

DOE PAGES

Wang, Siwei; Chen, Yan; Zhang, Lingling; ...

2015-10-14

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. Here, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improvedmore » to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. Moreover, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less

Effect of temperature on porosity of iron ore sinter with biochar derived from EFB

NASA Astrophysics Data System (ADS)

Purwanto, H.; Rozhan, A. N.; Zakiyuddin, A.; Mohamad, A. S.

2018-01-01

In this research, the replacement of fossil fuel energy (coke) with oil palm empty fruit bunch as a potential energy in sintering of iron ore was investigated. Carbon derived biomass has been produced by using oil palm empty fruit bunch by heat treatment process. In the present investigation, sintering process was carried out by heating the mixed iron ore and biochar at various temperatures. The apparent density and porosity for iron sinter show a significant increase and gradual decrement as the temperature increase, respectively. The porosity of iron sinter shows a gradual decrement from 950 °C to 1050 °C but up to 1150 °C it shows a significant decrement about 44%. Inferring to the micrograph, the agglomeration and assimilation of sinter at high temperature is better compared with low sintering temperature.

Reflow-oven-processing of pressureless sintered-silver interconnects

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wereszczak, Andrew A.; Chen, Branndon R.; Oistad, Brian A.

Here, a method was developed to pressurelessly fabricate strong and consistent sinterable-silver joints or interconnects using reflow oven heating. Circular sinterable-silver interconnects, having nominal diameter of 5 mm and 0.1 mm thickness were stencil printed, contact-dried, and then pressurelessly sinter-bonded to Au-plated direct copper bonded ceramic substrates at 250 °C in ambient air. That sintering was done in either a reflow oven or a convective oven (latter being a conventional heating source for processing sinterable-silver). Consistently strong (>40 MPa) interconnects were produced with reflow oven heating and were as strong as those produced with convective oven heating. This is significantmore » because reflow oven technology affords better potential for continuous mass production and it was shown that strong sintered-silver bonds can indeed be achieved with its use.« less

Reflow-oven-processing of pressureless sintered-silver interconnects

DOE PAGES

Wereszczak, Andrew A.; Chen, Branndon R.; Oistad, Brian A.

2018-01-04

Here, a method was developed to pressurelessly fabricate strong and consistent sinterable-silver joints or interconnects using reflow oven heating. Circular sinterable-silver interconnects, having nominal diameter of 5 mm and 0.1 mm thickness were stencil printed, contact-dried, and then pressurelessly sinter-bonded to Au-plated direct copper bonded ceramic substrates at 250 °C in ambient air. That sintering was done in either a reflow oven or a convective oven (latter being a conventional heating source for processing sinterable-silver). Consistently strong (>40 MPa) interconnects were produced with reflow oven heating and were as strong as those produced with convective oven heating. This is significantmore » because reflow oven technology affords better potential for continuous mass production and it was shown that strong sintered-silver bonds can indeed be achieved with its use.« less

Flash microwave synthesis and sintering of nanosized La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}o{sub 3-{delta}} for fuel cell application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Combemale, L., E-mail: lionel.combemale@u-bourgogne.f; Caboche, G.; Stuerga, D.

2009-10-15

Perovskite-oxide nanocrystals of La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}O{sub 3-{delta}} with a mean size around 10 nm were prepared by microwave flash synthesis. This reaction was performed in alcoholic solution using metallic salts, sodium ethoxide and microwave autoclave. The obtained powder was characterised after purification by energy dispersive X-ray analysis (EDX), X-ray powder diffraction (XRD), BET adsorption technique, photon correlation spectroscopy (PCS) and transmission electron microscopy (TEM). The results show that integrated perovskite-type phase and uniform particle size were obtained in the microwave treated samples. At last the synthesised powder was directly used in a sintering process. A porous solid, inmore » accordance with the expected applications, was then obtained at low sintering temperature (1000 deg. C) without use of pore forming agent. - Graphical abstract: TEM photograph of La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}O{sub 3-{delta}} obtained by microwave flash synthesis. This picture confirms the nanometric size of the ceramic particles.« less

Rapid synthesis of barium titanate microcubes using composite-hydroxides-mediated avenue

DOE Office of Scientific and Technical Information (OSTI.GOV)

He, Xi; Ouyang, Jing, E-mail: jingouyang@csu.edu.cn; Jin, Jiao

2014-04-01

Highlights: • Barium titanate oxides microcubes can be synthesized within 1 min. • Composite-hydroxides-mediated strategy provided a possible large scale production. • BST obtained in the strategy showed fairly good crystallinity and tetragonality. - Abstract: This paper reports the rapid synthesis of barium titanate (BaTiO{sub 3}, BTO) microcubes via composite-hydroxides-mediated reaction within 1 min. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion spectrum (EDS) results confirmed both cubic and tetragonal lattices in the sample and the uniform microcubes with an average size of 1 μm. Ultraviolet–visible (UV–vis) spectrum indicated that the band gap of the BTO powder wasmore » 3.05 eV. Ferroelectric polarization vs. electric field (P–E) tests showed that the ferroelectric domains had formed in the as-synthesized BTO microcubes and sintered ceramics. BTO ceramics sintered at 1100 °C for 3 h showed fairly good tetragonality and possessed a maximum polarization of 0.21 μC/cm{sup 2}, indicating that the sintering temperature for the BTO powders prepared via this method was relatively low. The process and equipment reported herein provided a potential method for the rapid synthesis of titanate based perovskites.« less

Semiconductor structural damage attendant to contact formation in III-V solar cells

NASA Technical Reports Server (NTRS)

Fatemi, Navid S.; Weizer, Victor G.

1991-01-01

In order to keep the resistive losses in solar cells to a minimum, it is often necessary for the ohmic contacts to be heat treated to lower the metal-semiconductor contact resistivity to acceptable values. Sintering of the contacts, however can result in extensive mechanical damage of the semiconductor surface under the metallization. An investigation of the detailed mechanisms involved in the process of contact formation during heat treatment may control the structural damage incurred by the semiconductor surface to acceptable levels, while achieving the desired values of contact resistivity for the ohmic contacts. The reaction kinetics of sintered gold contacts to InP were determined. It was found that the Au-InP interaction involves three consecutive stages marked by distinct color changes observed on the surface of the Au, and that each stage is governed by a different mechanism. A detailed description of these mechanisms and options to control them are presented.

Densification behavior, nanocrystallization, and mechanical properties of spark plasma sintered Fe-based bulk amorphous alloys

NASA Astrophysics Data System (ADS)

Singh, Ashish Kumar

Fe-based amorphous alloys are gaining increasing attention due to their exceptional wear and corrosion resistance for potential structural applications. Two major challenges that are hindering the commercialization of these amorphous alloys are difficulty in processing of bulk shapes (diameter > 10 mm) and lack of ductility. Spark plasma sintering (SPS) is evolving as a promising technique for processing bulk shapes of amorphous and nanocrystalline materials. The objective of this work is to investigate densification behavior, nanocrystallization, and mechanical properties of SPS sintered Fe-based amorphous alloys of composition Fe48Cr15Mo14Y2C15B6. SPS processing was performed in three distinct temperature ranges of amorphous alloys: (a) below glass transition temperature (Tg), (b) between Tg and crystallization temperature (Tx), and (c) above Tx. Punch displacement data obtained during SPS sintering was correlated with the SPS processing parameters such as temperature, pressure, and sintering time. Powder rearrangement, plastic deformation below T g, and viscous flow of the material between Tg and Tx were observed as the main densification stages during SPS sintering. Micro-scale temperature distributions at the point of contact and macro-scale temperature distribution throughout the sample during SPS of amorphous alloys were modeled. The bulk amorphous alloys are expected to undergo structural relaxation and nanocrystallization during SPS sintering. X-ray diffraction (XRD), small angle neutron scattering (SANS), and transmission electron microscopy (TEM) was performed to investigate the evolution of nanocrystallites in SPS sintered Fe-based bulk amorphous alloys. The SANS analysis showed significant scattering for the samples sintered in the supercooled region indicating local structural and compositional changes with the profuse nucleation of nano-clusters (~4 nm). Compression tests and microhardness were performed on the samples sintered at different temperatures ranging from 570 °C to 800 °C. Maximum compression strength (1.1+/-0.2 MPa) was obtained for the samples sintered in the supercooled region. Effects of crystallization on tribological behavior of sintered samples were also investigated where crystallization resulted in increase in wear resistance. Laser surface hardening of SPS sintered amorphous samples were performed. Depending on the processing parameters, the laser surface irradiation causes structural relaxation and nanocrystallization, resulting in surface hardening.

Development of a sintering process for recycling oil shale fly ash and municipal solid waste incineration bottom ash into glass ceramic composite.

PubMed

Zhang, Zhikun; Zhang, Lei; Li, Aimin

2015-04-01

Oil shale fly ash and municipal solid waste incineration bottom ash are industrial and municipal by-products that require further treatment before disposal to avoid polluting the environment. In the study, they were mixed and vitrified into the slag by the melt-quench process. The obtained vitrified slag was then mixed with various percentages of oil shale fly ash and converted into glass ceramic composites by the subsequent sintering process. Differential thermal analysis was used to study the thermal characteristics and determine the sintering temperatures. X-ray diffraction analysis was used to analyze the crystalline phase compositions. Sintering shrinkage, weight loss on ignition, density and compressive strength were tested to determine the optimum preparation condition and study the co-sintering mechanism of vitrified amorphous slag and oil shale fly ash. The results showed the product performances increased with the increase of sintering temperatures and the proportion of vitrified slag to oil shale fly ash. Glass ceramic composite (vitrified slag content of 80%, oil shale fly ash content of 20%, sintering temperature of 1000 °C and sintering time of 2h) showed the properties of density of 1.92 ± 0.05 g/cm(3), weight loss on ignition of 6.14 ± 0.18%, sintering shrinkage of 22.06 ± 0.6% and compressive strength of 67 ± 14 MPa. The results indicated that it was a comparable waste-based material compared to previous researches. In particular, the energy consumption in the production process was reduced compared to conventional vitrification and sintering method. Chemical resistance and heavy metals leaching results of glass ceramic composites further confirmed the possibility of its engineering applications. Copyright © 2015 Elsevier Ltd. All rights reserved.

Stress-dislocation interaction mechanism in low-temperature thermo-compression sintering of Ag NPs

NASA Astrophysics Data System (ADS)

Wang, Fuliang; Tang, Zikai; He, Hu

2018-04-01

The sintering of metal nanoparticles (NPs) has been widely studied in the field of nanotechnology, and low-temperature sintering has become the industry standard. In this study, a molecular dynamics (MD) model was established to study the sintering behaviour of silver NPs during low-temperature thermo-compression. Primarily, we studied the sintering process, in which the ratio of neck radius to particle radius (x/r) changes. Under a uniaxial pressure, the maximum ratio in the temperature range 420-425 K was 1. According to the change of x/r, the process can be broken down into three stages: the neck-formation stage, neck-growth stage, and neck-stability stage. In addition, the relationship between potential energy, internal stress, and dislocation density during sintering is discussed. The results showed that cycling internal stress played an important role in sintering. Under the uniaxial pressure, the stress-dislocation interaction was found to be the major mechanism for thermo-compression sintering because the plastic deformation product dislocation intensified the diffusion of atoms. Also, the displacement vector, the mean square displacement, and the changing crystal structure during sintering were studied.

Phenomenological analysis of densification mechanism during spark plasma sintering of MgAl2O4

NASA Astrophysics Data System (ADS)

Bernard-Granger, Guillaume; Benameur, Nassira; Addad, Ahmed; Nygren, Mats; Guizard, Christian; Deville, Sylvain

2009-05-01

Spark plasma sintering (SPS) of MgAl2O4 powder was investigated at temperatures between 1200 and 1300{\\deg}C. A significant grain growth was observed during densification. The densification rate always exhibits at least one strong minimum, and resumes after an incubation period. Transmission electron microscopy investigations performed on sintered samples never revealed extensive dislocation activity in the elemental grains. The densification mechanism involved during SPS was determined by anisothermal (investigation of the heating stage of a SPS run) and isothermal methods (investigation at given soak temperatures). Grain-boundary sliding, accommodated by an in-series {interface-reaction/lattice diffusion of the O$^2$-anions} mechanism controlled by the interface-reaction step, governs densification. The zero-densification-rate period, detected for all soak temperatures, arise from the difficulty of annealing vacancies, necessary for the densification to proceed. The detection of atomic ledges at grain boundaries and the modification of the stoichiometry of spinel during SPS could be related to the difficulty to anneal vacancies at temperature soaks.

Effect of surface oxide films on the properties of pulse electric-current sintered metal powders

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Yamaguchi, Norio; Wang, Airu

2003-11-01

Metallic powders with various thermodynamic stability oxide films (Ag, Cu, and Al powders) were sintered using a pulse electric-current sintering (PECS) process. Behavior of oxide films at powder surfaces and their effect on the sintering properties were investigated. The results showed that the sintering properties of metallic powders in the PECS process were subject to the thermodynamic stability of oxide films at particles surfaces. The oxide films at Ag powder surfaces are decomposed during sintering with the contact region between the particles being metal/metal bond. The oxide films at Cu powder surfaces are mainly broken via loading pressure at a low sintering temperature. At a high sintering temperature, they are mainly dissolved in the parent metal, and the contact regions turn into the direct metal/metal bonding. Excellent sintering properties can be received. The oxide films at Al powder surfaces are very stable, and cannot be decomposed and dissolved, but broken by plastic deformation of particles under loading pressure at experimental temperatures. The interface between particles is partially bonded via the direct metal/metal bonding making it difficult to achieve good sintered properties.

Enhanced thermal conductivity of uranium dioxide-silicon carbide composite fuel pellets prepared by Spark Plasma Sintering (SPS)

NASA Astrophysics Data System (ADS)

Yeo, S.; Mckenna, E.; Baney, R.; Subhash, G.; Tulenko, J.

2013-02-01

Uranium dioxide (UO2)-10 vol% silicon carbide (SiC) composite fuel pellets were produced by oxidative sintering and Spark Plasma Sintering (SPS) at a range of temperatures from 1400 to 1600 °C. Both SiC whiskers and SiC powder particles were utilized. Oxidative sintering was employed over 4 h and the SPS sintering was employed only for 5 min at the highest hold temperature. It was noted that composite pellets sintered by SPS process revealed smaller grain size, reduced formation of chemical products, higher density, and enhanced interfacial contact compared to the pellets made by oxidative sintering. For given volume of SiC, the pellets with powder particles yielded a smaller grain size than pellets with SiC whiskers. Finally thermal conductivity measurements at 100 °C, 500 °C, and 900 °C revealed that SPS sintered UO2-SiC composites exhibited an increase of up to 62% in thermal conductivity compared to UO2 pellets, while the oxidative sintered composite pellets revealed significantly inferior thermal conductivity values. The current study points to the improved processing capabilities of SPS compared to oxidative sintering of UO2-SiC composites.

Borax as flux on sintering of iron Ancor Steel 1000® under glow discharge

NASA Astrophysics Data System (ADS)

Ariza Suarez, H. G.; Sarmiento Santos, A.; Ortiz Otálora, C. A.

2016-02-01

This work studies the flux effect of borax (di sodium tetraborate decahydrate) on sintering of iron Ancor Steel 1000® in abnormal glow discharge. The incidence of the percentage by weight of borax and the sintering temperature in the process were observed. Samples of powder metallurgical iron were prepared with proportions of 0.50%, 2.0%, 4.0% and 6.0% by weight of borax using the procedures of powder metallurgy. The samples were sintered at 800 and 1100°C for 30min, by glow discharge at low pressure in a reducing atmosphere composed of 20% H2+80% Ar. The samples in compact green-state were analyzed by TGA-DSC to determine the fusion process and mass loss during sintering. The analysis of microhardness and density, shows that at a sintering temperature of 800°C the sample density decreases and the sample microhardness increases with respect to sintered samples without borax. Sintered samples were analysed by DRX showing the absence of precipitates.

[Application of sintered Ti powder to dental prostheses].

PubMed

Hikosaka, Tatsuya; Tanaka, Yoshinobu; Hoshiai, Kazumoto; Kanazawa, Takeshi; Nakamura, Yoshinori; Tsuda, Kenji; Ohasi, Hideya

2005-04-01

Powder metallurgy is a metal processing technology. Porous titanium produced from powder is widely used. The method is applied to titanium, which is not easy to cast as it sinters under melting point. In prosthetic dentistry, powder metallurgy can be applied to high fusing metal that is biocompatible. In this study, we examined the mechanical characteristics of the Ti sheet produced by sintering and discussed its application to dental prosthesis manufacturing. Ti sheets of 1-mm thickness, in which a binder was added to spherical Ti powder, were produced with the Doctor Blade Method. The sintering was carried out between 900-1150 degrees C at 6 temperatures. The sintered compact was evaluated by dimensional change rate, hardness test, bending strength, tensile strength and SEM observation. Another compact was sintered on the refractory cast. Mechanical strength significantly increased with sintering temperature. In addition, excellent mechanical strength was acquired by adding crushed powder and performing the de-binder process. In the sintering on the refractory cast, pre-baking for more than 100 minutes and sintering at over 1050 degrees C was needed for practical application. It thus seems possible to apply sintered titanium to dental prostheses. However, it will be necessary to examine the control of the shrinkage of the sintered compact in the future too.

Experimental Study on Reaction Characteristics of PTFE/Ti/W Energetic Materials under Explosive Loading

PubMed Central

Li, Yan; Jiang, Chunlan; Wang, Zaicheng; Luo, Puguang

2016-01-01

Metal/fluoropolymer composites represent a new category of energetic structural materials that release energy through exothermic chemical reactions initiated under shock loading conditions. This paper describes an experiment designed to study the reaction characteristics of energetic materials with low porosity under explosive loading. Three PTFE (polytetrafluoroethylene)/Ti/W mixtures with different W contents are processed through pressing and sintering. An inert PTFE/W mixture without reactive Ti particles is also prepared to serve as a reference. Shock-induced chemical reactions are recorded by high-speed video through a narrow observation window. Related shock parameters are calculated based on experimental data, and differences in energy release are discussed. The results show that the reaction propagation of PTFE/Ti/W energetic materials with low porosity under explosive loading is not self-sustained. As propagation distance increases, the energy release gradually decreases. In addition, reaction failure distance in PTFE/Ti/W composites is inversely proportional to the W content. Porosity increased the failure distance due to higher shock temperature. PMID:28774056

Accelerated sintering in phase-separating nanostructured alloys

PubMed Central

Park, Mansoo; Schuh, Christopher A.

2015-01-01

Sintering of powders is a common means of producing bulk materials when melt casting is impossible or does not achieve a desired microstructure, and has long been pursued for nanocrystalline materials in particular. Acceleration of sintering is desirable to lower processing temperatures and times, and thus to limit undesirable microstructure evolution. Here we show that markedly enhanced sintering is possible in some nanocrystalline alloys. In a nanostructured W–Cr alloy, sintering sets on at a very low temperature that is commensurate with phase separation to form a Cr-rich phase with a nanoscale arrangement that supports rapid diffusional transport. The method permits bulk full density specimens with nanoscale grains, produced during a sintering cycle involving no applied stress. We further show that such accelerated sintering can be evoked by design in other nanocrystalline alloys, opening the door to a variety of nanostructured bulk materials processed in arbitrary shapes from powder inputs. PMID:25901420

Understanding proton-conducting perovskite interfaces using atom probe tomography

NASA Astrophysics Data System (ADS)

Clark, Daniel R.

Proton-conducting ceramics are under intense scientific investigation for a number of exciting applications, including fuel cells, electrolyzers, hydrogen separation membranes, membrane reactors, and sensors. However, commercial application requires deeper understanding and improvement of proton conductivity in these materials. It is well-known that proton conductivity in these materials is often limited by highly resistive grain boundaries (GBs). While these conductivity-limiting GBs are still not well understood, it is hypothesized that their blocking nature stems from the formation of a positive (proton-repelling) space-charge zone. Furthermore, it has been observed that the strength of the blocking behavior can change dramatically depending on the fabrication process used to make the ceramic. This thesis applies laser-assisted atom probe tomography (LAAPT) to provide new insights into the GB chemistry and resulting space-charge behavior of BaZr0.9Y0.1O 3--delta (BZY10), a prototypical proton-conducting ceramic. LAAPT is an exciting characterization technique that allows for three-dimensional nm-scale spatial resolution and very high chemical resolution (up to parts-per-million). While it is challenging to quantitatively apply LAAPT to complex, multi-cation oxide materials, this thesis successfully develops a method to accurately quantify the stoichiometry of BZY10 and maintain minimal quantitative cationic deviation at a laser energies of approximately 10--20 pJ. With the analysis technique specifically optimized for BZY10, GB chemistry is then examined for BZY10 samples prepared using four differing processing methods: (1) spark plasma sintering (SPS), (2) conventional sintering using powder prepared by solid-state reaction followed by high-temperature annealing (HT), (3) conventional sintering using powder prepared by solid-state reaction with NiO used as a sintering aid (SSR-Ni), and (4) solid-state reactive sintering directly from BaCO3, ZrO2, and Y2O3 precursor powders with 1 wt. % NiO as a reactive sintering aid (SSRS-Ni). It is observed that oxygen depletion (oxygen-vacancy accumulation) occurs at all GBs. Segregation of the constituent cations, Ba, Zr, and Y, is found to be variable across all samples although zirconium depletion and yttrium accumulation are most prevalent. Additionally, impurities such as Al, Fe, Mg, Ni, Si, and Sr are shown to generally accumulate at the GBs. Finally, LAAPT-derived GB chemistry data is combined with electrostatic modeling to examine the electronic structure of a BZY10 GB, revealing significant non-uniformity in the space charge region at the GB with an average space-charge potential of approximately 580 mV, extending 5--7 nm in width from the GB core. This result demonstrates how LAAPT can not only be used to further understand the role of GB chemistry within oxide materials, but can also be used to examine the electronic structure, allowing for the possibility of engineering these interfaces to improve their electrochemical performance.

Electrochemical oxidation of hydrolyzed poly oxymethylene-dimethyl ether by PtRu catalysts on Nb-doped SnO(2-δ) supports for direct oxidation fuel cells.

PubMed

Kakinuma, Katsuyoshi; Kim, In-Tae; Senoo, Yuichi; Yano, Hiroshi; Watanabe, Masahiro; Uchida, Makoto

2014-12-24

We synthesized Pt and PtRu catalysts supported on Nb-doped SnO(2-δ) (Pt/Sn0.99Nb0.01O(2-δ), PtRu/Sn0.99Nb0.01O(2-δ)) for direct oxidation fuel cells (DOFCs) using poly oxymethylene-dimethyl ether (POMMn, n = 2, 3) as a fuel. The onset potential for the oxidation of simulated fuels of POMMn (methanol-formaldehyde mixtures; n = 2, 3) for Pt/Sn0.99Nb0.01O(2-δ) and PtRu/Sn0.99Nb0.01O(2-δ) was less than 0.3 V vs RHE, which was much lower than those of two commercial catalysts (PtRu black and Pt2Ru3/carbon black). In particular, the onset potential of the oxidation reaction of simulated fuels of POMMn (n = 2, 3) for PtRu/Sn0.99Nb0.01O(2-δ) sintered at 800 °C in nitrogen atmosphere was less than 0.1 V vs RHE and is thus considered to be a promising anode catalyst for DOFCs. The mass activity (MA) of PtRu/Sn0.99Nb0.01O(2-δ) sintered at 800 °C was more than five times larger than those of the commercial catalysts in the measurement temperature range from 25 to 80 °C. Even though the MA for the methanol oxidation reaction was of the same order as those of the commercial catalysts, the MA for the formaldehyde oxidation reaction was more than five times larger than those of the commercial catalysts. Sn from the Sn0.99Nb0.01O(2-δ) support was found to have diffused into the Pt catalyst during the sintering process. The Sn on the top surface of the Pt catalyst accelerated the oxidation of carbon monoxide by a bifunctional mechanism, similar to that for Pt-Ru catalysts.

Ice sintering timescales at the surface of Europa and implications for surface properties

NASA Astrophysics Data System (ADS)

Phillips, C. B.; Molaro, J.; Meirion-Griffith, G.

2017-12-01

The planned exploration of Europa by NASA's Europa Clipper Mission and the possibility of a future Europa lander have driven the need to characterize its surface strength, roughness, porosity, thermal conductivity, and regolith depth in order to accurately interpret remote sensing data and develop appropriate spacecraft landing systems. Many processes contribute to Europa's landscape evolution, such as sputtering, mass wasting, thermal segregation, and impact gardening, driving the creation and distribution of icy regolith across the surface. While the efficacy of these processes are not well constrained, any amount of regolith emplaced at the surface will undergo subsequent processing due to sintering. Ice sintering is a form of frost metamorphism whereby contacting ice grains experience the diffusion of material into their contact region, forming a "neck" between them and densifying over time. Over long enough timescales, ice aggregates will sinter into solid material, which may contribute to the incorporation of non-ice material into Europa's subsurface and help to drive subsurface chemistry. Sintering also interacts with other processes, adding to the complexity of icy surface evolution. For example, sputtering preferentially removes larger grains and may enhance sintering rates, and changes in ice porosity may affect the response of the surface to micrometeorite impacts. Quantifying the effects of ice sintering will allow us to predict the microstructural properties of Europa's surface at spacecraft scales. To this end, we have modeled pressure-less (no overburden) sintering of spherical water-ice grains and validated the results with a laboratory experiment. We also modeled ice at the surface of Europa to obtain a first-order approximation of the sintering timescale and surface properties. Preliminary results indicate that ice grains will experience neck growth but not significant densification over Europa's surface age, suggesting that loose surface ice forms a weak and porous crust. Furthermore, our results suggest that existing models do not accurately quantify all stages of the sintering process for ice, emphasizing the need for more laboratory studies on this topic.

Sintering, thermal stability and mechanical properties of ZrO2-WC composites obtained by pulsed electric current sintering

NASA Astrophysics Data System (ADS)

Huang, Shuigen; Vanmeensel, Kim; van der Biest, Omer; Vleugels, Jozef

2011-03-01

ZrO2-WC composites exhibit comparable mechanical properties as traditional WC-Co materials, which provides an opportunity to partially replace WC-Co for some applications. In this study, 2 mol.% Y2O3 stabilized ZrO2 composites with 40 vol.% WC were consolidated in the 1150°C-1850°C range under a pressure of 60 MPa by pulsed electric current sintering (PECS). The densification behavior, microstructure and phase constitution of the composites were investigated to clarify the role of the sintering temperature on the grain growth, mechanical properties and thermal stability of ZrO2 and WC components. Analysis results indicated that the composites sintered at 1350°C and 1450°C exhibited the highest tetragonal ZrO2 phase transformability, maximum toughness, and hardness and an optimal flexural strength. Chemical reaction of ZrO2 and C, originating from the graphite die, was detected in the composite PECS for 20 min at 1850°C in vacuum.

Effect of various sintering temperature on resistivity behaviour and magnetoresistance of La{sub 0.67}Ba{sub 0.33}MnO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pratama, R.; Kurniawan, B., E-mail: bkuru07@gmail.com; Manaf, A.

2016-04-19

A detail work was conducted in order to investigate effect of various sintering temperature on resistivity behavior and its relation with the magneto-resistance effect of La{sub 0.67}Ba{sub 0.33}MnO{sub 3} (LBMO). The LBMO samples were synthesized using solid state reaction. Characterization using X-ray diffraction shows that all LBMO samples have a single phase for each variation. Variation of sintering temperature on the LBMO samples affects its lattice parameters. The resistivity measurement in an absence and under applied magnetic field resulted in a highly significant different values. In one of the sintering temperature variation of LBMO, an increasing resistivity had shown atmore » a low temperature and had reached its maximum value at a specific temperature, and then the resistivity decreases to the lowest value near the room temperature. Similar result observed at higher varieties of sintering temperature but with significant lower maximum resistivity.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Siwei; Chen, Yan; Zhang, Lingling

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ(BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. In this paper, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering wasmore » improved to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. In conclusion, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Siwei; Chen, Yan; Zhang, Lingling

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. Here, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improvedmore » to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. Moreover, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less

Effect of Spark-Plasma-Sintering Conditions on Tensile Properties of Aluminum Matrix Composites Reinforced with Multiwalled Carbon Nanotubes (MWCNTs)

NASA Astrophysics Data System (ADS)

Chen, B.; Imai, H.; Umeda, J.; Takahashi, M.; Kondoh, K.

2017-04-01

In this study, aluminum (Al) matrix composites containing 2 wt.% multiwalled carbon nanotubes (CNTs) were fabricated by powder metallurgy using high-energy ball milling (HEBM), spark plasma sintering (SPS), and subsequent hot extrusion. The effect of SPS conditions on the tensile properties of CNT/Al composites was investigated. The results showed that composites with well-dispersed CNTs and nearly full-density CNT/Al can be obtained. During HEBM, CNTs were shortened, inserted into welded Al powder particles, bonded to Al, and still stable without CNT-Al reaction. After consolidation, Al4C3 phases formed in composites under different sintering conditions. With the increase of sintering temperature and holding time, the strength decreased. Conversely, the ductility and toughness noticeably increased. As a result, a good balance between strength (367 MPa in ultimate tensile strength) and ductility (13% in elongation) was achieved in the as-extruded CNT/Al composite sintered at 630°C with a holding time of 300 min.

Optimization of Sinter Plant Operating Conditions Using Advanced Multivariate Statistics: Intelligent Data Processing

NASA Astrophysics Data System (ADS)

Fernández-González, Daniel; Martín-Duarte, Ramón; Ruiz-Bustinza, Íñigo; Mochón, Javier; González-Gasca, Carmen; Verdeja, Luis Felipe

2016-08-01

Blast furnace operators expect to get sinter with homogenous and regular properties (chemical and mechanical), necessary to ensure regular blast furnace operation. Blends for sintering also include several iron by-products and other wastes that are obtained in different processes inside the steelworks. Due to their source, the availability of such materials is not always consistent, but their total production should be consumed in the sintering process, to both save money and recycle wastes. The main scope of this paper is to obtain the least expensive iron ore blend for the sintering process, which will provide suitable chemical and mechanical features for the homogeneous and regular operation of the blast furnace. The systematic use of statistical tools was employed to analyze historical data, including linear and partial correlations applied to the data and fuzzy clustering based on the Sugeno Fuzzy Inference System to establish relationships among the available variables.

Sintering activation energy MoSi2-WSi2-Si3N4 ceramic

NASA Astrophysics Data System (ADS)

Titov, D. D.; Lysenkov, A. S.; Kargin, Yu F.; Frolova, M. G.; Gorshkov, V. A.; Perevislov, S. N.

2018-04-01

The activation energy of sintering process was calculated based on dilatometric studies of shrinkage processes (Mo,W)Si2 + Si3N4 composite ceramic. (Mo,W)Si2 powders was obtained by solid-phase solutions of 70 wt% MoSi2 and 30 wt% WSi2 by SHS in the ISMAN RAS. The concentration rate Si3N4 was from 1 to 15 wt.%. The sintering was carried out to 1850°C in Ar atmosphere the heating rate of 5, 10, 12 and 15°C/min by the way of dilatometer tests. Based on the differential kinetic analysis method (Friedman’s method), the sintering process activation energy of (Mo,W)Si2 + Si3N4 were calculated. The two-stage sintering process and the dependence of the activation energy on the Si3N4 content was shown. Average value of 370 kJ/mol for Q was obtained.

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

PubMed

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.

Radiation-Thermal Sintering of Zirconia Powder Compacts Under Conditions of Bilateral Heating Using Beams of Low-Energy Electrons

NASA Astrophysics Data System (ADS)

Ghyngazov, S. A.; Frangulyan, T. S.; Chernyavskii, A. V.; Goreev, A. K.; Naiden, E. P.

2015-06-01

Comparative experiments on sintering zirconia ceramics are performed using colliding beams of low-energy electrons and under conditions of thermal heating. The density and microhardness of ceramic materials manufactured via different processes are determined. The use of a regime of bilateral heating by high-intensity,low-energy electron beams is shown to intensify the sintering process and yield material specimens with improved characteristics compared to those formed by thermal sintering.

Molten salt synthesis of nanocrystalline phase of high dielectric constant material CaCu3Ti4O12.

PubMed

Prakash, B Shri; Varma, K B R

2008-11-01

Nanocrystalline powders of giant dielectric constant material, CaCu3Ti4O12 (CCTO), have been prepared successfully by the molten salt synthesis (MSS) using KCl at 750 degrees C/10 h, which is significantly lower than the calcination temperature (approximately 1000 degrees C) that is employed to obtain phase pure CCTO in the conventional solid-state reaction route. The water washed molten salt synthesized powder, characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) confirmed to be a phase pure CCTO associated with approximately 150 nm sized crystallites of nearly spherical shape. The decrease in the formation temperature/duration of CCTO in MSS method was attributed to an increase in the diffusion rate or a decrease in the diffusion length of reacting ions in the molten salt medium. As a consequence of liquid phase sintering, pellets of as-synthesized KCl containing CCTO powder exhibited higher sinterability and grain size than that of KCl free CCTO samples prepared by both MSS method and conventional solid-state reaction route. The grain size and the dielectric constant of KCl containing CCTO ceramics increased with increasing sintering temperature (900 degrees C-1050 degrees C). Indeed the dielectric constants of these ceramics were higher than that of KCl free CCTO samples prepared by both MSS method and those obtained via the solid-state reaction route and sintered at the same temperature. Internal barrier layer capacitance (IBLC) model was invoked to correlate the observed dielectric constant with the grain size in these samples.

Development of a sintering process for recycling oil shale fly ash and municipal solid waste incineration bottom ash into glass ceramic composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Zhikun; Zhang, Lei; Li, Aimin, E-mail: leeam@dlut.edu.cn

Highlights: • Glass ceramic composite is prepared from oil shale fly ash and MSWI bottom ash. • A novel method for the production of glass ceramic composite is presented. • It provides simple route and lower energy consumption in terms of recycling waste. • The vitrified slag can promote the sintering densification process of glass ceramic. • The performances of products decrease with the increase of oil shale fly ash content. - Abstract: Oil shale fly ash and municipal solid waste incineration bottom ash are industrial and municipal by-products that require further treatment before disposal to avoid polluting the environment.more » In the study, they were mixed and vitrified into the slag by the melt-quench process. The obtained vitrified slag was then mixed with various percentages of oil shale fly ash and converted into glass ceramic composites by the subsequent sintering process. Differential thermal analysis was used to study the thermal characteristics and determine the sintering temperatures. X-ray diffraction analysis was used to analyze the crystalline phase compositions. Sintering shrinkage, weight loss on ignition, density and compressive strength were tested to determine the optimum preparation condition and study the co-sintering mechanism of vitrified amorphous slag and oil shale fly ash. The results showed the product performances increased with the increase of sintering temperatures and the proportion of vitrified slag to oil shale fly ash. Glass ceramic composite (vitrified slag content of 80%, oil shale fly ash content of 20%, sintering temperature of 1000 °C and sintering time of 2 h) showed the properties of density of 1.92 ± 0.05 g/cm{sup 3}, weight loss on ignition of 6.14 ± 0.18%, sintering shrinkage of 22.06 ± 0.6% and compressive strength of 67 ± 14 MPa. The results indicated that it was a comparable waste-based material compared to previous researches. In particular, the energy consumption in the production process was reduced compared to conventional vitrification and sintering method. Chemical resistance and heavy metals leaching results of glass ceramic composites further confirmed the possibility of its engineering applications.« less

Hybrid processing and anisotropic sintering shrinkage in textured ZnO ceramics

PubMed Central

Keskinbora, Kahraman; Suzuki, Tohru S; Ozgur Ozer, I; Sakka, Yoshio; Suvaci, Ender

2010-01-01

We have studied the combined effects of the templated grain growth and magnetic alignment processes on sintering, anisotropic sintering shrinkage, microstructure development and texture in ZnO ceramics. Suspensions of 0–10 vol % ZnO template particles were slip cast in a 12 T rotating magnetic field. Sintering and texture characteristics were investigated via thermomechanical analysis and electron backscatter diffraction, respectively. Sintering as well as texture characteristics depend on template concentration. For the studied ZnO system, there is a critical template concentration (2 vol % in this study) above which densification is limited by the templates owing to constrained sintering. Below this limit, the densification is enhanced and the anisotropic shrinkage is reduced, which is attributed to densifying characteristics of the templates. PMID:27877373

Production of cerium dioxide microspheres by an internal gelation sol–gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Katalenich, Jeffrey A.

An internal gelation sol-gel technique was used to prepare cerium dioxide microspheres with uniform diameters near 100 µm. In this process, chilled aqueous solutions containing cerium, hexamethylenetetramine (HMTA), and urea are transformed into a solid gel by heat addition and are subsequently washed, dried, and sintered to produce pure cerium dioxide. Cerous nitrate and ceric ammonium nitrate solutions were compared for their usefulness in microsphere production. Gelation experiments were performed with both cerous nitrate and ceric ammonium nitrate to determine desirable concentrations of cerium, HMTA, and urea in feed solutions as well as the necessary quantity of ammonium hydroxide addedmore » to cerium solutions. Analysis of the pH before and after sample gelation was found to provide a quantitative metric for optimal parameter selection along with subjective evaluations of gel qualities. The time necessary for chilled solutions to gel upon inserting into a hot water bath was determined for samples with a variety of parameters and also used to determine desirable formulations for microsphere production. A technique for choosing the optimal mixture of ceric ammonium nitrate, HMTA, and urea was determined using gelation experiments and used to produce microspheres by dispersion of the feed solution into heated silicone oil. Gelled spheres were washed to remove excess reactants and reaction products before being dried and sintered. X-ray diffraction of air-dried microspheres, sintered microspheres, and commercial CeO 2 powders indicated that air-dried and sintered spheres were pure CeO 2.« less

Study on the influences of reduction temperature on nickel-yttria-stabilized zirconia solid oxide fuel cell anode using nickel oxide-film electrode

NASA Astrophysics Data System (ADS)

Jiao, Zhenjun; Ueno, Ai; Suzuki, Yuji; Shikazono, Naoki

2016-10-01

In this study, the reduction processes of nickel oxide at different temperatures were investigated using nickel-film anode to study the influences of reduction temperature on the initial performances and stability of nickel-yttria-stabilized zirconia anode. Compared to conventional nickel-yttria-stabilized zirconia composite cermet anode, nickel-film anode has the advantage of direct observation at nickel-yttria-stabilized zirconia interface. The microstructural changes were characterized by scanning electron microscopy. The reduction process of nickel oxide is considered to be determined by the competition between the mechanisms of volume reduction in nickel oxide-nickel reaction and nickel sintering. Electrochemical impedance spectroscopy was applied to analyze the time variation of the nickel-film anode electrochemical characteristics. The anode performances and microstructural changes before and after 100 hours discharging and open circuit operations were analyzed. The degradation of nickel-film anode is considered to be determined by the co-effect between the nickel sintering and the change of nickel-yttria-stabilized zirconia interface bonding condition.

Fabrication of porous silicon nitride ceramics using binder jetting technology

NASA Astrophysics Data System (ADS)

Rabinskiy, L.; Ripetsky, A.; Sitnikov, S.; Solyaev, Y.; Kahramanov, R.

2016-07-01

This paper presents the results of the binder jetting technology application for the processing of the Si3N4-based ceramics. The difference of the developed technology from analogues used for additive manufacturing of silicon nitride ceramics is a method of the separate deposition of the mineral powder and binder without direct injection of suspensions/slurries. It is assumed that such approach allows reducing the technology complexity and simplifying the process of the feedstock preparation, including the simplification of the composite materials production. The binders based on methyl ester of acrylic acid with polyurethane and modified starch were studied. At this stage of the investigations, the technology of green body's fabrication is implemented using a standard HP cartridge mounted on the robotic arm. For the coordinated operation of the cartridge and robot the specially developed software was used. Obtained green bodies of silicon powder were used to produce the ceramic samples via reaction sintering. The results of study of ceramics samples microstructure and composition are presented. Sintered ceramics are characterized by fibrous α-Si3N4 structure and porosity up to 70%.

Electrochemical Synthesis of Core–Shell-Structured NbC–Fe Composite Powder for Enforcement in Low-Carbon Steel

PubMed Central

Song, Qiushi; Xu, Qian; Chen, Ying; Xu, Liang; Man, Tiannan

2017-01-01

An NbC–Fe composite powder was synthesized from an Nb2O5/Fe/C mixture by electrochemical reduction and subsequent carbonization in molten CaCl2–NaCl. The composite has a core–shell structure, in which NbC acts as the cores distributing in the Fe matrix. A strong bonding between NbC and Fe is benefit from the core–shell structure. The sintering and electrochemical reduction processes were investigated to probe the mechanism for the reactions. The results show that NbC particles about several nanometers were embraced by the Fe shell to form a composite about 100 nm in size. This featured structure can feasibly improve the wettability and sinterability of NbC as well as the uniform distribution of the carbide in the cast steel. By adding the composite into steel in the casting process, the grain size of the casted steel was markedly deceased from 1 mm to 500 μm on average, favoring the hardening of the casted steel. PMID:29104266

Advanced Ceramic Technology for Space Applications at NASA MSFC

NASA Technical Reports Server (NTRS)

Alim, Mohammad A.

2003-01-01

The ceramic processing technology using conventional methods is applied to the making of the state-of-the-art ceramics known as smart ceramics or intelligent ceramics or electroceramics. The sol-gel and wet chemical processing routes are excluded in this investigation considering economic aspect and proportionate benefit of the resulting product. The use of ceramic ingredients in making coatings or devices employing vacuum coating unit is also excluded in this investigation. Based on the present information it is anticipated that the conventional processing methods provide identical performing ceramics when compared to that processed by the chemical routes. This is possible when sintering temperature, heating and cooling ramps, peak temperature (sintering temperature), soak-time (hold-time), etc. are considered as variable parameters. In addition, optional calcination step prior to the sintering operation remains as a vital variable parameter. These variable parameters constitute a sintering profile to obtain a sintered product. Also it is possible to obtain identical products for more than one sintering profile attributing to the calcination step in conjunction with the variables of the sintering profile. Overall, the state-of-the-art ceramic technology is evaluated for potential thermal and electrical insulation coatings, microelectronics and integrated circuits, discrete and integrated devices, etc. applications in the space program.

Enery Efficient Press and Sinter of Titanium Powder for Low-Cost Components in Vehicle Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas Zwitter; Phillip Nash; Xiaoyan Xu

2011-03-31

This is the final technical report for the Department of Energy NETL project NT01931 Energy Efficient Press and Sinter of Titanium Powder for Low-Cost Components in Vehicle Applications. Titanium has been identified as one of the key materials with the required strength that can reduce the weight of automotive components and thereby reduce fuel consumption. Working with newly developed sources of titanium powder, Webster-Hoff will develop the processing technology to manufacture low cost vehicle components using the single press/single sinter techniques developed for iron based powder metallurgy today. Working with an automotive or truck manufacturer, Webster-Hoff will demonstrate the feasibilitymore » of manufacturing a press and sinter titanium component for a vehicle application. The project objective is two-fold, to develop the technology for manufacturing press and sinter titanium components, and to demonstrate the feasibility of producing a titanium component for a vehicle application. The lowest cost method for converting metal powder into a net shape part is the Powder Metallurgy Press and Sinter Process. The method involves compaction of the metal powder in a tool (usually a die and punches, upper and lower) at a high pressure (up to 60 TSI or 827 MPa) to form a green compact with the net shape of the final component. The powder in the green compact is held together by the compression bonds between the powder particles. The sinter process then converts the green compact to a metallurgically bonded net shape part through the process of solid state diffusion. The goal of this project is to expand the understanding and application of press and sinter technology to Titanium Powder applications, developing techniques to manufacture net shape Titanium components via the press and sinter process. In addition, working with a vehicle manufacturer, demonstrate the feasibility of producing a titanium component for a vehicle. This is not a research program, but rather a project to develop a process for press and sinter of net shape Titanium components. All of these project objectives have been successfully completed.« less

Synthesis of Silicon Nitride and Silicon Carbide Nanocomposites through High Energy Milling of Waste Silica Fume for Structural Applications

NASA Astrophysics Data System (ADS)

Suri, Jyothi

Nanocomposites have been widely used in a multitude of applications in electronics and structural components because of their improved mechanical, electrical, and magnetic properties. Silicon nitride/Silicon carbide (Si 3N4/SiC) nanocomposites have been studied intensively for low and high temperature structural applications, such as turbine and automobile engine components, ball bearings, turbochargers, as well as energy applications due to their superior wear resistance, high temperature strength, high oxidation resistance and good creep resistance. Silica fume is the waste material produced during the manufacture of silicon and ferro-silicon alloys, and contains 94 to 97 wt.% SiO2. In the present dissertation, the feasibility of using waste silica fume as the raw material was investigated to synthesize (I) advanced nanocomposites of Si3N4/SiC, and (2) porous silicon carbide (SiC) for membrane applications. The processing approach used to convert the waste material to advanced ceramic materials was based on a novel process called, integrated mechanical and thermal activation process (IMTA) process. In the first part of the dissertation, the effect of parameters such as carbothermic nitridation and reduction temperature and the graphite concentration in the starting silica fume plus graphite mixture, were explored to synthesize nanocomposite powders with tailored amounts of Si3N4 and SiC phases. An effective way to synthesize carbon-free Si3N 4/SiC composite powders was studied to provide a clear pathway and fundamental understanding of the reaction mechanisms. Si3N4/SiC nanocomposite powders were then sintered using two different approaches, based on liquid phase sintering and spark plasma sintering processes, with Al 2O3 and Y2O3 as the sintering aids. The nanocomposites were investigated for their densification behavior, microstructure, and mechanical properties. Si3N4/SiC nanocomposites thus obtained were found to possess superior mechanical properties at much lower costs. The second part of the work has comprised of the successful fabrication of bilayered SiC membranes with a graded porosity, consisting of porous nano-SiC layer on the surface of a porous coarse-grained SiC support layer. The effect of different particle sizes of SiC in the support layers was systematically studied. Also, the effects of sintering temperature were investigated to control the pore size, particle size and overall density of the bi-layered SiC membrane.

Removable partial denture alloys processed by laser-sintering technique.

PubMed

Alageel, Omar; Abdallah, Mohamed-Nur; Alsheghri, Ammar; Song, Jun; Caron, Eric; Tamimi, Faleh

2018-04-01

Removable partial dentures (RPDs) are traditionally made using a casting technique. New additive manufacturing processes based on laser sintering has been developed for quick fabrication of RPDs metal frameworks at low cost. The objective of this study was to characterize the mechanical, physical, and biocompatibility properties of RPD cobalt-chromium (Co-Cr) alloys produced by two laser-sintering systems and compare them to those prepared using traditional casting methods. The laser-sintered Co-Cr alloys were processed by the selective laser-sintering method (SLS) and the direct metal laser-sintering (DMLS) method using the Phenix system (L-1) and EOS system (L-2), respectively. L-1 and L-2 techniques were 8 and 3.5 times more precise than the casting (CC) technique (p < 0.05). Co-Cr alloys processed by L-1 and L-2 showed higher (p < 0.05) hardness (14-19%), yield strength (10-13%), and fatigue resistance (71-72%) compared to CC alloys. This was probably due to their smaller grain size and higher microstructural homogeneity. All Co-Cr alloys exhibited low porosity (2.1-3.3%); however, pore distribution was more homogenous in L-1 and L-2 alloys when compared to CC alloys. Both laser-sintered and cast alloys were biocompatible. In conclusion, laser-sintered alloys are more precise and present better mechanical and fatigue properties than cast alloys for RPDs. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 1174-1185, 2018. © 2017 Wiley Periodicals, Inc.

Effects of the addition of municipal solid waste incineration fly ash on the behavior of polychlorinated dibenzo-p-dioxins and furans in the iron ore sintering process.

PubMed

Min, Yi; Liu, Chengjun; Shi, Peiyang; Qin, Chongda; Feng, Yutao; Liu, Baichen

2018-04-11

Raw materials were co-sintered with municipal solid waste incineration (MSWI) fly ash through iron ore sintering to promote the safe treatment and utilization of MSWI fly ash. To assess the feasibility of this co-sintering method, in this study, the effects of the addition of MSWI fly ash on the formation and emission of polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs) were estimated via iron ore sintering pot experiments. During co-sintering, most of the PCDD/Fs in the added MSWI fly ash were decomposed and transformed into PCDD/Fs associated with iron sintering, and the concentrations of lower- and mid-chlorinated congeners increased. As there was a sufficient chlorine source and the sintering bed permeability was decreased by the addition of MSWI fly ash, the PCDD/F concentration in the exhaust gas increased. The mass emission of PCDD/Fs decreased; however, the emission of toxic PCDD/Fs increased beyond the total emissions from the independent MSW incineration and iron ore sintering processes due to the transformation of PCDD/F congeners. The co-sintering may be an important solution after technological improvements in the flue gas cleaning system and PCDD/F formation inhibition procedures. Copyright © 2018. Published by Elsevier Ltd.

Microwave sintering of nanopowder ZnNb2O6: Densification, microstructure and microwave dielectric properties

NASA Astrophysics Data System (ADS)

Bafrooei, H. Barzegar; Nassaj, E. Taheri; Hu, C. F.; Huang, Q.; Ebadzadeh, T.

2014-12-01

High density ZnNb2O6 ceramics were successfully fabricated by microwave sintering of ZnO-Nb2O5 and ZnNb2O6 nanopowders. Phase formation, microstructure and microwave electrical properties of the microwave sintered (MS) and microwave reaction sintered (MRS) specimens were examined using X-ray diffraction, field emission scanning electron microscopy and microwave dielectric properties measurement. Specimens were sintered in a temperature range from 950 to 1075 °C for 30 min at an interval of 25 °C using a microwave furnace operated at 2.45 GHz frequency, 3 kW power. XRD pattern revealed the formation of pure columbite phase of ZnNb2O6. The SEM micrographs show grain growth and reduction in porosity of specimens with the increase in sintering temperature. Good combination of microwave dielectric properties (εr~23.6, Qf~64,300 GHz and τf~-66 ppm/°C and εr~24, Qf~75,800 GHz and τf~-64 ppm/°C) was obtained for MS- and MRS-prepared samples at 1000 °C and 1050 °C for 30 min, respectively.

Thermal barrier coating resistant to sintering

DOEpatents

Subramanian, Ramesh; Seth, Brig B.

2005-08-23

A device (10) is made, having a ceramic thermal barrier coating layer (16) characterized by a microstructure having gaps (18) with a sintering inhibiting material (22) disposed on the columns (20) within the gaps (18). The sintering resistant material (22) is stable over the range of operating temperatures of the device (10), is not soluble with the underlying ceramic layer (16) and is applied by a process that is not an electron beam physical vapor deposition process. The sintering inhibiting material (22) has a morphology adapted to improve the functionality of the sintering inhibiting material (22), characterized as continuous, nodule, rivulet, grain, crack, flake and combinations thereof and being disposed within at least some of the vertical and horizontal gaps.

Si-Ca species modification and microwave sintering for NiZn ferrites

NASA Astrophysics Data System (ADS)

Yang, Yin-Ju; Sheu, Ching-Iuan; Cheng, Syh-Yuh; Chang, Horng-Yi

2004-12-01

NiZn ferrite particles were precoated with Si-Ca precursor by sol-gel method. Thus convention-sintered particles exhibited small grain size about 2 μm and lowered magnetic permeability as well as increased coercive magnetic field effectively. Microwave sintering could suppress grain growth as the same result of conventional sintering specimens with SiO2-CaO precoating. In microwave process, the grain growth inhibition expressed more obviously for the SiO2-CaO precoated specimens. The magnetic permeability (∼300) after SiO2-CaO precoating became lower than original ferrite (∼800) without SiO2-CaO precoating in conventional sintering. However, the magnetic permeability was lowered no matter whether SiO2-CaO precoating in microwave process. On the other hand, microwave sintering possessed short processing time, for example, 1250 °C/5 min, to prohibit ZnO volatilization in accompanied with grain size reduction. Therefore, such contribution increased resistivity to about 12×106 Ω cm compared to 3×106 Ω cm of original NiZn ferrite. The large coercive magnetic field (Hc) was ascribed to the superposition of small grain size and stress induced by microwave sintering.

Thermal Test on Target with Pressed Disks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Woloshun, Keith Albert; Dale, Gregory E.; Olivas, Eric Richard

A thorough test of the thermal performance of a target for Mo 99 production using solid Mo 100 target to produce the Mo 99 via a gamma-n reaction has previously been conducted at Argonne National Laboratory (ANL). The results are reported in “Zero Degree Line Mo Target Thermal Test Results and Analysis,” LANL report Number LA-UR-15-23134 dated 3/27/15. This target was comprised of 25 disks 1 mm thick and 12 mm in diameter, separated by helium coolant gaps 0.5 mm wide. The test reported in the above referenced report was conducted with natural Mo disks all cut from commercial rod.more » The production plant will have Mo 100 disks pressed and sintered using a process being developed at Oak Ridge National Laboratory (ORNL). The structural integrity of press-and-sinter disks is of some concern. The test reported herein included 4 disks made by the ORNL process and placed in the high heat, and therefore high thermal stress, region of the target. The electron beam energy was 23 MeV for these tests. Beam spot size was 3.5 mm horizontal and 3 mm vertical, FWHM. The thermal stress test of pressed-and-sintered disks resulted in no mechanical failures. The induced thermal stresses were below yield stress for natural Mo, indicating that up to that stress state no inherent deficiencies in the mechanical properties of the fabricated disks were evident.« less

Improved carbon control in the sintering of structural PM parts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nowotarski, M.; Gaines, G.

1981-12-01

The use of a nitrogen-methanol atmosphere and a system of control of the atmosphere in furnace zones to provide improved control of carbon in sintering of sprockets are described.A new process has been developed by the Linde Div. of Union Carbide for the sintering of structural PM parts. The process is based on a nitrogen/methanol sintering atmosphere and features superior carbon control (/plus or minus/.03%), elimination of sooting due to lubricant decomposition, and significantly reduced furnace atmosphere gas flows as compared to typical endothermic atmosphere gas consumption.

Processing and Characterization of Porous Ti2AlC with Controlled Porosity and Pore Size

DTIC Science & Technology

2012-09-11

fabricated by spark plasma sintering , were also characterized. The effects of porosity and/or pore size on the room temperature elastic moduli...pressureless- sintered without NaCl pore former, or fabricated by spark plasma sintering , were also characterized. The effects of porosity and/or pore size...as well as several samples sintered using spark plasma sintering (SPS). Furthermore, we demon- strate that the developed methodology can be implemented

Stability investigation of a high number density Pt1/Fe2O3 single-atom catalyst under different gas environments by HAADF-STEM

NASA Astrophysics Data System (ADS)

Duan, Sibin; Wang, Rongming; Liu, Jingyue

2018-05-01

Catalysis by supported single metal atoms has demonstrated tremendous potential for practical applications due to their unique catalytic properties. Unless they are strongly anchored to the support surfaces, supported single atoms, however, are thermodynamically unstable, which poses a major obstacle for broad applications of single-atom catalysts (SACs). In order to develop strategies to improve the stability of SACs, we need to understand the intrinsic nature of the sintering processes of supported single metal atoms, especially under various gas environments that are relevant to important catalytic reactions. We report on the synthesis of high number density Pt1/Fe2O3 SACs using a facial strong adsorption method and the study of the mobility of these supported Pt single atoms at 250 °C under various gas environments that are relevant to CO oxidation, water–gas shift, and hydrogenation reactions. Under the oxidative gas environment, Fe2O3 supported Pt single atoms are stable even at high temperatures. The presence of either CO or H2 molecules in the gas environment, however, facilitates the movement of the Pt atoms. The strong interaction between CO and Pt weakens the binding between the Pt atoms and the support, facilitating the movement of the Pt single atoms. The dissociation of H2 molecules on the Pt atoms and their subsequent interaction with the oxygen species of the support surfaces dislodge the surface oxygen anchored Pt atoms, resulting in the formation of Pt clusters. The addition of H2O molecules to the CO or H2 significantly accelerates the sintering of the Fe2O3 supported Pt single atoms. An anchoring-site determined sintering mechanism is further proposed, which is related to the metal–support interaction.

Stability investigation of a high number density Pt1/Fe2O3 single-atom catalyst under different gas environments by HAADF-STEM.

PubMed

Duan, Sibin; Wang, Rongming; Liu, Jingyue

2018-05-18

Catalysis by supported single metal atoms has demonstrated tremendous potential for practical applications due to their unique catalytic properties. Unless they are strongly anchored to the support surfaces, supported single atoms, however, are thermodynamically unstable, which poses a major obstacle for broad applications of single-atom catalysts (SACs). In order to develop strategies to improve the stability of SACs, we need to understand the intrinsic nature of the sintering processes of supported single metal atoms, especially under various gas environments that are relevant to important catalytic reactions. We report on the synthesis of high number density Pt 1 /Fe 2 O 3 SACs using a facial strong adsorption method and the study of the mobility of these supported Pt single atoms at 250 °C under various gas environments that are relevant to CO oxidation, water-gas shift, and hydrogenation reactions. Under the oxidative gas environment, Fe 2 O 3 supported Pt single atoms are stable even at high temperatures. The presence of either CO or H 2 molecules in the gas environment, however, facilitates the movement of the Pt atoms. The strong interaction between CO and Pt weakens the binding between the Pt atoms and the support, facilitating the movement of the Pt single atoms. The dissociation of H 2 molecules on the Pt atoms and their subsequent interaction with the oxygen species of the support surfaces dislodge the surface oxygen anchored Pt atoms, resulting in the formation of Pt clusters. The addition of H 2 O molecules to the CO or H 2 significantly accelerates the sintering of the Fe 2 O 3 supported Pt single atoms. An anchoring-site determined sintering mechanism is further proposed, which is related to the metal-support interaction.

Production of sintered porous metal fluoride pellets

DOEpatents

Anderson, L.W.; Stephenson, M.J.

1973-12-25

Porous pellets characterized by a moderately reactive crust and a softer core of higher reactivity are produced by forming agglomerates containing a metal fluoride powder and a selected amount ofwater. The metal fluoride is selected to be sinterable and essentially non-reactive with gaseous fluorinating agents. The agglomerates are contacted with a gaseous fluorinating agent under controlled conditions whereby the heat generated by localized reaction of the agent and water is limited to values effccting bonding by localized sintering. Porous pellets composed of cryolite (Na/sub 3/AlF/sub 6/) can be used to selectively remove trace quantities of niobium pentafluoride from a feed gas consisting predominantly of uranium hexafluoride. (Official Gazette)

Ice sintering timescales at the surface of Europa and implications for surface properties

NASA Astrophysics Data System (ADS)

Molaro, Jamie; Phillips, Cynthia B.; Meirion-Griffith, Gareth

2017-10-01

The planned exploration of Europa by NASA’s Europa Clipper Mission and the possibility of a future Europa lander have driven the need to characterize its surface strength, roughness, porosity, thermal conductivity, and regolith depth in order to accurately interpret remote sensing data and develop appropriate spacecraft landing systems. Many processes contribute to Europa’s landscape evolution, such as sputtering, mass wasting, thermal segregation, and impact gardening, driving the creation and distribution of icy regolith across the surface. While the efficacy of these processes are not well constrained, any amount of regolith emplaced at the surface will undergo subsequent processing due to sintering. Ice sintering is a form of frost metamorphism whereby contacting ice grains experience the diffusion of material into their contact region, forming a “neck” between them and densifying over time. Over long enough timescales, ice aggregates will sinter into solid material, which may contribute to the incorporation of non-ice material into Europa’s subsurface and help to drive subsurface chemistry. Sintering also interacts with other processes, adding to the complexity of icy surface evolution. For example, sputtering preferentially removes larger grains and may enhance sintering rates, and changes in ice porosity may affect the response of the surface to micrometeorite impacts.Quantifying the effects of ice sintering will allow us to predict the microstructural properties of Europa’s surface at spacecraft scales. To this end, we have modeled pressure-less (no overburden) sintering of spherical water-ice grains and validated the results with a laboratory experiment. We also modeled ice at the surface of Europa to obtain a first-order approximation of the sintering timescale and surface properties. Preliminary results indicate that ice grains will experience neck growth but not significant densification over Europa’s surface age, suggesting that loose surface ice forms a weak and porous crust. Furthermore, our results suggest that existing models do not accurately quantify all stages of the sintering process for ice, emphasizing the need for more laboratory studies on this topic.

Optimal Design of Material and Process Parameters in Powder Injection Molding

NASA Astrophysics Data System (ADS)

Ayad, G.; Barriere, T.; Gelin, J. C.; Song, J.; Liu, B.

2007-04-01

The paper is concerned with optimization and parametric identification for the different stages in Powder Injection Molding process that consists first in injection of powder mixture with polymer binder and then to the sintering of the resulting powders part by solid state diffusion. In the first part, one describes an original methodology to optimize the process and geometry parameters in injection stage based on the combination of design of experiments and an adaptive Response Surface Modeling. Then the second part of the paper describes the identification strategy that one proposes for the sintering stage, using the identification of sintering parameters from dilatometeric curves followed by the optimization of the sintering process. The proposed approaches are applied to the optimization of material and process parameters for manufacturing a ceramic femoral implant. One demonstrates that the proposed approach give satisfactory results.

Field assisted sintering of refractory carbide ceramics and fiber reinforced ceramic matrix composites

NASA Astrophysics Data System (ADS)

Gephart, Sean

The sintering behaviors of silicon carbide (SiC) and boron carbide (B4C) based materials were investigated using an emerging sintering technology known as field assisted sintering technology (FAST), also known as spark plasma sintering (SPS) and pulse electric current sintering (PECS). Sintering by FAST utilizes high density electric current, uniaxial pressure, and relatively high heating rate compared to conventional sintering techniques. This effort investigated issues of scaling from laboratory FAST system (25 ton capacity) to industrial FAST system (250 ton capacity), as well as exploring the difference in sintering behavior of single phase B4C and SiC using FAST and conventional sintering techniques including hot-pressing (HP) and pressure-less sintering (PL). Materials were analyzed for mechanical and bulk properties, including characterization of density, hardness, fracture toughness, fracture (bend) strength, elastic modulus and microstructure. A parallel investigation was conducted in the development of ceramic matrix composites (CMC) using SiC powder impregnation of fiber compacts followed by FAST sintering. The FAST technique was used to sinter several B4C and SiC materials to near theoretical density. Preliminary efforts established optimized sintering temperatures using the smaller 25 ton laboratory unit, targeting a sample size of 40 mm diameter and 8 mm thickness. Then the same B4C and SiC materials were sintered by the larger 250 ton industrial FAST system, a HP system, and PL sintering system with a targeted dense material geometry of 4 x 4 x 0.315 inches3 (101.6 x 101.6 x 8 mm3). The resulting samples were studied to determine if the sintering dynamics and/or the resulting material properties were influenced by the sintering technique employed. This study determined that FAST sintered ceramic materials resulted in consistently higher averaged values for mechanical properties as well as smaller grain size when compared to conventionally sintered materials. While FAST sintered materials showed higher average values, in general they also showed consistently larger variation in the scattered data and consequently larger standard deviation for the resulting material properties. In addition, dynamic impact testing (V50 test) was conducted on the resulting materials and it was determined that there was no discernable correlation between observed mechanical properties of the ceramic materials and the resulting dynamic testing. Another study was conducted on the sintering of SiC and carbon fiber reinforced SiC ceramic matrix composites (CMC) using FAST. There has been much interest recently in fabricating high strength, low porosity SiC CMC.s for high temperature structural applications, but the current methods of production, namely chemical vapor infiltration (CVI), melt infiltration (MI), and polymer infiltration and pyrolysis (PIP), are considered time consuming and involve material related shortcomings associated with their respective methodologies. In this study, SiC CMC.s were produced using the 25 ton laboratory unit with a target sample size of 40 mm diameter and 3 mm thickness, as well as on the larger 250 ton industrial FAST system targeting a sample size of 101.6 x 101.6 x 3 mm3 to investigate issues associated with scaling. Several sintering conditions were explored including: pressure of 35-65 MPa, temperature of 1700-1900°C, and heating rates between 50-400°C/min. The SiC fibers used in this study were coated using chemical vapor deposition (CVD) with boron nitride (BN) and pyrolytic carbon to act as a barrier layer and preserve the integrity of the fibers during sintering. Then the barrier coating was coated by an outer layer of SiC to enhance the bonding between the fibers and the SiC matrix. Microstructures of the sintered samples were examined by FE-SEM. Mechanical properties including flexural strength-deflection and stress-strain were characterized using 4-point bend testing. Tensile testing was performed on the larger 101.6 x 101.6 x 3 mm samples. The microstructures of samples sintered using the 25 ton laboratory FAST system showed a reduction in porosity and good adhesion between the fiber-fiber and fiber-matrix interface. The microstructures of samples sintered on the 250 ton industrial FAST system showed a reduction in porosity, but there was visible reaction of the fiber and fiber coatings with the surrounding matrix. Additionally, there was significant radial cracking of the fibers visible in the microstructures. There is gap in the understanding of sintering behavior between laboratory and industrial scale FAST systems. The vast majority of publications on FAST sintering have been primarily focused on small sample geometries (20 mm diameter, less than 3 mm thick). A study was coordinated to investigate the thermal properties during heating and cooling using a 250 ton industrial FAST system at 900°C using B4C and SiC materials inside the graphite die assembly. The thermal properties were then compared to the resulting material properties of the identically sintered B4C and SiC to approximately 94% relative density, at a temperature of 1950°C, pressure of 45 MPa, 10 minute hold, and heated at a rate of 100°C/min. The study determined that at 900°C there were significant thermal gradients within the system for the examined materials, and that these gradients correlated well with the material property difference of the samples sintered at higher temperatures where the gradients are presumably larger due to an increase in radiative heat loss. The observed temperatures throughout the graphite were significantly different between B4C and SiC. These temperatures also correlated well with the material properties of the sintered products which showed more substantial variation for B4C when compared to SiC which was overall less affected by thermal gradients. This was attributed to the intrinsic thermal conductivity difference between the two subject materials which was manifested as thermal gradients throughout the material and graphite die assembly. Additionally, both the observed temperature gradients throughout the graphite die assembly and the difference in temperature reading between the optical pyrometer and thermocouples were significantly larger for the 250 ton FAST system than previous publications have demonstrated experimentally or via modeling of smaller laboratory scale systems. The findings from this work showed that relative to conventional sintering methods, the FAST process demonstrated comparable or improved material and mechanical properties with a significantly shorter processing cycle. However, the results demonstrated on the 25 ton laboratory scale unit were significantly different compared to results for the same materials sintered using the 250 ton industrial scale unit. The temperature gradients observed on the 250 ton FAST unit were significantly larger than previous reports on smaller FAST units. This result showed future efforts to scale up the FAST sintering process while maintaining similar results will require careful attention to minimizing temperature gradients. This could potentially be achieved by reducing radiative heat loss during processing and/or optimizing the graphite die design and implementing heat spreaders in specific locations dependent on the host material.s thermal and electrical properties as well as the sample geometry.

Synthesis of Y1Ba2Cu3O(sub x) superconducting powders by intermediate phase reaction

NASA Technical Reports Server (NTRS)

Moore, C.; Fernandez, J. F.; Recio, P.; Duran, P.

1990-01-01

One of the more striking problems for the synthesis of the Y1Ba2Cu3Ox compound is the high-temperature decomposition of the BaCO3. This compound is present as raw material or as an intermediate compound in chemical processes such as amorphous citrate, coprecipitation oxalate, sol-gel process, acetate pyrolisis, etc. This fact makes difficult the total formation reaction of the Y1Ba2Cu3Ox phase and leads to the presence of undesirable phases such as the BaCuO2 phase, the 'green phase', Y2BaCuO5 and others. Here, a new procedure to overcome this difficulty is studied. The barium cation is previously combined with yttrium and/or copper to form intermediate compounds which can react between them to give Y1Ba2Cu3Ox. BaY2O4 and BaCu2O3 react according to the equation BaY2O4+3BaCu2O3 yields 2Y1Ba2Cu3Ox. BaY2O4 is a stable compound of the Y2O3-BaO system; BaCu2O3 is an intimate mixture of BaCuO2 and uncombined CuO. The reaction kinetics of these phases have been established between 860 and 920 C. The phase evolution has been determined. The crystal structure of the Y1Ba2Cu3Ox obtained powder was studied. According to the results obtained from the kinetics study the Y1Ba2Cu3Ox the synthesis was performed at temperatures of 910 to 920 C for short treatment times (1 to 2 hours). Pure Y1Ba2Cu3Ox was prepared, which develops orthorombic type I structure despite of the cooling cycle. Superconducting transition took place at 91 K. The sintering behavior and the superconducting properties of sintered samples were studied. Density, microstructure and electrical conductivity were measured. Sintering densities higher than 95 percent D(sub th) were attained at temperatures below 940 C. Relatively fine grained microstructure was observed, and little or no-liquid phase was detected.

Determining optimal operation parameters for reducing PCDD/F emissions (I-TEQ values) from the iron ore sintering process by using the Taguchi experimental design.

PubMed

Chen, Yu-Cheng; Tsai, Perng-Jy; Mou, Jin-Luh

2008-07-15

This study is the first one using the Taguchi experimental design to identify the optimal operating condition for reducing polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/ Fs) formations during the iron ore sintering process. Four operating parameters, including the water content (Wc; range = 6.0-7.0 wt %), suction pressure (Ps; range = 1000-1400 mmH2O), bed height (Hb; range = 500-600 mm), and type of hearth layer (including sinter, hematite, and limonite), were selected for conducting experiments in a pilot scale sinter pot to simulate various sintering operating conditions of a real-scale sinter plant We found that the resultant optimal combination (Wc = 6.5 wt%, Hb = 500 mm, Ps = 1000 mmH2O, and hearth layer = hematite) could decrease the emission factor of total PCDD/Fs (total EF(PCDD/Fs)) up to 62.8% by reference to the current operating condition of the real-scale sinter plant (Wc = 6.5 wt %, Hb = 550 mm, Ps = 1200 mmH2O, and hearth layer = sinter). Through the ANOVA analysis, we found that Wc was the most significant parameter in determining total EF(PCDD/Fs (accounting for 74.7% of the total contribution of the four selected parameters). The resultant optimal combination could also enhance slightly in both sinter productivity and sinter strength (30.3 t/m2/day and 72.4%, respectively) by reference to those obtained from the reference operating condition (29.9 t/m (2)/day and 72.2%, respectively). The above results further ensure the applicability of the obtained optimal combination for the real-scale sinter production without interfering its sinter productivity and sinter strength.

Microstructure and Mechanical Properties of Graphene-Reinforced Titanium Matrix/Nano-Hydroxyapatite Nanocomposites

PubMed Central

Li, Feng; Shao, Zhenyi; Zhu, Degui; Zhu, Minhao

2018-01-01

Biomaterial composites made of titanium and hydroxyapatite (HA) powder are among the most important biomedicalmaterials due to their good mechanical properties and biocompatibility. In this work, graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites were prepared by vacuum hot-pressing sintering. The microstructure and mechanical properties of graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were systematically investigated. Microstructures of the nanocomposites were examined by X-ray diffraction (XRD), back scattered electron imaging (BSE), scanning electron microscope (SEM) equipped with energy dispersive spectrometer (EDS), electron probe microanalyzer (EPMA), and transmission electron microscope (TEM). The mechanical properties were determined from microhardness, shear strength, and compressive strength. Results showed that during the high-temperature sintering process, complex chemical reactions occurred, resulting in new phases of nucleation such as Ca3(PO4)2, TixPy, and Ti3O.The new phases, which easily dropped off under the action of external force, could hinder the densification of sintering and increase the brittleness of the nanocomposites. Results demonstrated that graphene had an impact on the microstructure and mechanical properties of the nanocomposites. Based on the mechanical properties and microstructure of the nanocomposites, the strengthening and fracture mechanisms of the graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were analyzed. PMID:29659504

Microstructure and Mechanical Properties of Graphene-Reinforced Titanium Matrix/Nano-Hydroxyapatite Nanocomposites.

PubMed

Li, Feng; Jiang, Xiaosong; Shao, Zhenyi; Zhu, Degui; Zhu, Minhao

2018-04-16

Biomaterial composites made of titanium and hydroxyapatite (HA) powder are among the most important biomedicalmaterials due to their good mechanical properties and biocompatibility. In this work, graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites were prepared by vacuum hot-pressing sintering. The microstructure and mechanical properties of graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were systematically investigated. Microstructures of the nanocomposites were examined by X-ray diffraction (XRD), back scattered electron imaging (BSE), scanning electron microscope (SEM) equipped with energy dispersive spectrometer (EDS), electron probe microanalyzer (EPMA), and transmission electron microscope (TEM). The mechanical properties were determined from microhardness, shear strength, and compressive strength. Results showed that during the high-temperature sintering process, complex chemical reactions occurred, resulting in new phases of nucleation such as Ca₃(PO₄)₂, Ti x P y , and Ti₃O.The new phases, which easily dropped off under the action of external force, could hinder the densification of sintering and increase the brittleness of the nanocomposites. Results demonstrated that graphene had an impact on the microstructure and mechanical properties of the nanocomposites. Based on the mechanical properties and microstructure of the nanocomposites, the strengthening and fracture mechanisms of the graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were analyzed.

An experimental study on effect of coke ratio on SO2 and NOx emissions in sintering process

NASA Astrophysics Data System (ADS)

Wang, Hui; Zhang, Pu; Yang, Jingling

2018-02-01

By using the sinter cup experiment, the effects of different coke ratios of 0%, 25%, 50%, 75%, and 100% on the formation and total emissions of SO2 and NOx in the sintering process were studied with the Testo350 flue gas analyzer. The experimental results show that the emissions of SO2 and NOx are closely related to sintering process. With the increase of the coke proportion, the sintering temperature changes and the maximum peak time appears earlier. SO2 concentration has a bimodal distribution and NOx concentration has a triple peak. Besides, the both maximum peaks appear at the end of sintering. In addition, due to the increasing of the S and N contents in the fuel with the coke ratios from 0% to 100%, the amounts of SO2 and NOx emissions are raised respectively at 10.82 mg, 11.42 mg, 13.84 mg, 13.69 mg, 20.36 mg and 3.11 mg, 3.39 mg, 4.44 mg, 4.31 mg, 6.16 mg.

Solar Thermochemical Fuel Production via a Novel Low Pressure, Magnetically Stabilized, Non-volatile Iron Oxide Looping Process (University of Florida)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hahn, David W.

The UF Solar Fuels team has developed a modular reactor at the 10kW scale for the thermochemical conversion of H2O and CO2 to H2 and CO, respectively, using concentrated solar energy to drive high-temperature redox reactions. Various materials, including ferrites, doped and mixed metal ferrites, and ceria, were investigated and reported on. Ceria was chosen as the reactive material, with thermogravimetric and bench-scale analysis concurring with literature review and pointing towards reasonable kinetics and stability at temperatures on the order of 1500 °C. A combined radiation, conduction, and species reaction/mass transport model was developed, utilizing Monte Carlo ray tracing, Latticemore » Boltzmann, and random walk particle tracking for the respective components to direct development and optimization of the reactor. With experimental data used for reaction rates, the model showed a path to efficiencies >20%, which could be market competitive with current PV-hydrolysis hydrogen generation systems. Economic analysis of a larger-scale plant (100kW modular system with cost performed at 500 modules) has been performed, assuming 0.5% and 10% internal rate of return. Without compression costs, H2 production cost using this is technology at $12/kg H2 and $17/kg H2 for realized efficiencies of 20% and 15%, respectively. An interaction of ceria and alumina, with the formation of CeAlO3 occurring at ~1700 °C, had been reported in the literature, but the UF Solar Fuels team observed and reported on it at a large scale, confirming its presence as an engineering consideration when working ceria and alumina at extreme temperatures. CeAlO3 could be being produced at lower temperatures due to the oxidation and reducing environments or due to local hotspots in the reactor. A solar thermogravimeter was developed, to take advantage of the high heating rates available at the UF Solar Simulator Facility to allow investigation of species evolution and material stability in extreme heating rate scenarios. A novel flash-boiling centrifugal-separation steam generator was developed to provide inexpensive, identical steam flows to modular systems, using water-metering and generating the steam for each flow in separate chambers. Several novel methods of reactant material preparation were developed, including: • Sacrificial Pore Formation - Uses a component, such as graphite, designed to be carried away in gaseous form at some point in the preparation process to aid in the formation of pathways and porosity for the enhancement of fluid flow and radiative heat transport at elevated temperatures. • Particle stacking and sintering – Using material that has been pre-sintered (at the temperatures expected for reaction) and mechanically broken apart. The particles are then separated by size to allow the process to be repeated several times with a given particle size range. The resulting stacked and sintered structure maintains micro- to millimeter size pore structure for fluid transport at temperatures that previously demonstrated some contraction or collapse of the reactive material due to porosity reduction due to sintering. In addition, novel seals utilizing graphite and boron nitride particle filler as an internally compressed seal were developed. These seals allow sealing of a ceramic Efficiencies of >4% solar-to-fuel were demonstrated, which at the time of demonstration was the highest yet reported. Hydrogen and CO production rates targets that averaged ~3 cc/gram of reactive material were achieved.« less

Development of Dielectric Material with Ceramic Matrix Composite (CMC) Produced from Kaolinite and CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yin, Wong Swee; Hassan, Jumiah; Hashim, Mansor

Ceramic matrix composites (CMC) combine reinforcing ceramic phases, CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) with a ceramic matrix, kaolinite to create materials with new and superior properties. 10% and 20% CCTO were prepared by using a conventional solid state reaction method. CMC samples were pre-sintered at 800 deg. C and sintered at 1000 deg. C. The dielectric properties of samples were measured using HP 4192A LF Impedance Analyzer. Microstructures of the samples were observed using an optical microscope. XRD was used to determine the crystalline structure of the samples. The AFM showed the morphology of the samples. The results showed thatmore » the dielectric constant and dielectric loss factor of both samples are frequency dependent. At 10 Hz, the dielectric constant is 10{sup 11} for both samples. The CMC samples were independent with temperature with low dielectric constant in the frequency range of 10{sup 4}-10{sup 6} Hz. Since the CMC samples consist of different amount of kaolinite, so each sample exhibit different defect mechanism. Different reaction may occur for different composition of material. The effects of processing conditions on the microstructure and electrical properties of CMC are also discussed.« less

Fabrication and luminescent properties of La2O2S:Eu3+ translucent ceramic by pressureless reaction sintering

NASA Astrophysics Data System (ADS)

Lian, Jingbao; Wang, Bingxin; Liang, Ping; Liu, Feng; Wang, Xuejiao

2014-04-01

La2O2S:Eu3+ translucent ceramic (LOS:Eu) was fabricated by pressureless reaction sintering method. It is found that the (La, Eu)2(OH)4SO4ṡ2H2O precursor is synthesized by co-precipitation using commercially available La(NO3)3, Eu(NO3)3, (NH4)2SO4 and NH3ṡH2O as the starting materials. And this precursor can be converted into pure La2O2SO4:Eu3+ phosphor by calcination at 800 °C for 1 h in air, which is composed of a few small needle agglomerated particles. Then the La2O2SO4:Eu3+ phosphor compact can be sintered into the LOS:Eu at 1500 °C for 2 h in the hybrid atmosphere of flowing hydrogen and argon. Under 387 nm UV light excitation, the LOS:Eu reveals a red light emission at 628 nm as the most prominent peak, which corresponds to the 5D0 → 7F2 transition of Eu3+ ions.

Durability characterization of ceramic materials for gas turbines

NASA Technical Reports Server (NTRS)

Carruthers, W. D.; Lindberg, L. J.

1987-01-01

The strength retention of ceramic materials during extended high-temperature cyclic exposure is critical to their widespread application in gas turbine engines. During a continuing NASA funded program initated in 1979, reaction bonded silicon nitride (RBSN), sintered silicon carbide (SSC), reaction sintered silicon carbide (RSSC), and sintered silicon nitride (SSN) materials were evaluated following simulated gas turbine engine exposures. Exposures were performed by cycling specimens five times per hour between a high velocity burner discharge and a rapid air quench. The retained flexural strengths were determined following up to 3500 hours of exposure at temperatures up to 1370 C. Post-exposure strengths have been correlated with fractography and surface examination using SEM. Results illustrate excellent strength retention of SSC materials after 3500 hours of exposure to 1370 C. At 1200 C, RBSN and RSSC also demonstrate significant strength retention. Although SSN materials typically suffer significant strength losses during exposures at 1200 C, a new composition, which has improved high-temperature strength, also shows improved durability. In the majority of the materials, strength loss is typically associated with flaw formation in the protective SiO2 layer.

Sintering mechanism of the CaF2 on hydroxyapatite by a 10.6-l microm CO2 laser.

PubMed

Wu, Cheng-Chei; Roan, Rong-Tai; Chen, Jeng-Huey

2002-01-01

Laser has been reported as a heat source for melting and re-crystallization. Occurring at about 1100 degrees C, the melting of surface dental enamel along with re-crystallization might have an assistant role in the therapy of hypersensitive tooth, apical sealing of endodontic surgery in dentistry, preventive dentistry for pit and fissure sealing, and fluoridation. For laser to be accepted in clinical applications, it is desired that, studies must show the incorporation of CaF(2) into hydroxyapatite could reduce the sintering temperature for the sake of safety. In this study, the Sharplan 20XJ CO(2) laser with 10.6- microm wavelength was set under the following parameters: power, 5 W; repetitive mode, 0.1 second; beam, focused. Fluorite was added to hydroxyapatite as a synthetic compound to lower the sintering temperature. Human dental enamel without caries was used for in vitro sintering test. Scanning electron microscopy (SEM), X-ray diffractometer (XRD), Fourier transforming infrared spectroscopy (FTIR), and differential thermal analysis/thermogravimetric analysis (DAT/TGA) were used for the investigation of sintering mechanism of CaF(2). Fusion between hexagonal shape crystals and cubic shape crystals (CaF(2)) were observed under SEM study. Hexagonal shape crystals indicated the formation of fluorapatite under XRD analysis. Under FTIR study, we examined reductions of water (3445 cm(-1)) and hydroxyl bands (3567 and 627 cm(-1)) in irradiated compounds. From the DTA pattern of synthetic compound, it showed the endothermic reaction reaching its peak point around 1180 +/- 20 degrees C. It was attributed to the phase transformation and/or initial melting. In this study, we proposed the interrelationship of the eutectics between initiator (CaF(2)) and the reaction product (calcium hydroxide) that reduced the sintering temperature. It appeared that the co-eutectics interacted to reduce the sintering temperature of hydroxyapatite below 800 degrees C and that the key eutectic was calcium hydroxide. The clinical feasibility of the melting and re-crystallization of hydroxyapatite under 10.6-microm CO(2) laser would be therefore enhanced. Copyright 2002 Wiley-Liss, Inc.

Isothermal reduction kinetics and mineral phase of chromium-bearing vanadium-titanium sinter reduced with CO gas at 873-1273 K

NASA Astrophysics Data System (ADS)

Yang, Song-tao; Zhou, Mi; Jiang, Tao; Xue, Xiang-xin

2018-02-01

Reduction of chromium-bearing vanadium-titanium sinter (CVTS) was studied under simulated conditions of a blast furnace, and thermodynamics and kinetics were theoretically analyzed. Reduction kinetics of CVTS at different temperatures was evaluated using a shrinking unreacted core model. The microstructure, mineral phase, and variation of the sinter during reduction were observed by X-ray diffraction, scanning electron microscopy, and metallographic microscopy. Results indicate that porosity of CVTS increased with temperature. Meanwhile, the reduction degree of the sinter improved with the reduction rate. Reduction of the sinter was controlled by a chemical reaction at the initial stage and inner diffusion at the final stage. Activation energies measured 29.22-99.69 kJ/mol. Phase transformations in CVTS reduction are as follows: Fe2O3→Fe3O4→FeO→Fe; Fe2TiO5→Fe2TiO4→FeTiO3; FeO·V2O3→V2O3; FeO·Cr2O3→Cr2O3.

Study of sintering behavior of vapor forms of 1-octanethiol coated copper nanoparticles for application to ink-jet printing technology.

PubMed

Kwon, Jinhyeong; Park, Shinyoung; Haque, Md Mominul; Kim, Young-Seok; Lee, Caroline Sunyong

2012-04-01

Sub-50 nm copper nanoparticles coated with sub-5 nm 1-octanethiol layer for oxidation inhibition were examined to confirm the 1-octanethiol removal temperature as the sub-50 nm copper nanoparticles are sintered. As a result, 1-octanethiol Self-Assembled Multi-layers (SAMs) on sub-50 nm copper nanoparticles were successfully removed before sintering of copper nanoparticles so that a high density of copper line could be obtained. Finally, the line resistivity was measured and compared to verify the effect of sintering in different atmospheres. As a result, electrical resistivity of the copper pattern sintered in hydrogen atmosphere was measured at 6.96 x 10(-6) ohm-cm whereas that of the copper pattern sintered in mixed gas atmosphere was measured at 2.62 x 10(-5) ohm-cm. Thus, sintering of copper patterns was successfully done to show low electrical resistivity values. Moreover, removal of 1-octanethiol coating after sintering process was confirmed using X-ray photoelectron spectroscopy (XPS) analysis. By showing no sulfur content, XPS results indicate that 1-octanethiol is completely removed. Therefore, the vapor form of 1-octanethiol coating layers can be safely used as an oxidation inhibition layer for low temperature sintering processes and ink-jet applications.

Vacuum Pressureless Sintering of Ti-6Al-4V Alloy with Full Densification and Forged-Like Mechanical Properties

NASA Astrophysics Data System (ADS)

Zhang, Ce; Lu, Boxin; Wang, Haiying; Guo, Zhimeng; Paley, Vladislav; Volinsky, Alex A.

2018-01-01

Ti-6Al-4V ingots with a nearly 100% density, fine and homogeneous basket-weave microstructure, and better comprehensive mechanical properties (UTS = 935 MPa, Y.S. = 865 MPa, El. = 15.8%), have been manufactured by vacuum pressureless sintering of blended elemental powders. Coarse TiH2 powder, Al powder (2, 20 μm), V powder, and Al-V master alloy powder were used as raw materials to produce different powder mixtures ( D 50 = 10 μm). Then, the compacts made by cold isostatic pressing were consolidated by different sintering curves. A detailed investigation of different as-sintered samples revealed that a higher density can be obtained by generating transient molten Al in the sintering process. Coarse Al powder and a rapid heating rate under the melting point of Al contribute to molten Al formation. The presence of temporary liquid phase changes the sintering mechanism, accelerating the sintering neck formation, improving sinterability of the powder mixtures. Density of 99.5% was achieved at 1150 °C, which is markedly lower than the sintering temperatures reported for conventional blended elemental powder metallurgy routes. In addition, low interstitial content, especially for oxygen (0.17 wt.%), is obtained by strict process control.

Preparation of Porous Stainless Steel Hollow-Fibers through Multi-Modal Particle Size Sintering towards Pore Engineering

PubMed Central

Allioux, Francois-Marie; Etxeberria Benavides, Miren

2017-01-01

The sintering of metal powders is an efficient and versatile technique to fabricate porous metal elements such as filters, diffusers, and membranes. Neck formation between particles is, however, critical to tune the porosity and optimize mass transfer in order to minimize the densification process. In this work, macro-porous stainless steel (SS) hollow-fibers (HFs) were fabricated by the extrusion and sintering of a dope comprised, for the first time, of a bimodal mixture of SS powders. The SS particles of different sizes and shapes were mixed to increase the neck formation between the particles and control the densification process of the structure during sintering. The sintered HFs from particles of two different sizes were shown to be more mechanically stable at lower sintering temperature due to the increased neck area of the small particles sintered to the large ones. In addition, the sintered HFs made from particles of 10 and 44 μm showed a smaller average pore size (<1 μm) as compared to the micron-size pores of sintered HFs made from particles of 10 μm only and those of 10 and 20 μm. The novel HFs could be used in a range of applications, from filtration modules to electrochemical membrane reactors. PMID:28777352

Reaction of Unalloyed and Cr-Mo Alloyed Steels with Nitrogen from the Sintering Atmosphere

NASA Astrophysics Data System (ADS)

Dlapka, Magdalena; Gierl-Mayer, Christian; Calderon, Raquel de Oro; Danninger, Herbert; Bengtsson, Sven; Dudrova, Eva

2016-12-01

Nitrogen is usually regarded as an inert sintering atmosphere for PM steels; however, this cannot be taken for granted in particular for steels alloyed with nitride forming elements. Among those elements, chromium has become more and more important as an alloying element in sintered low alloy structural steels in the last decade due to the moderate alloying cost and the excellent mechanical properties obtainable, in particular when sinter hardening is applied. The high affinity of Cr to oxygen and the possible ways to overcome related problems have been the subject of numerous studies, while the fact that chromium is also a fairly strong nitride forming element has largely been neglected at least for low alloy steel grades, although frequently used materials like steels from Cr and Cr-Mo prealloyed powders are commonly sintered in atmospheres consisting mainly of nitrogen. In the present study, nitrogen pickup during sintering at different temperatures and for varying times has been studied for Cr-Mo prealloyed steel grades as well as for unalloyed carbon steel. Also the effect of the cooling rate and its influence on the properties, of the microstructure and the composition have been investigated. It showed that the main nitrogen uptake occurs not during isothermal sintering but rather during cooling. It could be demonstrated that a critical temperature range exists within which the investigated CrM-based steel is particularly sensitive to nitrogen pickup.

Ultra-low temperature sintering of Cu@Ag core-shell nanoparticle paste by ultrasonic in air for high-temperature power device packaging.

PubMed

Ji, Hongjun; Zhou, Junbo; Liang, Meng; Lu, Huajun; Li, Mingyu

2018-03-01

Sintering of low-cost Cu nanoparticles (NPs) for interconnection of chips to substrate at low temperature and in atmosphere conditions is difficult because they are prone to oxidation, but dramatically required in semiconductor industry. In the present work, we successfully synthesized Cu@Ag NPs paste, and they were successfully applied for joining Cu/Cu@Ag NPs paste/Cu firstly in air by the ultrasonic-assisted sintering (UAS) at a temperature of as low as 160 °C. Their sintered microstructures featuring with dense and crystallized cells are completely different from the traditional thermo-compression sintering (TCS). The optimized shear strength of the joints reached to 54.27 MPa, exhibiting one order of magnitude higher than TCS at the same temperature (180 °C) under the UAS. This ultra-low sintering temperature and high performance of the sintered joints were ascribed to ultrasonic effects. The ultrasonic vibrations have distinct effects on the metallurgical reactions of the joints, resulting in the contact and growth of Cu core and the stripping and connection of Ag shell, which contributes to the high shear strength. Thus, the UAS of Cu@Ag NPs paste has a great potential to be applied for high-temperature power device packaging. Copyright © 2017 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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.

Selective laser sintering: A qualitative and objective approach

NASA Astrophysics Data System (ADS)

Kumar, Sanjay

2003-10-01

This article presents an overview of selective laser sintering (SLS) work as reported in various journals and proceedings. Selective laser sintering was first done mainly on polymers and nylon to create prototypes for audio-visual help and fit-to-form tests. Gradually it was expanded to include metals and alloys to manufacture functional prototypes and develop rapid tooling. The growth gained momentum with the entry of commercial entities such as DTM Corporation and EOS GmbH Electro Optical Systems. Computational modeling has been used to understand the SLS process, optimize the process parameters, and enhance the efficiency of the sintering machine.

Influence of Hydrogen on Atomized Titanium Powders Sintering

NASA Astrophysics Data System (ADS)

Senkevich, K. S.

2018-07-01

The aim of this work is to study the effect of hydrogen reversible alloying (thermohydrogen processing, THP) on low-temperature sintering of atomized titanium powders. It is stated that alloying with 0.2 to 0.8 wt pct of hydrogen beneficially affects titanium powders sintering. The effect is caused by phase transformations occurring upon hydrogen saturation of powders and dehydrogenation, which substantially intensifies sintering at temperatures from 800 °C to 900 °C. The role of certain THP stages (sintering in hydrogenated state and upon dehydrogenation) on formation of sintered contacts in porous materials is shown.

Influence of Hydrogen on Atomized Titanium Powders Sintering

NASA Astrophysics Data System (ADS)

Senkevich, K. S.

2018-05-01

The aim of this work is to study the effect of hydrogen reversible alloying (thermohydrogen processing, THP) on low-temperature sintering of atomized titanium powders. It is stated that alloying with 0.2 to 0.8 wt pct of hydrogen beneficially affects titanium powders sintering. The effect is caused by phase transformations occurring upon hydrogen saturation of powders and dehydrogenation, which substantially intensifies sintering at temperatures from 800 °C to 900 °C. The role of certain THP stages (sintering in hydrogenated state and upon dehydrogenation) on formation of sintered contacts in porous materials is shown.

Improvement of mechanical strength of sintered Mo alloyed steel by optimization of sintering and cold-forging processes with densification

NASA Astrophysics Data System (ADS)

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 without surface machining.

Characteristics of iron ore sinter with EFB addition

NASA Astrophysics Data System (ADS)

Purwanto, H.; Rozhan, A. N.; Mohamad, A. S.; Zakiyuddin, A.

2018-04-01

Utilization of EFB-derived biochar in sintering of iron ore has been conducted in this work with regards to the porosity of iron sinter. EFB has been heated up in argon atmosphere to 450°C in order to produce biochar. In the present work, the sintering process was conducted at 1150°C with variations of biochar content from 5% to 10%. In this case, the apparent density for iron sinter shows significant decrease as the biochar addition increase. The porosity of iron sinter showed a gradual increment from 5% to 7.5% and escalated at 10% biochar content. The results of porosity and apparent density were in line with the micrograph of iron sinter.

Production of superconductor/carbon bicomponent fibers

NASA Technical Reports Server (NTRS)

Wise, S. A.; Fain, C. C.; Leigh, H. D.; Sherrill, M.

1990-01-01

Certain materials are unable to be drawn or spun into fiber form due to their improper melting characteristics or brittleness. However, fibrous samples of such materials are often necessary for the fabrication of intricate shapes and composites. In response to this problem, a unique process, referred to as the piggyback process, was developed to prepare fibrous samples of a variety of nonspinnable ceramics. In this technique, specially produced C-shaped carbon fibers serve as micromolds to hold the desired materials prior to sintering. Depending on the sintering atmosphere used, bicomponent or single component fibers result. While much has been demonstrated worldwide concerning the YBa2Cu3O(7-x) superconductor, fabrication into unique forms has proven quite difficult. However, a variety of intricate shapes are necessary for rapid commercialization of the superconducting materials. The potential for producing fibrous samples of the YBa2Cu3O(7-x) compound by the piggyback process is being investigated. Various organic and acrylic materials were investigated to determine suspending ability, reactivity with the YBa2Cu3O(7-x) compound during long term storage, and burn out characteristics. While many questions were answered with respect to the interfacial reactions between YBa2Cu3O(7-x) and carbon, much work is still necessary to improve the quality of the sintered material if the fibers produced are to be incorporated into useful composites or cables. Additional research is necessary to evaluate quality of the barrier layer during long soakings at the peak temperature; adjust the firing schedule to avoid microcracking and improve densification; and increase the solids loading in the superconductive suspension to decrease porosity.

Temperature Field Simulation of Powder Sintering Process with ANSYS

NASA Astrophysics Data System (ADS)

He, Hongxiu; Wang, Jun; Li, Shuting; Chen, Zhilong; Sun, Jinfeng; You, Ying

2018-03-01

Aiming at the “spheroidization phenomenon” in the laser sintering of metal powder and other quality problems of the forming parts due to the thermal effect, the finite element model of the three-dimensional transient metal powder was established by using the atomized iron powder as the research object. The simulation of the mobile heat source was realized by means of parametric design. The distribution of the temperature field during the sintering process under different laser power and different spot sizes was simulated by ANSYS software under the condition of fully considering the influence of heat conduction, thermal convection, thermal radiation and thermophysical parameters. The influence of these factors on the actual sintering process was also analyzed, which provides an effective way for forming quality control.

Numerical study of the process parameters in spark plasma sintering (sps)

NASA Astrophysics Data System (ADS)

Chowdhury, Redwan Jahid

Spark plasma sintering (SPS) is one of the most widely used sintering techniques that utilizes pulsed direct current together with uniaxial pressure to consolidate a wide variety of materials. The unique mechanisms of SPS enable it to sinter powder compacts at a lower temperature and in a shorter time than the conventional hot pressing, hot isostatic pressing and vacuum sintering process. One of the limitations of SPS is the presence of temperature gradients inside the sample, which could result in non-uniform physical and microstructural properties. Detailed study of the temperature and current distributions inside the sintered sample is necessary to minimize the temperature gradients and achieve desired properties. In the present study, a coupled thermal-electric model was developed using finite element codes in ABAQUS software to investigate the temperature and current distributions inside the conductive and non-conductive samples. An integrated experimental-numerical methodology was implemented to determine the system contact resistances accurately. The developed sintering model was validated by a series of experiments, which showed good agreements with simulation results. The temperature distribution inside the sample depends on some process parameters such as sample and tool geometry, punch and die position, applied current and thermal insulation around the die. The role of these parameters on sample temperature distribution was systematically analyzed. The findings of this research could prove very useful for the reliable production of large size sintered samples with controlled and tailored properties.

Effect of Alloying Type and Lean Sintering Atmosphere on the Performance of PM Components

NASA Astrophysics Data System (ADS)

Sundaram, M. Vattur; Shvab, R.; Millot, S.; Hryha, E.; Nyborg, L.

2017-12-01

In order to be cost effective and to meet increasing performance demands, powder metallurgy steel components require continuous improvement in terms of materials and process development. This study demonstrates the feasibility of manufacturing structural components using two different alloys systems, i.e. lean Cr-prealloyed and diffusion bonded water atomised powders with different processing conditions. The components were sintered at two different temperatures, i.e. 1120 and 1250 °C for 30 minutes in three different atmospheres: vacuum, N2- 10%H2 atmosphere as well as lean N2-5%H2-0.5%CO-(0.1-0.4)%CH4 sintering atmosphere. Components after sintering were further processed by either low pressure carburizing, sinterhardening or case hardening. All trials were performed in the industrial furnaces to simulate the actual production of the components. Microstructure, fractography, apparent and micro hardness analyses were performed close to the surface and in the middle of the sample to characterize the degree of sintering (temperature and atmosphere) and the effect of heat treatment. In all cases, components possess mostly martensitic microstructure with a few bainitic regions. The fracture surface shows well developed sinter necks. Inter- and trans-granular ductile and cleavage fracture modes are dominant and their fraction is determined by the alloy and processing route.

Effect of sintering temperature on the microstructure, electrical and magnetic properties of Zn0.98 Mn0.02O material

NASA Astrophysics Data System (ADS)

Sebayang, K.; Aryanto, D.; Simbolon, S.; Kurniawan, C.; Hulu, S. F.; Sudiro, T.; Ginting, M.; Sebayang, P.

2018-02-01

Zn0.98Mn0.02O material was synthesized from ZnO and MnO2 powders using solid state reaction method. The microstructure, electrical and magnetic properties of Zn0.98Mn0.02O were studied as a function of sintering temperature. The X-ray diffraction analysis indicates that the main phase of synthesized sample is composed of hexagonal wurtzite ZnO phase. While the secondary phase of ZnMnO3 were found at the sintering temperature of 700°C and 900°C. The electrical properties measurement of Zn0.98Mn0.02O sample revealed that the resistivity and the dielectric constant of samples increase with the increase of sintering temperature. The ferromagnetic properties at room temperature were observed in the Zn0.98Mn0.02O samples sintered at 500°C and 700°C. It also found that the increase in sintering temperature leads to a tendency toward the changes in the magnetic properties into paramagnetic. The presence of ZnMnO3 secondary phases in Zn0.98Mn0.02O system is believed to be a factor that affects the decrease of the electrical and magnetic properties of the sample.

Consolidation & Factors Influencing Sintering Process in Polymer Powder Based Additive Manufacturing

NASA Astrophysics Data System (ADS)

Sagar, M. B.; Elangovan, K.

2017-08-01

Additive Manufacturing (AM) is two decade old technology; where parts are build layer manufacturing method directly from a CAD template. Over the years, AM techniques changes the future way of part fabrication with enhanced intricacy and custom-made features are aimed. Commercially polymers, metals, ceramic and metal-polymer composites are in practice where polymers enhanced the expectations in AM and are considered as a kind of next industrial revolution. Growing trend in polymer application motivated to study their feasibility and properties. Laser sintering, Heat sintering and Inhibition sintering are the most successful AM techniques for polymers but having least application. The presentation gives up selective sintering of powder polymers and listed commercially available polymer materials. Important significant factors for effective processing and analytical approaches to access them are discussed.

Processing, characterization, and in vitro/in vivo evaluations of powder metallurgy processed Ti-13Nb-13Zr alloys.

PubMed

Bottino, Marco C; Coelho, Paulo G; Henriques, Vinicius A R; Higa, Olga Z; Bressiani, Ana H A; Bressiani, José C

2009-03-01

This article presents details of processing, characterization and in vitro as well as in vivo evaluations of powder metallurgy processed Ti-13Nb-13Zr samples with different levels of porosity. Sintered samples were characterized for density, crystalline phases (XRD), and microstructure (SEM and EDX). Samples sintered at 1000 degrees C showed the highest porosity level ( approximately 30%), featuring open and interconnected pores ranging from 50 to 100 mum in diameter but incomplete densification. In contrast, samples sintered at 1300 and 1500 degrees C demonstrated high densification with 10% porosity level distributed in a homogeneous microstructure. The different sintering conditions used in this study demonstrated a coherent trend that is increase in temperature lead to higher sample densification, even though densification represents a drawback for bone ingrowth. Cytotoxicity tests did not reveal any toxic effects of the starting and processed materials on surviving cell percentage. After an 8-week healing period in rabbit tibias, the implants were retrieved, processed for nondecalcified histological evaluation, and then assessed by backscattered electron images (BSEI-SEM) and EDX. Bone growth into the microstructure was observed only in samples sintered at 1000 degrees C. Overall, a close relation between newly formed bone and all processed samples was observed. (c) 2008 Wiley Periodicals, Inc.

A sinter-resistant catalyst using an alumina support recycled from AlP fumigation residue: trash to treasure.

PubMed

Dong, Jinshi; Wang, Jun; Wang, Jianqiang; Cheng, Guanghao; Huang, Tianming; Shen, Meiqing

2018-05-07

Sintering is a long-standing issue especially in high temperature catalytic applications. In this paper, we report an effective method to slow down metal particle migration and coalescence (PMC) by using a thermally stable alumina support. Noteworthily, the alumina sample was developed from AlP fumigation residue, which is a very dangerous substance for living creatures and environment protection. By optimizing the heated hydrolysis and ball-milling conditions, we recycled a phosphate-stabilized alumina material that retained a 117 m 2 g -1 surface area after 1050 °C hydrothermal aging. The catalyst using this newly developed alumina support had Pd dispersion 1.7 times higher than that using a commercial alumina support after aging. The kinetics and XPS experiments showed that phosphate neither participated in the catalytic reaction process nor changed the active sites. This catalyst also exhibited extraordinary water tolerance and durability, making it a promising material in automotive exhaust purification and other catalytic applications.

Effect of Germanium on the TiO2 Photoanode for Dye Sensitized Solar Cell Applications. A Potential Sintering Aid

NASA Astrophysics Data System (ADS)

Ahmad, M. S.; Pandey, AK; Rahim, N. A.

2018-05-01

Anatase titanium-germanium (TiO2-Ge) nanocomposite has been prepared by using colloidal suspension process and investigated for photoanode to be used in dye sensitized solar cell. Ge possesses lower band gap energy compared to TiO2 and has the capability to absorb infrared region of solar spectrum. Its remarkable absorption and good electron transfer ability due to lower band gap energy makes it a potential candidate material in the field of DSSCs to counter important disadvantages such as high probability of electron recombination reactions and absorption of small region (UV region) of solar spectrum. Another advantage is its low sintering temperature which proved to be an added advantage to increase inter-particle contact which in turn leads to improved electron transfer. Scanning electron microscopy (SEM), uv-vis spectroscopy and electron impedance spectroscopy (EIS) have been employed to evaluate the effect of Ge on TiO2photoanode.

Effects of particle packing on the sintered microstructure

NASA Astrophysics Data System (ADS)

Barringer, E. A.; Bowen, H. K.

1988-04-01

The sintering process is shown to be critically dependent on particle-packing density and porosity uniformity. Sintering experiments were conducted on compacts consisting of monodisperse, spherical TiO2 particles. Densification kinetics and microstructure evolution for two initial packing densities, 55% and 69% of theoretical, were investigated. The lower-density compacts sintered rapidly to theoretical density, yet improved particle-packing density and uniformity significantly enhanced densification.

Concentrated solar energy used for sintering magnesium titanates for electronic applications

NASA Astrophysics Data System (ADS)

Apostol, Irina; Rodríguez, Jose; Cañadas, Inmaculada; Galindo, Jose; Mendez, Senen Lanceros; de Abreu Martins, Pedro Libȃnio; Cunha, Luis; Saravanan, Kandasamy Venkata

2018-04-01

Solar energy is an important renewable source of energy with many advantages: it is unlimited, clean and free. The main objective of this work was to sinter magnesium titanate ceramics in a solar furnace using concentrated solar energy, which is a novel and original process. The direct conversion of solar power into high temperature makes this process simple, feasible and ecologically viable/environmentally sustainable. We performed the solar sintering experiments at Plataforma Solar de Almeria-CIEMAT, Spain. This process takes place in a vertical axis solar furnace (SF5-5 kW) hosting a mobile flat mirror heliostat, a fixed parabolic mirror concentrator, an attenuator and a test table the concentrator focus. We sintered (MgO)0.63(TiO2)0.37, (MgO)0.49(TiO2)0.51, (MgO)0.50(TiO2)0.50 ceramics samples in air at about 1100 °C for a duration of 16 min, 1 h, 2 h and 3 h in the solar furnace. The MgO/TiO2 ratio and the dwell time was varied in order to obtain phase pure MgTiO3 ceramic. We obtained a pure MgTiO3 geikielite phase by solar sintering of (MgO)0.63(TiO2)0.37 samples at 1100 °C (16 min-3 h). Samples of (MgO)0.63(TiO2)0.37, solar sintered at 1100 °C for 3 h, resulted in well-sintered, non-porous samples with good density (3.46 g/cm3). The sintered samples were analyzed by XRD for phase determination. The grain and surface morphology was observed using SEM. Electrical measurements were carried out on solar sintered samples. The effect of processing parameters on microstructure and dielectric properties were investigated and is presented.

Assessing Effects of Oxidizer Characteristics on Composite Reaction Kinetics

DTIC Science & Technology

2013-12-01

in its spark gap is ionized and creates conductive plasma allowing current flow to the EBW. The EBW is a type of detonator which utilizes shockwaves...flow rate of 70 mL min-1 for the remainder of the cycle. Sintering can occur during heating and melting, ultimately affecting heat transfer in the...argon at a flow rate of 70 mL min-1 for the remainder of the cycle. Sintering can occur during heating and melting, ultimately affecting heat transfer

Studies of reaction geometry in oxidation and reduction of the alkaline silver electrode

NASA Technical Reports Server (NTRS)

Butler, E. A.; Blackham, A. U.

1971-01-01

Two methods of surface area estimations of sintered silver electrodes have given roughness factors of 58 and 81. One method is based on constant current oxidation, the other is based on potentiostatic oxidation. Examination of both wire and sintered silver electrodes via scanning electron microscopy at various stages of oxidation have shown that important structural features are mounds of oxide. In potentiostatic oxidations these appear to form on sites instantaneously nucleated while in constant current oxidations progressive nucleation is indicated.

Copper Chloride Cathode For Liquid-Sodium Cell

NASA Technical Reports Server (NTRS)

Bugga, Ratnakumar V.; Distefano, Salvador; Nagasubramanian, Ganesan; Bankston, Clyde P.

1990-01-01

Rechargeable liquid-sodium cell with copper chloride cathode offers substantial increase in energy density over cells made with other cathode materials. Unit has theoretical maximum energy density of 1135 W.h/kg. Generates electricity by electrochemical reaction of molten sodium and solid copper chloride immersed in molten electrolyte, sodium tetrachloroaluminate at temperature of equal to or greater than 200 degrees C. Wall of alumina tube separates molten electrolyte from molten sodium anode. Copper chloride cathode embedded in pores of sintered nickel cylinder or directly sintered.

[Influence on microstructure of dental zirconia ceramics prepared by two-step sintering].

PubMed

Jian, Chao; Li, Ning; Wu, Zhikai; Teng, Jing; Yan, Jiazhen

2013-10-01

To investigate the microstructure of dental zirconia ceramics prepared by two-step sintering. Nanostructured zirconia powder was dry compacted, cold isostatic pressed, and pre-sintered. The pre-sintered discs were cut processed into samples. Conventional sintering, single-step sintering, and two-step sintering were carried out, and density and grain size of the samples were measured. Afterward, T1 and/or T2 of two-step sintering ranges were measured. Effects on microstructure of different routes, which consisted of two-step sintering and conventional sintering were discussed. The influence of T1 and/or T2 on density and grain size were analyzed as well. The range of T1 was between 1450 degrees C and 1550 degrees C, and the range of T2 was between 1250 degrees C and 1350 degrees C. Compared with conventional sintering, finer microstructure of higher density and smaller grain could be obtained by two-step sintering. Grain growth was dependent on T1, whereas density was not much related with T1. However, density was dependent on T2, and grain size was minimally influenced. Two-step sintering could ensure a sintering body with high density and small grain, which is good for optimizing the microstructure of dental zirconia ceramics.

Infiltration sintering properties of Ni-4B-4Si(wt.%) alloy powders

NASA Astrophysics Data System (ADS)

Yang, Q.; Zhang, X. C.; Wang, F. L.; Zou, J. T.

2018-01-01

The Ni-4B-4Si(wt.%) alloy powders were infiltrated into the nickel skeletons, the effects of sintering temperatures (1050-1150 °C) and skeletons (loose and compact nickel powders) on the microstructures and hardness of the sintered alloys were investigated. The Ni-B-Si alloy sintered at 1100 °C consisted of γ-Ni and Ni3B, and Si mainly solid soluted in the γ-Ni. The loose nickel powders favored to the infiltration of Ni-B-Si liquid alloy into the nickel skeletons, the sintered alloys exhibited dense microstructures and good interfacial bonding with Ni substrates. The interfacial hardness was equal to that of the sintered alloys and Ni substrates. Loose nickel powders ensured the density and interfacial bonding of the sintered alloys, the infiltration sintering process can be simplified and easily applied to practice.

Surface hardening of Al alloys through controlled ball-milling and sintering.

PubMed

Kim, Seek Hyeoun; Kim, Yong Jin; Ahn, Jung-Ho

2012-07-01

One of the drawbacks of aluminum and its alloys is the lack of proper heat-treatment for surface-hardening. In the present work, a new and simple method of hardening the surface of aluminum and its alloys was developed. Low-energy ball-milling using specific process control agents (PCAs) was employed, using subsequent sintering in a controlled atmosphere. The PCAs in the present work were very effective both for milling and the formation of hard nanocrystalline dispersoids during sintering. The residual oxygen in a sintering atmosphere also played an important role in the formation of AIN or Al-O-N dispersoids. Through the proper control of the processing atmosphere and PCAs, the hardness and thickness of the hardened layers could be adjusted. The results of the wear test showed that the present aluminum alloys can be effectively utilized as light-weight components with a good wear resistance. Furthermore, the present method involves a simple forming process of die-compaction and sintering.

A constitutive model and numerical simulation of sintering processes at macroscopic level

NASA Astrophysics Data System (ADS)

Wawrzyk, Krzysztof; Kowalczyk, Piotr; Nosewicz, Szymon; Rojek, Jerzy

2018-01-01

This paper presents modelling of both single and double-phase powder sintering processes at the macroscopic level. In particular, its constitutive formulation, numerical implementation and numerical tests are described. The macroscopic constitutive model is based on the assumption that the sintered material is a continuous medium. The parameters of the constitutive model for material under sintering are determined by simulation of sintering at the microscopic level using a micro-scale model. Numerical tests were carried out for a cylindrical specimen under hydrostatic and uniaxial pressure. Results of macroscopic analysis are compared against the microscopic model results. Moreover, numerical simulations are validated by comparison with experimental results. The simulations and preparation of the model are carried out by Abaqus FEA - a software for finite element analysis and computer-aided engineering. A mechanical model is defined by the user procedure "Vumat" which is developed by the first author in Fortran programming language. Modelling presented in the paper can be used to optimize and to better understand the process.

Porous Titanium Parts Fabricated by Sintering of TiH2 and Ti Powder Mixtures

NASA Astrophysics Data System (ADS)

Peng, Qin; Yang, Bin; Friedrich, Bernd

2018-01-01

A new simple powder metallurgy process by sintering TiH2 powders was used to manufacture porous Ti components. The effects of the processing parameters (pressure of cold isostatic pressing and sintering temperature) and the TiH2/Ti ratio in the powder mixtures on the impurities, the linear shrinkage and the pore properties (including overall and open porosities) were comprehensively determined. The addition of TiH2 as a reactant has been found beneficial for the synthesis of porous Ti components. The formation mechanisms of pores were demonstrated based on the dehydrogenation process of TiH2 during sintering, resulting in highest reactivity due to the "in statu nascendi" generation of the metal. In addition, the hardness and corrosion resistance of all the sintered samples were evaluated, related to the overall and open porosities. As a result, an optimal composition of Ti-40 wt.% TiH2 was defined, as its maximum open porosity was about 23%.

Numerical Study of the Features of Ti-Nb Alloy Crystallization during Selective Laser Sintering

NASA Astrophysics Data System (ADS)

Dmitriev, A. I.; Nikonov, A. Y.

2016-07-01

The demand for implants with individual shape requires the development of new methods and approaches to their production. The obvious advantages of additive technologies and selective laser sintering are the capabilities to form both the external shape of the product and its internal structure. Recently appeared and attractive from the perspective of biomechanical compatibility are beta alloys of titanium-niobium that have similar mechanical properties to those of cortical bone. This paper studies the processes occurring at different stages of laser sintering using computer simulation on atomic scale. The effect of cooling rate on the resulting crystal structure of Ti-Nb alloy was analysed. Also, the dependence of tensile strength of sintered particles on heating time and cooling rate was studied. It was shown that the main parameter, which determines the adhesive properties of sintered particles, is the contact area obtained during sintering process. The simulation results can both help defining the technological parameters of the process to provide the desired mechanical properties of the resulting products and serve as a necessary basis for calculations on large scale levels in order to study the behaviour of actually used implants.

The recovery of Zn and Pb and the manufacture of lightweight bricks from zinc smelting slag and clay.

PubMed

Hu, Huiping; Deng, Qiufeng; Li, Chao; Xie, Yue; Dong, Zeqin; Zhang, Wei

2014-04-30

Novel lightweight bricks have been produced by sintering mixes of zinc smelting slag and clay. A two-stage sintered process has been proposed to recovery of Zn and Pb and reutilization of the zinc smelting slag. In the first stage of the process, called reduction and volatilization procedure, zinc and lead were reduced by the carbon contained in the zinc smelting slag and volatilized into the dust, and the dust can be used as a secondary zinc resource. In the second stage of the process, called oxidation sintering procedure, a lightweight brick was produced. Samples containing up to 60 wt.% zinc smelting slag and 40 wt.% kaolin clay were reduced at 1050°C for 6h, and then sintered at 1050°C for 4h. The recoveries of Zn and Pb from the brick are 94.5 ± 0.6% and 97.6 ± 0.2%, respectively. Low bulk density (1.42 g cm(-3)) and relatively high compressive strength (2 2MPa) sintered bricks were produced, and the leaching toxicity of the sintered bricks was below the regulatory thresholds of Chinese National Standards. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation and properties of a MnCo2O4 for ceramic interconnect of solid oxide fuel cell via glycine nitrate process

NASA Astrophysics Data System (ADS)

Yoon, Mi Young; Lee, Eun Jung; Song, Rak Hyun; Hwang, Hae Jin

2011-12-01

MnCo2O4 powder was prepared by a wet chemistry method using metal nitrates and glycine in an aqueous solution. The phase stability, sintering behavior, thermal expansion and electrical conductivity were examined to characterize powder suitability as an interconnect material in solid oxide fuel cells (SOFCs). X-ray diffraction indicated that the MnCo2O4 spinel synthesized by the glycine nitrate process was stable until 1100 °C and it was possible to obtain a fully densified single phase spinel. On the other hand, the MnCo2O4 synthesized by a solid state reaction decomposed into a cubic spinel and CoO after being sintered at 1100 °C. This might be associated with the reduction of Co3+ in the octahedral site of the cubic spinel phase. MnCo2O4 showed a thermal expansion coefficient comparable to that of other SOFCs components, as well as good electrical conductivity. Therefore, MnCo2O4 is a potential candidate for the ceramic interconnects in SOFCs, provided the phase instability under reducing environments can be improved.

Epsilon Metal Waste Form for Immobilization of Noble Metals from Used Nuclear Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crum, Jarrod V.; Strachan, Denis M.; Rohatgi, Aashish

2013-10-01

Epsilon metal (ε-metal), an alloy of Mo, Pd, Rh, Ru, and Tc, is being developed as a waste form to treat and immobilize the undissolved solids and dissolved noble metals from aqueous reprocessing of commercial used nuclear fuel. Epsilon metal is an attractive waste form for several reasons: increased durability relative to borosilicate glass, it can be fabricated without additives (100% waste loading), and in addition it also benefits borosilicate glass waste loading by eliminating noble metals from the glass and thus the processing problems related there insolubility in glass. This work focused on the processing aspects of the epsilonmore » metal waste form development. Epsilon metal is comprised of refractory metals resulting in high reaction temperatures to form the alloy, expected to be 1500 - 2000°C making it a non-trivial phase to fabricate by traditional methods. Three commercially available advanced technologies were identified: spark-plasma sintering, microwave sintering, and hot isostatic pressing, and investigated as potential methods to fabricate this waste form. Results of these investigations are reported and compared in terms of bulk density, phase assemblage (X-ray diffraction and elemental analysis), and microstructure (scanning electron microscopy).« less

Method of preparing uranium nitride or uranium carbonitride bodies

DOEpatents

Wilhelm, Harley A.; McClusky, James K.

1976-04-27

Sintered uranium nitride or uranium carbonitride bodies having a controlled final carbon-to-uranium ratio are prepared, in an essentially continuous process, from U.sub.3 O.sub.8 and carbon by varying the weight ratio of carbon to U.sub.3 O.sub.8 in the feed mixture, which is compressed into a green body and sintered in a continuous heating process under various controlled atmospheric conditions to prepare the sintered bodies.

Thermal barrier coating resistant to sintering

DOEpatents

Subramanian, Ramesh; Seth, Brij B.

2004-06-29

A device (10) is made, having a ceramic thermal barrier coating layer (16) characterized by a microstructure having gaps (18) with a sintering inhibiting material (22) disposed on the columns (20) within the gaps (18). The sintering resistant material (22) is stable over the range of operating temperatures of the device (10), is not soluble with the underlying ceramic layer (16) and is applied by a process that is not an electron beam physical vapor deposition process.

Nanocrystalline Iron-Cobalt Alloys for High Saturation Indutance

DTIC Science & Technology

2016-02-24

toroid. Before fully embarking on the problem of creating the toroid’s from particles sintered by a process known as sparked plasma sintering which...allows the particles to be rapidly sintered without compromising the nano crystalline particle size, it was deemed necessary to anticipate the

SINTERING AND SULFATION OF CALCIUM SILICATE-ALUMINATE

EPA Science Inventory

The effect of sintering on the reactivity of solids at high temperature was studied. The nature of the interaction was studied with calcium silicate-aluminate reacting with SO2 between 665 and 800 C. The kinetics of the sintering and sulfation processes were measured independentl...

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

NASA Astrophysics Data System (ADS)

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.

Development and Investigation of Tungsten Copper Sintered Parts for Using in Medium and High Voltage Switching Devices

NASA Astrophysics Data System (ADS)

Lungu, M. V.; Lucaci, M.; Tsakiris, V.; Brătulescu, A.; Cîrstea, C. D.; Marin, M.; Pătroi, D.; Mitrea, S.; Marinescu, V.; Grigore, F.; Tălpeanu, D.; Stancu, N.; Godeanu, P.; Melnic, C.

2017-06-01

Abstract Tungsten-copper (W-Cu) sintered parts with 75 wt.% W, 24 wt.% Cu and 1 wt.% Ni for using as arcing contacts in medium and high voltage switching devices were developed successfully by powder metallurgy (PM) techniques. Sintered parts with diameter of 50±0.5 mm and height of 6±0.5 mm were manufactured by pressing-sintering-infiltration (P-S-I) and spark plasma sintering (SPS) at sintering temperature of 1150°C, and 1050°C, respectively. Physical, chemical, electrical, thermal and mechanical properties of the samples were investigated. Microstructure was analyzed by optical microscopy and scanning electron microscopy. Material properties were influenced by the consolidation processes. The best results were achieved by SPS process. The relative density was more than 95 %, Vickers hardness HV1/15 was over 227, elastic modulus was over 143 GPa, and homogeneous microstructure was revealed. These good properties can contribute to higher lifetime of arcing contacts under severe working conditions.

Toward Interpreting Failure in Sintered-Silver Interconnection Systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wereszczak, Andrew A; Waters, Shirley B

2016-01-01

The mechanical strength and subsequent reliability of a sintered-silver interconnection system is a function of numerous independent parameters. That system is still undergoing process development. Most of those parameters (e.g., choice of plating) are arguably and unfortunately taken for granted and are independent of the silver s cohesive strength. To explore such effects, shear strength testing and failure analyses were completed on a simple, mock sintered-silver interconnection system consisting of bonding two DBC ceramic substrates. Silver and gold platings were part of the test matrix, as was pre-drying strategies, and the consideration of stencil-printing vs. screen-printing. Shear strength of sintered-silvermore » interconnect systems was found to be was insensitive to the choice of plating, drying practice, and printing method provided careful and consistent processing of the sintered-silver are practiced. But if the service stress in sintered silver interconnect systems is anticipated to exceed ~ 60 MPa, then the system will likely fail.« less

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

NASA Astrophysics Data System (ADS)

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.

Electric field-assisted sintering of nanocrystalline hydroxyapatite for biomedical applications

NASA Astrophysics Data System (ADS)

Tran, Tien Bich

As the main inorganic component of bone, hydroxyapatite (HA, Ca 10(PO4)6(OH)2) should be an ideal candidate in biomaterials selection. When grain sizes are in the nanometric regime, protein adsorption and cell adhesion are enhanced, while strength, hardness, and wear resistance are improved. Unfortunately, low phase stability, poor sinterability, and a tendency towards exaggerated grain coarsening challenge full densification of nanocrystalline hydroxyapatite by conventional sintering methods. The field-assisted sintering technique (FAST) has successfully consolidated a variety of nanocrystalline metals and ceramics in dramatically reduced times. The sintering enhancements observed during FAST can be attributed to thermal and athermal effects. The rapid heating rates (up to ˜1000ºC/min) afforded by FAST contribute a significant thermal effect. Since fast heating rates reduce powder exposure to sub-sintering temperatures, non-densifying surface diffusion is limited. The athermal effects of FAST are less well understood and can include plasma generation, dielectric breakdown, particle surface cleaning, grain boundary pinning, and space charge effects. Applying the field-assisted sintering technique to nanocrystalline hydroxyapatite yielded surprising results. Deviations from conventional densification behavior were observed, with dehydroxylation identified as the most deleterious process to densification as well as mechanical and biological performance. Since hydroxyapatite is not a stable phase at high temperatures and low water partial pressure atmospheres, desintering due to dehydroxylation-related pore formation became apparent during Stage III sintering. In fact, the degree of desintering and pore formation increased with the extent of Stage III sintering and grain growth. The atomic rearrangements taking place during grain boundary migration are believed to favor the formation of more-stable oxyapatite through hydroxyapatite dehydroxylation. This behavior was consistent during varied heating rate (50--400ºC/min) and varied pressure application (25--90 MPa) studies. While in vitro cytocompatibility studies using MG63 osteoblast-like cells demonstrated the biocompatibility of the FAST-processed specimens, bioactivity was sensitive to processing parameters. Since extensive dehydroxylation reduces the surface charge of the sintered materials, apatite deposition during simulated body fluid immersion only occurred when dehydroxylation was mild---i.e., on specimens sintered at low temperatures (800--900ºC) or for short periods. Microstructural investigations revealed that HA sintered at temperatures above 900ºC under an applied electric field contained nanometric residual pores in grain interiors, as well as micron-sized dehydroxylation-related pores at grain boundaries and grain boundary junctions. These larger pores were responsible for the increasing embrittlement of specimens sintered at higher temperatures. Although grain size dependence could not be found in the 60--100 nm grain size range, fracture toughness (KIC = 1.92 MPa√m, maximum) increased with decreasing sintering temperature. Results from the suite of investigations conducted demonstrate that biocompatible and bioactive nanocrystalline hydroxyapatite with enhanced mechanical properties can be efficiently manufactured by field-assisted sintering under controlled processing conditions.

Phosphorus as sintering activator in powder metallurgical steels: characterization of the distribution and its technological impact.

PubMed

Krecar, Dragan; Vassileva, Vassilka; Danninger, Herbert; Hutter, Herbert

2004-06-01

Powder metallurgy is a highly developed method of manufacturing reliable ferrous parts. The main processing steps in a powder metallurgical line are pressing and sintering. Sintering can be strongly enhanced by the formation of a liquid phase during the sintering process when using phosphorus as sintering activator. In this work the distribution (effect) of phosphorus was investigated by means of secondary ion mass spectrometry (SIMS) supported by Auger electron spectroscopy (AES) and electron probe micro analysis (EPMA). To verify the influence of the process conditions (phosphorus content, sintering atmosphere, time) on the mechanical properties, additional measurements of the microstructure (pore shape) and of impact energy were performed. Analysis of fracture surfaces was performed by means of scanning electron microscopy (SEM). The concentration of phosphorus differs in the samples from 0 to 1% (w/ w). Samples with higher phosphorus concentrations (1% (w/ w) and above) are also measurable by EPMA, whereas the distributions of P at technically relevant concentrations and the distribution of possible impurities are only detectable (visible) by means of SIMS. The influence of the sintering time on the phosphorus distribution will be demonstrated. In addition the grain boundary segregation of P was measured by AES at the surface of in-situ broken samples. It will be shown that the distribution of phosphorus depends also on the concentration of carbon in the samples.

A Fully Coupled Simulation and Optimization Scheme for the Design of 3D Powder Injection Molding Processes

NASA Astrophysics Data System (ADS)

Ayad, G.; Song, J.; Barriere, T.; Liu, B.; Gelin, J. C.

2007-05-01

The paper is concerned with optimization and parametric identification of Powder Injection Molding process that consists first in injection of powder mixture with polymer binder and then to the sintering of the resulting powders parts by solid state diffusion. In the first part, one describes an original methodology to optimize the injection stage based on the combination of Design Of Experiments and an adaptive Response Surface Modeling. Then the second part of the paper describes the identification strategy that one proposes for the sintering stage, using the identification of sintering parameters from dilatometer curves followed by the optimization of the sintering process. The proposed approaches are applied to the optimization for manufacturing of a ceramic femoral implant. One demonstrates that the proposed approach give satisfactory results.

Selective Laser Sintering of Nano Al2O3 Infused Polyamide

PubMed Central

Warnakula, Anthony; Singamneni, Sarat

2017-01-01

Nano Al2O3 polyamide composites are evaluated for processing by selective laser sintering. A thermal characterization of the polymer composite powders allowed us to establish the possible initial settings. Initial experiments are conducted to identify the most suitable combinations of process parameters. Based on the results of the initial trials, more promising ranges of different process parameters could be identified. The post sintering characterization showed evidence of sufficient inter-particle sintering and intra-layer coalescence. While the inter-particle coalescence gradually improved, the porosity levels slightly decreased with increasing laser power. The nano-filler particles tend to agglomerate around the beads along the solid tracks, possibly due to Van der Walls forces. The tensile stress results showed an almost linear increase with increasing nano-filler content. PMID:28773220

The effect of impurities elements on titanium alloy (Ti-6Al-4V) MIM sintered part properties

NASA Astrophysics Data System (ADS)

Ahmad, M. Azmirruddin; Jabir, M.; Johari, N.; Ibrahim, R.; Hamidi, N.

2017-12-01

The titanium alloys (Ti-6Al-4V) compact were fabricated by Metal Injection Molding (MIM). However, the real challenge of MIM processing for titanium alloy is its affinity to be contaminated by interstitial light elements such as oxygen and carbon which could degrade the mechanical properties of sintered titanium alloy such as its tensile strength and ductility. The sintering temperature effect on carbon and oxygen content that affects its physical and mechanical properties of the sintered titanium alloy was studied. The titanium MIM brown specimen was sintered at four different sintering temperatures which are 1100 °C, 1150 °C, 1200 °C and 1250 °C for 4 hours under furnace control atmosphere. The experimental result indicated that the specimen which has been made from 100% gas atomized powder have a relative density of 92.2 % - 97.6 %, the range of porosity percent around 2.38 %-3.84 %. Ultimate tensile strength of 873.11 MPa - 1007.19 MPa and ductility percent in range of 1.89 %-3.46 %. The titanium alloy MIM specimen which was sintered at 1150 °C contained 0.145 % of carbon and 0.143 % of oxygen possess the highest value of density and tensile strength, with value of 4.344 gcm-3 and 1007.2 MPa respectively. Meanwhile, the titanium alloy MIM specimen which was sintered at 1200 °C contains 0.130 % of carbon and 0.127 % of oxygen, has the highest percentage of ductility with 3.46 %. The carbon content level increased as the sintering temperature increased due to decomposition of high molecule weight of residue binder system which could not be eliminated during solvent extraction debinding process and sintered at low temperature. Contrarily, the oxygen content level indicates a decrease as the sintering temperature increased. Briefly, the sintering temperature could influence the physical and mechanical properties of titanium alloy MIM sintered specimen as it influences the oxygen and carbon content level in the alloys.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sudiana, I. Nyoman, E-mail: sudiana75@yahoo.com; Ngkoimani, La Ode; Usman, Ida

Microwave sintering of materials has attracted much research interest because of its significant advantages (e.g. reduced sintering temperatures and soaking times) over the conventional heating. Most researchers compared processes that occurred during the microwave and conventional heating at the same temperature and time. The enhancements found in the former method are indicated as a 'non-thermal effect' which is usually used for explaining the phenomena in microwave processing. Numerous recent studies have been focused on the effect to elucidate the microwave interaction mechanism with materials. Moreover, recent progress on microwave sources such as gyrotrons has opened the possibility for processing materialsmore » by using a higher microwave frequency. Therefore, the technology is expected to exhibit a stronger non-thermal effect. This paper presents results from a series of experiments to study the non-thermal effect on microwave sintered alumina. Sintering by using a wide rage of microwave frequencies up to 300 GHz as well as a conventional furnace was carried out. The linear shrinkages of samples for each sintering method were measured. Pores and grains taken from scanning electron microstructure (SEM) images of cut surfaces were also examined. The results of a comparative study of the shrinkages and microstructure evolutions of the sintered samples under annealing in microwave heating systems and in an electric furnace were analyzed. A notably different behavior of the shrinkages and microstructures of alumina after being annealed was found. The results suggested that microwave radiations provided an additional force for mass transports. The results also indicated that the sintering process depended on microwave frequencies.« less

Improved Tubulars for Better Economics in Deep Gas Well Drilling Using Microwave Technology

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dinesh Agrawal

2006-09-30

The main objective of the entire research program has been to improve the rate-of-penetration in deep hostile environments by improving the life cycle and performance of coiled-tubing, an important component of a deep well drilling system for oil and gas exploration, by utilizing the latest developments in the microwave materials technology. Based on the results of the Phase I and insurmountable difficulties faced in the extrusion and de-waxing processes, the approach of achieving the goals of the program was slightly changed in the Phase II in which an approach of microwave sintering combined with Cold Isostatic Press (CIP) and joiningmore » (by induction or microwave) has been adopted. This process can be developed into a semicontinuous sintering process if the CIP can produce parts fast enough to match the microwave sintering rates. The main objective of the Phase II research program is to demonstrate the potential to economically manufacture microwave processed coiled tubing with improved performance for extended useful life under hostile coiled tubing drilling conditions. After the completion of the Phase II, it is concluded that scale up and sintering of a thin wall common O.D. size tubing that is widely used in the market is still to be proved and further experimentation and refinement of the sintering process is needed in Phase III. Actual manufacturing capability of microwave sintered, industrial quality, full length tubing will most likely require several million dollars of investment.« less

Improved Tubulars for Better Economics in Deep Gas Well Drilling using Microwave Technology

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dinesh Agrawal; Paul Gigl; Mark Hunt

2007-07-31

The main objective of the entire research program has been to improve the rate-of-penetration in deep hostile environments by improving the life cycle and performance of coiled-tubing, an important component of a deep well drilling system for oil and gas exploration, by utilizing the latest developments in the microwave materials technology. Based on the results of the Phase I and insurmountable difficulties faced in the extrusion and de-waxing processes, the approach of achieving the goals of the program was slightly changed in the Phase II in which an approach of microwave sintering combined with Cold Isostatic Press (CIP) and joiningmore » (by induction or microwave) has been adopted. This process can be developed into a semicontinuous sintering process if the CIP can produce parts fast enough to match the microwave sintering rates. The main objective of the Phase II research program is to demonstrate the potential to economically manufacture microwave processed coiled tubing with improved performance for extended useful life under hostile coiled tubing drilling conditions. After the completion of the Phase II, it is concluded that scale up and sintering of a thin wall common O.D. size tubing that is widely used in the market is still to be proved and further experimentation and refinement of the sintering process is needed in Phase III. Actual manufacturing capability of microwave sintered, industrial quality, full length tubing will most likely require several million dollars of investment.« less

A feasibility study for high-temperature titanium reduction from TiCl4 using a magnesiothermic process

NASA Astrophysics Data System (ADS)

Ivanov, S. L.; Zablotsky, D.

2018-05-01

The current industrial practice for titanium extraction is a complex procedure, which produces a porous reaction mass of sintered titanium particulates fused to a steel retort wall with magnesium and MgCl2 trapped in the interstices. The reactor temperature is limited to approx. 900 °C due to the formation of fusible TiFe eutectic, which corrodes the retort and degrades the quality of titanium sponge. Here we examine the theoretical foundations and technological possibilities to design a shielded retort of niobium-zirconium alloy NbZr(1%), which is resistant to corrosion by titanium at high temperature. We consider the reactor at a temperature of approx. 1150 °C. Supplying stoichiometric quantities of reagents enables the reaction in the gas phase, whereas the exothermic process sustains the combustion of the reaction zone. When the pathway to the condenser is open, vacuum separation and evacuation of vaporized magnesium dichloride and excess magnesium into the water-cooled condenser take place. As both the reaction and the evacuation occur within seconds, the yield of the extraction is improved. We anticipate new possibilities for designing a device combining the retort function to conduct the reduction in the gas phase with fast vacuum separation of the reaction products and distillation of magnesium dichloride.

Relationship between fabrication method and chemical stability of Ni-BaZr0.8Y0.2O3-δ membrane

NASA Astrophysics Data System (ADS)

Fang, Shumin; Wang, Siwei; Brinkman, Kyle S.; Su, Qing; Wang, Haiyan; Chen, Fanglin

2015-03-01

NiO effectively promotes the sintering of highly refractory Y-doped BaZrO3 (BZY) through the formation of BaY2NiO5, providing a simple and cost-effective method for the fabrication of dense BZY electrolyte and Ni-BZY hydrogen separation membrane at ∼1400 °C. Unfortunately, insulating BaCO3 and Y2O3 phases formed on the surface of BZY and Ni-BZY prepared by solid state reaction method with NiO after annealing in wet CO2. Ni-BZY membranes prepared from different methods suffered different degree of performance loss in wet H2 at 900 °C. The chemical instability of Ni-BZY is attributed to the formation of a secondary phase (BaY2O4) generated from the reduction of BaY2NiO5 in H2 during the sintering process. Both BaY2O4 and BaY2NiO5 react with H2O, and CO2 at elevated temperatures, generating insulating Ba(OH)2 and BaCO3 phases, respectively. The less BaY2O4 is formed in the fabrication process, the better chemical stability the Ni-BZY membranes possess. Therefore, a new Ni-BZY membrane is prepared through a judicial combination of BZY powders prepared from combined EDTA-citric and solid state reaction methods, and demonstrates exceptional chemical stability in H2O and CO2, enabling stable and even improved hydrogen flux in wet 50% CO2 at 900 °C.

Sintering of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) with/without SrTiO3 Dopant

NASA Technical Reports Server (NTRS)

Dynys, F.; Sayir, A.; Heimann, P. J.

2004-01-01

The perovskite composition, BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta), displays excellent protonic conduction at high temperatures making it a desirable candidate for hydrogen separation membranes. This paper reports on the sintering behavior of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders doped with SrTiO3. Two methods were used to synthesize BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders: (1) solid state reaction and (2) wet chemical co-precipitation. Co-precipitated powder crystallized into the perovskite phase at 1000 C for 4 hrs. Complete reaction and crystallization of the perovskite phase by solid state was achieved by calcining at 1200 C for 24 hrs. Solid state synthesis produced a coarser powder with an average particle size of 1.3 microns and surface area of 0.74 sq m/g. Co-precipitation produced a finer powder with a average particle size of 65 nm and surface area of 14.9 sq m/g. Powders were doped with 1, 2, 5, and 10 mole % SrTiO3. Samples were sintered at 1450 C, 1550 C and 1650 C. SrTiO3 enhances sintering, optimal dopant level is different for powders synthesized by solid state and co-precipitation. Both powders exhibit similar grain growth behavior. Dopant levels of 5 and 10 mole % SrTiO3 significantly enhances the grain size.

Physical properties and microstructure study of 316L SS fabricated by metal injection moulding process

NASA Astrophysics Data System (ADS)

Dandang, Nur Aidah Nabihah; Harun, Wan Sharuzi Wan; Khalil, Nur Zalikha; Ismail, Muhammad Hussain; Ibrahim, Rosdi

2017-12-01

Metal injection moulding (MIM) has been practised to process alloy powders to become components with significant physical and mechanical properties. Dissimilar than other methods, MIM focuses on the production of high volume, a small, and complex shape of products. The performance of the compacts depends on the suitable sintering parameters that governs their strengths in the final phase which determines the excellent properties of the sintered compacts. Three different sintering temperatures were utilised; 1100, 1200, and 1300 °C with two different soaking times; 1 and 3 hours at 10 °C/min heating rate to study their effect on the physical properties and microstructure analysis of 316L SS alloy compacts. The shrinkage measurement, surface roughness, and density measurement had been conducted for physical properties study. Different sintering temperatures give an effect to the physical properties of the sintered compacts. The shrinkage measurement at 1300 °C and 3-hour sintering condition demonstrated the highest percentage reading which was 10.1 % compared to the lowest percentage reading of 6.4 % at 1100 °C and 1-hour sintering conditions. Whereas, the minimum percentage of density measurement can be found at sintering conditions of 1100 °C and 1-hour which is 83.9 % and the highest percentage is at 1300 °C and 3-hour sintering condition which is about 89.51 %. Therefore, it has been determined that there could be a significant relationship between sintering temperature and physical properties in which it can be found from the porosity of the compact based on the microstructure studies.

An application of powder metallurgy to dentistry.

PubMed

Oda, Y; Ueno, S; Kudoh, Y

1995-11-01

Generally, the dental casting method is used to fabricate dental prostheses made with metal. The method of fabricating dental prostheses from sintered titanium alloy has certain advantages: the elimination of casting defects, a sintering temperature that is lower than the melting point, and a shorter processing time. By examining (1) the properties of green, sintered compacts of titanium powder, (2) the effects of adding aluminum powder on the properties of green, sintered compacts of Ti-Al compound, and (3) the effects of adding copper powder on the properties of green, sintered compacts of Ti-Al-Cu compound, the authors developed a sintered titanium alloy on a trial basis. Because the properties satisfied the requirements of dental restorations, a powder metallurgical method of making dental restorations from this sintered titanium alloy was devised. Applications of such sintered titanium alloys for the metal coping of metal-ceramic crowns and denture base plates were discussed.

Grain growth effects on magnetic properties of Ni0.6Zn0.4Fe2O4 material prepared using mechanically alloyed nanoparticles

NASA Astrophysics Data System (ADS)

Syazwan, M. M.; Hapishah, A. N.; Azis, R. S.; Abbas, Z.; Hamidon, M. N.

2018-06-01

The effect of grain growth via sintering temperature on some magnetic properties is reported in this research. Ni0.6Zn0.4Fe2O4 nanoparticles were mechanically alloyed for 6 h and the sintering process starting from 600 to 1200 °C with 25 °C increment with only one sample subjected to all sintering scheme. The resulting change in the material was observed after each sintering. Single phase has been formed at 600 °C and above and the intensity peaks increased with sintering temperature as well as crystallinity increment. The morphological studies showed grain size increment as the sintering temperature increased. Moreover, the density increased while the porosity decreased with increasing sintering temperature. The saturation induction, Bs increased with the increased of grain size. On the other hand, the coercivity-vs-grain size plot reveals the critical single-domain-to-multidomain grain size to be about ∼400 nm. The initial permeability, μi value was increased with grain size enhancement. The microstructural grain growth, as exposed for the first time by this research, is shown as a process of multiple activation energy barriers.

Processing and characterization of zeta-Ta4C 3-x: A high toughness tantalum carbide

NASA Astrophysics Data System (ADS)

Sygnatowicz, Michael M.

Tantalum carbides are commonly processed by hot-pressing, canned hot-isostatic-pressing, or spark-plasma sintering because of their high melting temperatures and low diffusivities. This study reports processing of dense ζ-Ta4C 3-x by reaction sintering of a Ta and TaC powder mixture (C/Ta atomic ratio = 0.66). ζ-Ta4C3-x is of interest due to its rhombohedral (trigonal) crystal structure that may be characterized as a polytype with both face-centered-cubic (fcc) and hexagonal-close-packed (hcp) Ta stacking sequences interrupted by stacking faults and missing carbon layers. This structure leads to easy cleaving on the basal planes and high fracture toughness. A key step in processing is the hydrogenation of the Ta powder to produce beta-TaH x, a hard and brittle phase that enables efficient comminution during milling and production of small, equiaxed Ta particles that can be packed to high green density with the TaC powder. Studies of phase evolution by quantitative X-ray diffraction during sintering revealed several intermediate reactions: (a) decomposition of beta-TaHx to Ta, (b) diffusion of C from gamma-TaC to Ta leading to the formation of α-Ta2Cy' with the kinetics described by the Johnson-Mehl-Avrami-Kolmogorov (JMAK) equation with an exponent, n = 0.5, and an activation energy of 221 kJ/mole, (c) equilibration of α-Ta2Cy' and gamma-TaC 0.78 phases, and (d) formation of ζ-Ta4C2.56 from the equilibrated α-Ta2C and gamma-TaC0.78 phases with the kinetics characterized by a higher JMAK exponent ( n ≈ 3) and higher activation energy (1089 kJ/mole). The microstructure showed evidence of nucleation and growth of the ζ-Ta4C 2.56 phase in both the α-Ta2C and gamma-TaC0.78 parent phases with distinct difference in the morphology due to the different number of variants of the habit plane. A hot-pressed and hot-isostatic-pressed (HIPed) material (C/Ta atomic ratio = 0.66), having formed 95 w% ζ-phase, attained a fracture toughness of 15.6 +/- 0.5 MPa√m and a fracture strength of 508 +/- 97 MPa, while a pressureless sintered and HIPed counterpart, having formed 89 w% ζ-phase and 11 w% gamma-TaC0.78, attained a fracture toughness of 13.7 +/- 0.3 MPa√m and a fracture strength of 679 +/- 56 MPa. All ζ-phase containing materials showed rising R-curves. The high fracture toughness and rising R-curve were attributed to ligament bridging across the crack face. The ligaments, called lamella, were formed as a result of weak cleavage planes in the basal plane of the ζ-Ta4C 3-x crystal.

Behavior of oxide film at the interface between particles in sintered Al powders by pulse electric-current sintering

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Song, Minghui; Furuya, Kazuo; Noda, Tetsuji

2003-03-01

The microstructure of the bonding interfaces between particles in aluminum (Al) powder sintered specimens by the pulse electric-current sintering (PECS) process was observed, using conventional transmission electron microscopy (CTEM) and high-resolution transmission electron microscopy (HRTEM). The behavior of oxide film at the interface between Al particles and its effect on properties of the sintered specimens were investigated. The results showed there were two kinds of bonding interfaces in the sintered specimens, namely, the direct metal/metal bonding and the metal/oxide film layer/metal bonding interface. By increasing the fraction of the direct metal/metal bonding interfaces, the tensile strength of the sintered specimens increased, and the electrical resistivity decreased. By increasing the loading pressure at higher sintering temperatures or increasing the sintering temperature under loading pressure, the breakdown of oxide film was promoted. The broken oxide film debris was dispersed in aluminum metal near the bonding interfaces between particles.

Ir-based refractory superalloys by pulse electric current sintering (PECS) process (II prealloyed powder)

NASA Astrophysics Data System (ADS)

Huang, C.; Yamabe-Mitarai, Y.; Harada, H.

2002-02-01

Five prealloyed powder samples prepared from binary Ir-based refractory superalloys were sintered at 1800 °C for 4 h by Pulse Electric Current Sintering (PECS). No metal loss was observed during sintering. The relative densities of the sintered specimens all exceeded 90% T.D. The best one was Ir-13% Hf with the density of 97.82% T.D. Phases detected in sintered samples were in accordance with the phase diagram as expected. Fractured surfaces were observed in two samples (Ir-13% Hf and Ir-15% Zr). Some improvements obtained by using prealloyed powders instead of elemental powders, which were investigated in the previous studies, were presented.

Densification kinetics of nanocrystalline zirconia powder using microwave and spark plasma sintering--a comparative study.

PubMed

Vasylkiv, Oleg; Demirskyi, Dmytro; Sakka, Yoshio; Ragulya, Andrey; Borodianska, Hanna

2012-06-01

Two-stage densification process of nanosized 3 mol% yttria-stabilized zirconia (3Y-SZ) polycrystalline compacts during consolidation via microwave and spark-plasma sintering have been observed. The values of activation energies obtained for microwave and spark-plasma sintering 260-275 kJ x mol(-1) are quite similar to that of conventional sintering of zirconia, suggesting that densification during initial stage is controlled by the grain-boundary diffusion mechanism. The sintering behavior during microwave sintering was significantly affected by preliminary pressing conditions, as the surface diffusion mechanism (230 kJ x mol(-1)) is active in case of cold-isostatic pressing procedure was applied.

Process Parameter Optimization of Extrusion-Based 3D Metal Printing Utilizing PW-LDPE-SA Binder System.

PubMed

Ren, Luquan; Zhou, Xueli; Song, Zhengyi; Zhao, Che; Liu, Qingping; Xue, Jingze; Li, Xiujuan

2017-03-16

Recently, with a broadening range of available materials and alteration of feeding processes, several extrusion-based 3D printing processes for metal materials have been developed. An emerging process is applicable for the fabrication of metal parts into electronics and composites. In this paper, some critical parameters of extrusion-based 3D printing processes were optimized by a series of experiments with a melting extrusion printer. The raw materials were copper powder and a thermoplastic organic binder system and the system included paraffin wax, low density polyethylene, and stearic acid (PW-LDPE-SA). The homogeneity and rheological behaviour of the raw materials, the strength of the green samples, and the hardness of the sintered samples were investigated. Moreover, the printing and sintering parameters were optimized with an orthogonal design method. The influence factors in regard to the ultimate tensile strength of the green samples can be described as follows: infill degree > raster angle > layer thickness. As for the sintering process, the major factor on hardness is sintering temperature, followed by holding time and heating rate. The highest hardness of the sintered samples was very close to the average hardness of commercially pure copper material. Generally, the extrusion-based printing process for producing metal materials is a promising strategy because it has some advantages over traditional approaches for cost, efficiency, and simplicity.

Process Parameter Optimization of Extrusion-Based 3D Metal Printing Utilizing PW–LDPE–SA Binder System

PubMed Central

Ren, Luquan; Zhou, Xueli; Song, Zhengyi; Zhao, Che; Liu, Qingping; Xue, Jingze; Li, Xiujuan

2017-01-01

Recently, with a broadening range of available materials and alteration of feeding processes, several extrusion-based 3D printing processes for metal materials have been developed. An emerging process is applicable for the fabrication of metal parts into electronics and composites. In this paper, some critical parameters of extrusion-based 3D printing processes were optimized by a series of experiments with a melting extrusion printer. The raw materials were copper powder and a thermoplastic organic binder system and the system included paraffin wax, low density polyethylene, and stearic acid (PW–LDPE–SA). The homogeneity and rheological behaviour of the raw materials, the strength of the green samples, and the hardness of the sintered samples were investigated. Moreover, the printing and sintering parameters were optimized with an orthogonal design method. The influence factors in regard to the ultimate tensile strength of the green samples can be described as follows: infill degree > raster angle > layer thickness. As for the sintering process, the major factor on hardness is sintering temperature, followed by holding time and heating rate. The highest hardness of the sintered samples was very close to the average hardness of commercially pure copper material. Generally, the extrusion-based printing process for producing metal materials is a promising strategy because it has some advantages over traditional approaches for cost, efficiency, and simplicity. PMID:28772665

Processing of sintered alpha SiC

NASA Technical Reports Server (NTRS)

Storm, R. S.

1984-01-01

Processing methods of sintered alpha SiC for engine applications are developed in a cost effective manner, using a submicron sized powder blended with sintering aids (boron and carbon). The processes for forming a green powder compact, such as dry pressing, cold isostatic pressing and green machining, slip casting, aqueous extrusion, plastic extrusion, and injection molding, are described. Dry pressing is the simplest route to component fabrication, and is carried out at approximately 10,000 psi pressure, while in the cold isostatic method the pressure could go as high as 20,000 psi. Surfactants are added to control settling rates and casting characteristics in the slip casting. The aqueous extrusion process is accomplished by a hydraulic ram forcing the aqueous mixture through a die. The plastic forming processes of extrusion and injection molding offer the potential of greater diversity in shape capacity. The physical properties of sintered alpha SiC (hardness, Young's modulus, shear modulus, and thermal diffusivity) are extensively tested. Corrosion resistance test results of silicon carbide are included.

Combustion synthesis of ceramic-metal composite materials - The TiC-Al2O3-Al system

NASA Technical Reports Server (NTRS)

Feng, H. J.; Moore, John J.; Wirth, D. G.

1992-01-01

Combustion synthesis was applied for producing ceramic-metal composites with reduced levels of porosity, by allowing an excess amount of liquid metal, generated by the exothermic reaction during synthesis, to infiltrate the pores. It is shown that this method, when applied to TiC-Al2O3 system, led to a decreased level of porosity in the resulting TiC-Al2O3-Al product, as compared with that of TiC-Al2O3 system. This in situ procedure is more efficient than the two-stage conventional processes (i.e., sintering followed by liquid metal infiltration), although there are limitations with respect to total penetration of the liquid metal and maintaining a stable propagation of the combustion reaction.

Process for synthesizing compounds from elemental powders and product

DOEpatents

Rabin, B.H.; Wright, R.N.

1993-12-14

A process for synthesizing intermetallic compounds from elemental powders is described. The elemental powders are initially combined in a ratio which approximates the stoichiometric composition of the intermetallic compound. The mixed powders are then formed into a compact which is heat treated at a controlled rate of heating such that an exothermic reaction between the elements is initiated. The heat treatment may be performed under controlled conditions ranging from a vacuum (pressureless sintering) to compression (hot pressing) to produce a desired densification of the intermetallic compound. In a preferred form of the invention, elemental powders of Fe and Al are combined to form aluminide compounds of Fe[sub 3] Al and FeAl. 25 figures.

Process for synthesizing compounds from elemental powders and product

DOEpatents

Rabin, Barry H.; Wright, Richard N.

1993-01-01

A process for synthesizing intermetallic compounds from elemental powders. The elemental powders are initially combined in a ratio which approximates the stoichiometric composition of the intermetallic compound. The mixed powders are then formed into a compact which is heat treated at a controlled rate of heating such that an exothermic reaction between the elements is initiated. The heat treatment may be performed under controlled conditions ranging from a vacuum (pressureless sintering) to compression (hot pressing) to produce a desired densification of the intermetallic compound. In a preferred form of the invention, elemental powders of Fe and Al are combined to form aluminide compounds of Fe.sub.3 Al and FeAl.

Effect of heating parameters on sintering behaviors and properties of mullite whisker frameworks

NASA Astrophysics Data System (ADS)

Zhang, Y. M.; Zeng, D. J.; Wang, B.; Yang, J. F.

2018-04-01

Mullite whisker frameworks were fabricated by vapor-solid reaction with SiO2, Al2O3 and AlF3 powders as the whisker forming agent at high temperatures. The effects of heating temperature and soaking time on the weight loss, liner shrinkage, porosity, microstructure and compressive strength were investigated. The results showed that with the increasing of the sintering temperature and soaking time, the weight loss and liner shrinkage of the samples increased and the porosities decreased due to the accelerated vapor-solid reaction, resulting in strong bonding and grain growth of the mullite frameworks. The compressive strength of the samples increased with increasing the sintering temperature from 1500 to 1650 °C, and decreased with the soaking time extended to more than 5 h for 1500 °C and 2 h for 1650 °C. A maximum compressive strength of 142 MPa at a porosity of 62.3% was obtained for the mullite whisker framework heated at 1500 °C for 5 h. The enhanced strength was attributed to the strong bonding strength and fine mullite grains resulting from a relative lower heating temperature and a modest soaking time.

Low modulus and bioactive Ti/α-TCP/Ti-mesh composite prepared by spark plasma sintering.

PubMed

Guo, Yu; Tan, Yanni; Liu, Yong; Liu, Shifeng; Zhou, Rui; Tang, Hanchun

2017-11-01

A titanium mesh scaffold composite filled with Ti/α-TCP particles was prepared by spark plasma sintering (SPS). The microstructures and interfacial reactions of the composites were investigated by scanning electron microscopy (SEM), Energy Dispersive Spectroscopy (EDS) and X-ray diffraction (XRD) analyses. The compressive strength and elastic modulus were also measured. In vitro bioactivity and biocompatibility was evaluated by using simulated body fluid and cells culture, respectively. After high temperature sintering, Ti oxides, Ti x P y and CaTiO 3 were formed. The formation of Ti oxides and Ti x P y were resulted from the diffusion of O and P elements from α-TCP to Ti. CaTiO 3 was the reaction product of Ti and α-TCP. The composite of 70Ti/α-TCP incorporated with Ti mesh showed a high compressive strength of 589MPa and a low compressive modulus of 30GPa. The bioactivity test showed the formation of a thick apatite layer on the composite and well-spread cells attachment. A good combination of mechanical properties and bioactivity indicated a high potential application of Ti/α-TCP/Ti-mesh composite for orthopedic implants. Copyright © 2017. Published by Elsevier B.V.

Hydrothermal corrosion of silicon carbide joints without radiation

DOE PAGES

Koyanagi, Takaaki; Katoh, Yutai; Terrani, Kurt A.; ...

2016-09-28

In this paper, hydrothermal corrosion of four types of the silicon carbide (SiC) to SiC plate joints were investigated under pressurized water reactor and boiling water reactor relevant chemical conditions without irradiation. The joints were formed by metal diffusion bonding using molybdenum or titanium interlayer, reaction sintering using Ti—Si—C system, and SiC nanopowder sintering. Most of the joints withstood the corrosion tests for five weeks. The recession of the SiC substrates was limited. Based on the recession of the bonding layers, it was concluded that all the joints except for the molybdenum diffusion bond are promising under the reducing environmentsmore » without radiation. Finally, the SiC nanopowder sintered joint was the most corrosion tolerant under the oxidizing environment among the four joints.« less

Method of electrode fabrication for solid oxide electrochemical cells

DOEpatents

Jensen, R.R.

1990-11-20

A process for fabricating cermet electrodes for solid oxide electrochemical cells by sintering is disclosed. First, a porous metal electrode is fabricated on a solid oxide cell, such as a fuel cell by, for example, sintering, and is then infiltrated with a high volume fraction stabilized zirconia suspension. A second sintering step is used to sinter the infiltrated zirconia to a high density in order to more securely attach the electrode to the solid oxide electrolyte of the cell. High performance fuel electrodes can be obtained with this process. Further electrode performance enhancement may be achieved if stabilized zirconia doped with cerium oxide, chromium oxide, titanium oxide, and/or praseodymium oxide for electronic conduction is used. 5 figs.

Method of electrode fabrication for solid oxide electrochemical cells

DOEpatents

Jensen, Russell R.

1990-01-01

A process for fabricating cermet electrodes for solid oxide electrochemical cells by sintering is disclosed. First, a porous metal electrode is fabricated on a solid oxide cell, such as a fuel cell by, for example, sintering, and is then infiltrated with a high volume fraction stabilized zirconia suspension. A second sintering step is used to sinter the infiltrated zirconia to a high density in order to more securely attach the electrode to the solid oxide electrolyte of the cell. High performance fuel electrodes can be obtained with this process. Further electrode performance enhancement may be achieved if stabilized zirconia doped with cerium oxide, chromium oxide, titanium oxide, and/or praseodymium oxide for electronic conduction is used.

Preparation Of Sources For Plasma Vapor Deposition

NASA Technical Reports Server (NTRS)

Waters, William J.; Sliney, Hal; Kowalski, D.

1993-01-01

Multicomponent metal targets serving as sources of vapor for plasma vapor deposition made in modified pressureless-sintering process. By use of targets made in modified process, one coats components with materials previously plasma-sprayed or sintered but not plasma-vapor-deposited.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nagai, Daisuke; Kinemuchi, Yoshiaki, E-mail: y.kinemuchi@aist.go.jp; Suzuki, Kazuyuki

Alpha″-Fe{sub 16}N{sub 2} nanoparticles (NPs) with high magnetic crystalline anisotropy are useful for practical applications such as recording media. However, due to their strongly aggregated and/or sintered form, which occurs during synthesis, the utilization of the NPs has been limited thus far. Here, we report a method for synthesizing highly dispersive α″-Fe{sub 16}N{sub 2} NPs using hydroxyapatite (HAp). The chemically and thermally stable structure of the HAp coating results in the isolation of individual NPs, such that sintering is prevented during synthesis. Additionally, the acicular shape of the HAp crystal did not hinder gas diffusion during the gas reaction. Finally,more » HAp can be removed by a chelating agent without deteriorating the magnetic properties, resulting in highly dispersive α″-Fe{sub 16}N{sub 2} NPs. - Graphical abstract: Synthesis process of highly dispersive α″-Fe{sub 16}N{sub 2} particles using hydroxyapatite coating and SEM images of nanoparticles. - Highlights: • Highly dispersed α″-Fe{sub 16}N{sub 2} NPs were synthesized using hydroxyapatite (HAp). • HAp coating was stable chemically and thermally during gas reaction of α″-Fe{sub 16}N{sub 2} synthesis. • The magnetic property of the resultant Fe{sub 16}N{sub 2} NPs are M{sub s} of 170 emu/g and H{sub C} of 2450 Oe.« less

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

PubMed Central

Wang, Xingrun; Zhang, Fengsong; Nong, Zexi

2014-01-01

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(AsO4)2 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. PMID:24723798

Study of the suitability of a commercial hydroxyapatite powder to obtain sintered compacts for medical applications

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Tailoring of processing parameters for sintering microsphere-based scaffolds with dense-phase carbon dioxide

PubMed Central

Jeon, Ju Hyeong; Bhamidipati, Manjari; Sridharan, BanuPriya; Scurto, Aaron M.; Berkland, Cory J.; Detamore, Michael S.

2015-01-01

Microsphere-based polymeric tissue-engineered scaffolds offer the advantage of shape-specific constructs with excellent spatiotemporal control and interconnected porous structures. The use of these highly versatile scaffolds requires a method to sinter the discrete microspheres together into a cohesive network, typically with the use of heat or organic solvents. We previously introduced subcritical CO2 as a sintering method for microsphere-based scaffolds; here we further explored the effect of processing parameters. Gaseous or subcritical CO2 was used for making the scaffolds, and various pressures, ratios of lactic acid to glycolic acid in poly(lactic acid-co-glycolic acid), and amounts of NaCl particles were explored. By changing these parameters, scaffolds with different mechanical properties and morphologies were prepared. The preferred range of applied subcritical CO2 was 15–25 bar. Scaffolds prepared at 25 bar with lower lactic acid ratios and without NaCl particles had a higher stiffness, while the constructs made at 15 bar, lower glycolic acid content, and with salt granules had lower elastic moduli. Human umbilical cord mesenchymal stromal cells (hUCMSCs) seeded on the scaffolds demonstrated that cells penetrate the scaffolds and remain viable. Overall, the study demonstrated the dependence of the optimal CO2 sintering parameters on the polymer and conditions, and identified desirable CO2 processing parameters to employ in the sintering of microsphere-based scaffolds as a more benign alternative to heat-sintering or solvent-based sintering methods. PMID:23115065

A strategy to optimize the thermoelectric performance in a spark plasma sintering process

PubMed Central

Chiu, Wan-Ting; Chen, Cheng-Lung; Chen, Yang-Yuan

2016-01-01

Spark plasma sintering (SPS) is currently widely applied to existing alloys as a means of further enhancing the alloys’ figure of merit. However, the determination of the optimal sintering condition is challenging in the SPS process. This report demonstrates a systematic way to independently optimize the Seebeck coefficient S and the ratio of electrical to thermal conductivity (σ/κ) and thus achieve the maximum figure of merit zT = S2(σ/κ)T. Sb2−xInxTe3 (x = 0–0.2) were chosen as examples to validate the method. Although high sintering temperature and pressure are helpful in enhancing the compactness and electrical conductivity of pressed samples, the resultant deteriorated Seebeck coefficient and increasing thermal conductivity eventually offset the benefit. We found that the optimal sintering temperature coincides with temperatures at which the maximum Seebeck coefficient begins to degrade, whereas the optimal sintering pressure coincided with the pressure at which the σ/κ ratio reaches a maximum. Based on this principle, the optimized sintering conditions were determined, and the zT of Sb1.9In0.1Te3 is raised to 0.92 at 600 K, showing an approximately 84% enhancement. This work develops a facile strategy for selecting the optimal SPS sintering condition to further enhance the zT of bulk specimens. PMID:26975209

Processing and properties of SiC whisker reinforced Si sub 3 N sub 4 ceramic matrix composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nunn, S.D.

1991-01-01

Silicon carbide whiskers reinforced silicon nitride ceramic matrix composites were pressureless sintered to high density by liquid phase sintering. Important processing parameters included: whisker dispersion by ultrasonic shear homogenization, particle refinement by attrition milling, pressure slip casting to obtain high greed densities, and sintering in a protective powder bed to limit decomposition. Composites with a {beta}20-Si{sub 3}N{sub 4} solid solution matrix containing 20 vol.% SiC whiskers were sintered to 98-100% theoretical density; composites having a Si{sub 3}N{sub 4} matrix containing YAG sintering aid were sintered to 98% of the theoretical density with 20 vol.% SiC whiskers, and 94% density withmore » 30 vol.% SiC whiskers. Analysis of the pressureless sintered composites revealed orientation of the SiC whiskers and the Si{sub 3}N{sub 4} matrix grains. The mechanical properties of hot pressed Si{sub 3}N{sub 4} composites reinforced with 20 vol.% SiC whiskers were shown to depend on the characteristics of the intergranular phase. Variations in the properties of the composites were analyzed in terms of the amount and morphology of the secondary phase, and the development of internal residual stresses due to the thermal expansion mismatch between the sintering aid phase at the grain boundaries.« less

Toward the Design of a Hierarchical Perovskite Support: Ultra-Sintering-Resistant Gold Nanocatalysts for CO Oxidation

DOE PAGES

Tian, Chengcheng; Zhu, Xiang; Abney, Carter W.; ...

2017-04-12

An ultrastable Au nanocatalyst based on a heterostructured perovskite support with high surface area and uniform LaFeO3 nanocoatings was successfully synthesized and tested for CO oxidation. Strikingly, small Au nanoparticles (4-6 nm) are obtained after calcination in air at 700 °C and under reaction conditions. The designed Au catalyst not only possessed extreme sintering resistance but also showed high catalytic activity and stability because of the strong interfacial interaction between Au and the heterostructured perovskite support.

Production Process for Strong, Light Ceramic Tiles

NASA Technical Reports Server (NTRS)

Holmquist, G. R.; Cordia, E. R.; Tomer, R. S.

1985-01-01

Proportions of ingredients and sintering time/temperature schedule changed. Production process for lightweight, high-strength ceramic insulating tiles for Space Shuttle more than just scaled-up version of laboratory process for making small tiles. Boron in aluminum borosilicate fibers allows fusion at points where fibers contact each other during sintering, thereby greatly strengthening tiles structure.

A Review of Metal Injection Molding- Process, Optimization, Defects and Microwave Sintering on WC-Co Cemented Carbide

NASA Astrophysics Data System (ADS)

Shahbudin, S. N. A.; Othman, M. H.; Amin, Sri Yulis M.; Ibrahim, M. H. I.

2017-08-01

This article is about a review of optimization of metal injection molding and microwave sintering process on tungsten cemented carbide produce by metal injection molding process. In this study, the process parameters for the metal injection molding were optimized using Taguchi method. Taguchi methods have been used widely in engineering analysis to optimize the performance characteristics through the setting of design parameters. Microwave sintering is a process generally being used in powder metallurgy over the conventional method. It has typical characteristics such as accelerated heating rate, shortened processing cycle, high energy efficiency, fine and homogeneous microstructure, and enhanced mechanical performance, which is beneficial to prepare nanostructured cemented carbides in metal injection molding. Besides that, with an advanced and promising technology, metal injection molding has proven that can produce cemented carbides. Cemented tungsten carbide hard metal has been used widely in various applications due to its desirable combination of mechanical, physical, and chemical properties. Moreover, areas of study include common defects in metal injection molding and application of microwave sintering itself has been discussed in this paper.

Consolidation Process in Near Net Shape Manufacturing of Armstrong CP-Ti/Ti-6Al-4V Powders

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yamamoto, Yukinori; Kiggans, Jim; Clark, Michael B

2010-01-01

This paper summarizes our recent efforts to develop the manufacturing technologies of consolidated net-shape components by using new low-cost commercially pure titanium (CP-Ti) and Ti-6Al-4V alloy powders made by the Armstrong process. Fabrication processes of net shape/ near net shape components, such as uniaxial die-pressing, cold isostatic pressing (CIP), sintering, roll compaction and stamping, have been evaluated. The press-and-sinter processing of the powders were systematically investigated in terms of theoretical density and microstructure as a function of time, pressure, and temperature. Up to 96.4% theoretical density has been achieved with the press-and-sinter technology. Tensile properties of the consolidated samples exhibitmore » good ductility as well as equivalent yield/ultimate tensile strengths to those of fully consolidate materials, even with the presence of a certain amount of porosity. A consolidation model is also under development to interpret the powder deformation during processing. Net shape components made of the Armstrong powder can successfully be fabricated with clearer surface details by using press-and-sinter processing.« less

CALCIUM OXIDE SINTERING IN ATMOSPHERES CONTAINING WATER AND CARBON DIOXIDE

EPA Science Inventory

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 ...

Ceramic electrolyte coating methods

DOEpatents

Seabaugh, Matthew M.; Swartz, Scott L.; Dawson, William J.; McCormick, Buddy E.

2004-10-12

Processes for preparing aqueous suspensions of a nanoscale ceramic electrolyte material such as yttrium-stabilized zirconia. The invention also includes a process for preparing an aqueous coating slurry of a nanoscale ceramic electrolyte material. The invention further includes a process for depositing an aqueous spray coating slurry including a ceramic electrolyte material on pre-sintered, partially sintered, and unsintered ceramic substrates and products made by this process.

Aerosol Combustion Synthesis of Nanopowders and Processing to Functional Thin Films

NASA Astrophysics Data System (ADS)

Yi, Eongyu

In this dissertation, the advantages of liquid-feed flame spray pyrolysis (LF-FSP) process in producing nanoparticles (NPs) as well as processing the produced NPs to ceramic/polymer nanocomposite films and high density polycrystalline ceramic films are demonstrated. The LF-FSP process aerosolizes alcohol solutions of metalloorganic precursors by oxygen and combusts them at > 1500 °C. The combustion products are rapidly quenched ( 10s of ms) to < 400 °C, producing NPs with the same compositions as those of the precursor solutions. The high specific surface areas of NPs enable formulation of ceramic/polymer/interface(phase) ternary nanocomposites in which the interphase can be the determining factor of the final net properties. In ceramic processing, NPs show increased sinterability and provide access to small average grain sizes with fine control of microstructures, compared to when micron sized powders are used. Therefore, synthesis, processing, and characterization of NPs, NP derived nanocomposites and ceramic monoliths are of great interest. We first compare the LF-FSP to commercial FSP process by producing fumed silica. Combusting spirocyclic alkoxysilanes or Si(OEt)4 by LF-FSP process produced fumed silica very similar to SiCl4 derived products. Given LF-FSP approach does not require the containment constraints of the SiCl4 process and precursors are synthesized from rice hull ash, the reported approach represents a sustainable, green and potentially lower cost alternative. We then show the versatility of NPs in formulating flexible ceramic/polymer nanocomposites (BaTiO3/epoxy) with superior properties. Volume fractions of the BaTiO3 filler and composite film thicknesses were controlled to adjust the net dielectric constant and the capacitance. Measured net dielectric constants further deviated from theory, with increasing solids loadings, due to NP agglomeration. Wound nanocomposite capacitors showed ten times higher capacitance compared to the commercial counterpart. Following series of studies explore the use of flame made NPs in processing Li+ conducting membranes. Systematic doping studies were conducted in the LiTi2(PO4)3 system to modify the lattice constant, conduction channel width, and sintering behavior by introducing Al3+ and Si4+ dopants. Excess Li2O content was also adjusted to observe its effect on final microstructures and phase compositions. Improved densification rates were found in Li1.7 Al0.3Ti1.7Si0.4P2.6O 12 composition and thin films (52+/-1 microm) with conductivities of 0.3-0.5 mS cm-1 were achieved. Li6.25M0.25La3Zr2O12 (M = Al3+, Ga3+) thin films (25-28 microm) with conductivities of 0.2-1.3 mS cm-1 were also successfully processed using flame made NPs, overcoming processing challenges extant, resulting in significantly reduced energy input required for densification. Heating schedules, sintering atmospheres, and types of substrates were controlled to observe their effect on the sintering behavior. Furthermore, green film thicknesses were found to be a crucial variable determining the final microstructures and phase compositions due to the varying Li2O loss rates with change in thicknesses (surface/volume ratios). Using fully decomposed NP mixtures (Li2CO3/off-stoichiometric La2Zr2O 7), as obtained by LF-FSP, provides an ideal approach to use high surface/reaction energy and liquid phase sintering to drive densification.

Structural comparison of sintering products made of "TiC + Ti" composite powders and "Ti + C" powder mixtures

NASA Astrophysics Data System (ADS)

Krinitcyn, Maksim G.; Pribytkov, Gennadii A.; Korosteleva, Elena N.; Firsina, Irina A.; Baranovskii, Anton V.

2017-12-01

In this study, powder composite materials comprised of TiC and Ti with different ratios are processed by sintering of Ti and C powder mixtures and self-propagating high-temperature synthesis (SHS) in "Ti+C" system followed by sintering. The microstructure and porosity of obtained composites are investigated and discussed. The dependence of porosity on sintering time is explained theoretically. Optimal regimes that enable to obtain the most homogeneous structure with the least porosity are described.

Fabrication of turbine components and properties of sintered silicon nitride

NASA Technical Reports Server (NTRS)

Neil, J. T.; French, K. W.; Quackenbush, C. L.; Smith, J. T.

1982-01-01

This paper presents a status report on the injection molding of sinterable silicon nitride at GTE Laboratories. The effort involves fabrication of single axial turbine blades and monolithic radial turbine rotors. The injection molding process is reviewed and the fabrication of the turbine components discussed. Oxidation resistance and strength results of current injection molded sintered silicon nitride as well as dimensional checks on sintered turbine blades demonstrate that this material is a viable candidate for high temperature structural applications.

The effect of various sintering temperature on used refractory towards its physical properties

NASA Astrophysics Data System (ADS)

Sudibyo; Wulandari, Y. R.; Amin, M.; Azhar

2018-01-01

The used magnesia refractory from the kiln of cement industry was successfully recycled to new refractory using Kaolin as an adhesive. In this work, the temperatures of sintering were varied from 1000°C to 1500°C. The result shows that the increment temperature effects in sintering process will enhance refractory physical properties such as bulk density, cold crushing strength or pressure strength and thermal conductivity. Meanwhile, the porosity was decreased as the increase of the sintering temperature.

Homogeneity of Gd-based garnet transparent ceramic scintillators for gamma spectroscopy

NASA Astrophysics Data System (ADS)

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

2013-09-01

Transparent polycrystalline ceramic scintillators based on the composition Gd1.49Y1.49Ce0.02Ga2.2Al2.8O12 are being developed for gamma spectroscopy detectors. Scintillator light yield and energy resolution depend on the details of various processing steps, including powder calcination, green body formation, and sintering atmosphere. We have found that gallium sublimation during vacuum sintering creates compositional gradients in the ceramic and can degrade the energy resolution. While sintering in oxygen produces ceramics with uniform composition and little afterglow, light yields are reduced, compared to vacuum sintering. By controlling the atmosphere during the various process steps, we were able to minimize the gallium sublimation, resulting in a more homogeneous composition and improved gamma spectroscopy performance.

Comparison of aged polyamide powders for selective laser sintering

NASA Astrophysics Data System (ADS)

Martínez, A.; Ibáñez, A.; Sánchez, A.; León, M. A.

2012-04-01

Selective Laser Sintering (SLS) is an additive manufacturing technology in which a three-dimensional object is manufactured layer by layer by melting powder materials with heat generated from a CO2 laser. However, a disadvantage of sintered materials is that the unsintered powder material during the process can be reused only a limited number of cycles, as during the heating phase in the sintering chamber the material remains at a temperature near the fusion point for a certain period of time and lose properties. This work shows the study of two polyamides (PA12)-based powders used in SLS with the aim of understanding the modification of their properties mainly with the temperature and the time at which they are exposed during the processing.

Process for the recovery of alumina from fly ash

DOEpatents

Murtha, M.J.

1983-08-09

An improvement in the lime-sinter process for recovering alumina from pulverized coal fly ash is disclosed. The addition of from 2 to 10 weight percent carbon and sulfur to the fly ash-calcium carbonate mixture increase alumina recovery at lower sintering temperatures.

Dry Sintering Meets Wet Silver-Ion "Soldering": Charge-Transfer Plasmon Engineering of Solution-Assembled Gold Nanodimers From Visible to Near-Infrared I and II Regions.

PubMed

Fang, Lingling; Wang, Yueliang; Liu, Miao; Gong, Ming; Xu, An; Deng, Zhaoxiang

2016-11-07

Achieving highly tunable and localized surface plasmon resonance up to near infrared (NIR) regions is a key target in nanoplasmonics. In particular, a self-assembly process capable of producing highly uniform and solution-processable nanomaterials with tailor-made plasmonic properties is lacking. We herein address this problem through a conjunctive use of wet Ag + soldering and dry thermal sintering to produce nanodimer-derived structures with precisely engineered charge-transfer plasmon (CTP). The sintered dimers are water soluble, featuring gradually shifted CTP spanning an 800 nm wavelength range (up to NIR II). Upon silica removal, the products are grafted by DNA to offer surface functionality. This process is also adaptable to DNA-linked AuNP dimers toward plasmonic meta-materials via DNA-guided soldering and sintering. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Experimental Study on Hot Metal Desulfurization Using Sintered Red Mud-Based Flux

NASA Astrophysics Data System (ADS)

Li, Fengshan; Zhang, Yanling; Guo, Zhancheng

2017-09-01

This research presents the results of laboratory and pilot-scale tests conducted on the use of sintered red mud (RM)-based flux in the hot metal desulfurization (HMD) process. Al2O3/Na2O in RM can decrease the melting point of lime-based slag and can work as a flux in the HMD process. Good slag fluidity was observed throughout the process, and high desulfurization rates ( 80%) with a low final S content (<0.02%) were experimentally obtained when the RM:CaO ratio was between 1.2:1 and 2.4:1. The pilot-scale test results indicated that a desulfurization rate as high as 91% and a S content <0.0099% could be acquired when RM:lime = 1:1, verifying the feasibility of using sintered RM-based flux in HMD. The data obtained provide important information for promoting the large-scale application of sintered RM in steelmaking.

Chemical Sintering Generates Uniform Porous Hyaluronic Acid Hydrogels

PubMed Central

Cam, Cynthia; Segura, Tatiana

2014-01-01

Implantation of scaffolds for tissue repair has been met with limited success primarily due to the inability to achieve vascularization within the construct. Many strategies have shifted to incorporate pores into these scaffolds to encourage rapid cellular infiltration and subsequent vascular ingrowth. We utilized an efficient chemical sintering technique to create a uniform network of polymethyl methacrylate (PMMA) microspheres for porous hyaluronic acid hydrogel formation. The porous hydrogels generated from chemical sintering possessed comparable pore uniformity and interconnectivity as the commonly used non- and heat sintering techniques. Moreover, similar cell response to the porous hydrogels generated from each sintering approach was observed in cell viability, spreading, proliferation in vitro, as well as, cellular invasion in vivo. We propose chemical sintering of PMMA microspheres using a dilute acetone solution as an alternative method to generating porous hyaluronic acid hydrogels since it requires equal or ten-fold less processing time as the currently used non-sintering or heat sintering technique, respectively. PMID:24120847

Improved microstructure and thermoelectric properties of iodine doped indium selenide as a function of sintering temperature

NASA Astrophysics Data System (ADS)

Dhama, Pallavi; Kumar, Aparabal; Banerji, P.

2018-04-01

In this paper, we explored the effect of sintering temperature on the microstructure, thermal and electrical properties of iodine doped indium selenide in the temperature range 300 - 700 K. Samples were prepared by a collaborative process of vacuum melting, ball milling and spark plasma sintering at 570 K, 630 K and 690 K. Single phase samples were obtained at higher sintering temperature as InSe is stable only at lower temperature. With increasing sintering temperature, densities of the samples were found to improve with larger grain size formation. Negative values of Seebeck coefficient were observed which indicates n-type carrier transport. Seebeck coefficient increases with sintering temperature and found to be the highest for the sample sintered at 690 K. Thermal conductivity found to be lower in the samples sintered at lower temperatures. The maximum thermoelectric figure of merit found to be ˜ 1 at 700 K due to the enhanced power factor as a result of improved microstructure.

On the self-damping nature of densification in photonic sintering of nanoparticles

PubMed Central

MacNeill, William; Choi, Chang-Ho; Chang, Chih-Hung; Malhotra, Rajiv

2015-01-01

Sintering of nanoparticle inks over large area-substrates is a key enabler for scalable fabrication of patterned and continuous films, with multiple emerging applications. The high speed and ambient condition operation of photonic sintering has elicited significant interest for this purpose. In this work, we experimentally characterize the temperature evolution and densification in photonic sintering of silver nanoparticle inks, as a function of nanoparticle size. It is shown that smaller nanoparticles result in faster densification, with lower temperatures during sintering, as compared to larger nanoparticles. Further, high densification can be achieved even without nanoparticle melting. Electromagnetic Finite Element Analysis of photonic heating is coupled to an analytical sintering model, to examine the role of interparticle neck growth in photonic sintering. It is shown that photonic sintering is an inherently self-damping process, i.e., the progress of densification reduces the magnitude of subsequent photonic heating even before full density is reached. By accounting for this phenomenon, the developed coupled model better captures the experimentally observed sintering temperature and densification as compared to conventional photonic sintering models. Further, this model is used to uncover the reason behind the experimentally observed increase in densification with increasing weight ratio of smaller to larger nanoparticles. PMID:26443492

Expansion during the formation of the magnesium aluminate spinel (MgAl(2)O(4)) from its basic oxide (MgO and Al(2)O(3)) powders

NASA Astrophysics Data System (ADS)

Duncan, Flavia Cunha

The extraordinary expansion during the reaction sintering of the magnesium aluminate spinel (MgAl2O4) from its basic oxide (MgO and Al2O3) powders was studied. Experimental series of different size fractions of the reacting materials were formulated to produce the Mg-Al spinel. After batches were prepared, specimens were compacted and fired in air from 1200° to 1700°C for a fixed firing time. A separate set of specimens was fired as a function of time to determine the reaction kinetic parameters. Dimensional changes confirmed that extraordinary expansions of three to four times greater than the prediction from the reaction of solids occur. The solid-state reactions were monitored by X-ray diffraction. The activation energy of the spinel reaction formation was determined to be 280 +/- 20 kJ/mol. It is believed to be associated with the diffusivity of Mg 2+ in either magnesia or spinel during the development of the final spinel structure. New porosity developed in the compacts during the reaction formation of spinel. Scanning electron microscopy confirmed that the magnesia evaporated leaving behind porous magnesia grains, condensed on the alumina particles and reacted to form a shell of spinel. Hollow spinel particles resulted from the original particles of alumina. These porosities generated within the reacting materials influenced the expansions. Final volumetric expansion could potentially reach 56% as a result of the reaction of solids and the porosity generation within MgO and Al2O3. Models of a single alumina particle with and without development of internal porosity were developed. 3-D arrangements of particles showed additional porosity, influencing on the expansions. The decrease in porosity of some specimens fired at higher temperatures indicated that sintering and densification occur simultaneously with the reaction formation of spinel. The decrease in the interparticle porosity limits the full expansion of the particulates to levels lower than the predictions of the model. A term that accounts for this shrinkage should be a significant addition to the model of expansion. Although the spinel forming reaction for most of the particle systems reached near completion, the resulting porous specimens could be viewed as powder compacts in the early stages of sintering and densification.

Aluminum powder metallurgy processing

NASA Astrophysics Data System (ADS)

Flumerfelt, Joel Fredrick

In recent years, the aluminum powder industry has expanded into non-aerospace applications. However, the alumina and aluminum hydroxide in the surface oxide film on aluminum powder require high cost powder processing routes. A driving force for this research is to broaden the knowledge base about aluminum powder metallurgy to provide ideas for fabricating low cost aluminum powder components. The objective of this dissertation is to explore the hypothesis that there is a strong linkage between gas atomization processing conditions, as-atomized aluminum powder characteristics, and the consolidation methodology required to make components from aluminum powder. The hypothesis was tested with pure aluminum powders produced by commercial air atomization commercial inert gas atomization and gas atomization reaction synthesis (GARS). The commercial atomization methods are bench marks of current aluminum powder technology. The GARS process is a laboratory scale inert gas atomization facility. A benefit of using pure aluminum powders is an unambiguous interpretation of the results without considering the effects of alloy elements. A comparison of the GARS aluminum powders with the commercial aluminum powders showed the former to exhibit superior powder characteristics. The powders were compared in terms of size and shape, bulk chemistry, surface oxide chemistry and structure, and oxide film thickness. Minimum explosive concentration measurements assessed the dependence of explosibility hazard on surface area, oxide film thickness, and gas atomization processing conditions. The GARS aluminum powders were exposed to different relative humidity levels, demonstrating the effect of atmospheric conditions on post-atomization oxidation of aluminum powder. An Al-Ti-Y GARS alloy exposed in ambient air at different temperatures revealed the effect of reactive alloy elements on post-atomization powder oxidation. The pure aluminum powders were consolidated by two different routes, a conventional consolidation process for fabricating aerospace components with aluminum powder and a proposed alternative. The consolidation procedures were compared by evaluating the consolidated microstructures and the corresponding mechanical properties. A low temperature solid state sintering experiment demonstrated that tap densified GARS aluminum powders can form sintering necks between contacting powder particles, unlike the total resistance to sintering of commercial air atomization aluminum powder.

Rapid laser sintering of metal nano-particles inks.

PubMed

Ermak, Oleg; Zenou, Michael; Toker, Gil Bernstein; Ankri, Jonathan; Shacham-Diamand, Yosi; Kotler, Zvi

2016-09-23

Fast sintering is of importance in additive metallization processes and especially on sensitive substrates. This work explores the mechanisms which set limits to the laser sintering rate of metal nano-particle inks. A comparison of sintering behavior of three different ink compositions with laser exposure times from micro-seconds to seconds reveals the dominant factor to be the organic content (OC) in the ink. With a low OC silver ink, of 2% only, sintering time falls below 100 μs with resistivity <×4 bulk silver. Still shorter exposure times result in line delamination and deformation with a similar outcome when the OC is increased.

Effect of Al(OH)3 on the sintering of UO2-Gd2O3 fuel pellets with addition of U3O8 from recycle

NASA Astrophysics Data System (ADS)

dos Santos, Lauro Roberto; Durazzo, Michelangelo; Urano de Carvalho, Elita Fontenele; Riella, Humberto Gracher

2017-09-01

The incorporation of gadolinium as burnable poison directly into nuclear fuel is important for reactivity compensation, which enables longer fuel cycles. The function of the burnable poison fuel is to control the neutron population in the reactor core during its startup and the beginning of the fuel burning cycle to extend the use of the fuel. The implementation of UO2-Gd2O3 poisoned fuel in Brazil has been proposed according to the future requirements established for the Angra-2 nuclear power plant. The UO2 powder used is produced from the Ammonium Uranyl Carbonate (AUC). The incorporation of Gd2O3 powder directly into the AUC-derived UO2 powder by dry mechanical blending is the most attractive process, because of its simplicity. Nevertheless, processing by this method leads to difficulties while obtaining sintered pellets with the minimum required density. The cause of the low densities is the bad sintering behavior of the UO2-Gd2O3 mixed fuel, which shows a blockage in the sintering process that hinders the densification. This effect has been overcome by microdoping of the fuel with small quantities of aluminum. The process for manufacturing the fuel inevitably generates uranium-rich scraps from various sources. This residue is reincorporated into the production process in the form of U3O8 powder additions. The addition of U3O8 also hinders densification in sintering. This study was carried out to investigate the influence of both aluminum and U3O8 additives on the density of fuel pellets after sintering. As the effects of these additives are counterposed, this work studied the combined effect thereof, seeking to find an applicable composition for the production process. The experimental results demonstrated the effectiveness of aluminum, in the form of Al(OH)3, as an additive to promote increase in the densification of the (U,Gd)O2 pellets during sintering, even with high additions of U3O8 recycled from the manufacturing process.

Fabrication of Bi2223 bulks with high critical current properties sintered in Ag tubes

NASA Astrophysics Data System (ADS)

Takeda, Yasuaki; Shimoyama, Jun-ichi; Motoki, Takanori; Kishio, Kohji; Nakashima, Takayoshi; Kagiyama, Tomohiro; Kobayashi, Shin-ichi; Hayashi, Kazuhiko

2017-03-01

Randomly grain oriented Bi2223 sintered bulks are one of the representative superconducting materials having weak-link problem due to very short coherence length particularly along the c-axis, resulting in poor intergrain Jc properties. In our previous studies, sintering and/or post-annealing under moderately reducing atmospheres were found to be effective for improving grain coupling in Bi2223 sintered bulks. Further optimizations of the synthesis process for Bi2223 sintered bulks were attempted in the present study to enhance their intergrain Jc. Effects of applied pressure of uniaxial pressing and sintering conditions on microstructure and superconducting properties have been systematically investigated. The best sample showed intergrain Jc of 2.0 kA cm-2 at 77 K and 8.2 kA cm-2 at 20 K, while its relative density was low ∼65%. These values are quite high as for a randomly oriented sintered bulk of cuprate superconductors.

Influence of sulfur dioxide-related interactions on PM2.5 formation in iron ore sintering.

PubMed

Ji, Zhiyun; Fan, Xiaohui; Gan, Min; Chen, Xuling; Lv, Wei; Li, Qiang; Zhou, Yang; Tian, Ye; Jiang, Tao

2017-04-01

The formation of PM 2.5 (aerosol particulate matter less than 2.5 µm in aerodynamic diameter) in association with SO 2 emission during sintering process has been studied by dividing the whole sintering process into six typical sampling stages. A low-pressure cascade impactor was used to collect PM 2.5 by automatically segregating particulates into six sizes. It was found that strong correlation existed between the emission properties of PM 2.5 and SO 2 . Wet mixture layer (overwetted layer and raw mixture layer) had the function to simultaneously capture SO 2 and PM 2.5 during the early sintering stages, and released them back into flue gas mainly in the flue gas temperature-rising period. CaSO 4 crystals constituted the main SO 2 -related PM 2.5 during the disappearing process of overwetted layer, which was able to form perfect individual crystals or to form particles with complex chemical compositions. Besides the existence of individual CaSO 4 crystals, mixed crystals of K 2 SO 4 -CaSO 4 in PM 2.5 were also found during the first half of the temperature-rising period of flue gas. The interaction between fine-grained Ca-based fluxes, potassium vapors, and SO 2 was the potential source of SO 2 -related PM 2.5 . The emission property of PM 2.5 and SO 2 throughout the sintering process exhibited well similarity. This phenomenon tightened the relationship between the formation of PM 2.5 and the emission of SO 2 . Through revealing the properties of SO 2 -related PM 2.5 during sintering process, the potential interaction between fine-grained Ca-based fluxes, potassium vapors, and SO 2 was found to be the source of SO 2 -related PM 2.5 . This information can serve as the guidance to develop efficient techniques to control the formation and emission of PM 2.5 in practical sintering plants.

Direct metal laser sintering: a digitised metal casting technology.

PubMed

Venkatesh, K Vijay; Nandini, V Vidyashree

2013-12-01

Dental technology is undergoing advancements at a fast pace and technology is being imported from various other fields. One such imported technology is direct metal laser sintering technology for casting metal crowns. This article will discuss the process of laser sintering for making metal crowns and fixed partial dentures with a understanding of their pros and cons.

Pt-Zn Clusters on Stoichiometric MgO(100) and TiO2(110): Dramatically Different Sintering Behavior

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dadras, Mostafa J.; Shen, Lu; Alexandrova, Anastassia N.

2015-03-02

Zn was suggested to be a promising additive to Pt in the catalysis of dehydrogenation reactions. In this work, mixed Pt-Zn clusters deposited on two simple oxides, MgO(100) and TiO2(110), were investigated. The stability of these systems against cluster sintering, one of the major mechanisms of catalyst deactivation, is simulated using a Metropolis Monte Carlo scheme under the assumption of the Ostwald ripening mechanism. Particle migration, association to and dissociation from clusters, and evaporation and redeposition of monomers were all included in the simulations. Simulations are done at several high temperatures relevant to reactions of catalytic dehydrogenation. The effect ofmore » temperature is included via both the Metropolis algorithm and the Boltzmann-weighted populations of the global and thermally accessible local minima on the density functional theory potential energy surfaces of clusters of all sizes and compositions up to tetramers. On both surfaces, clusters are shown to sinter quite rapidly. However, the resultant compositions of the clusters most resistant to sintering are quite different on the two supports. On TiO2(110), Pt and Zn appear to phase separate, preferentially forming clusters rich in just one or the other metal. On MgO(100), Pt and Zn remain well-mixed and form a range of bimetallic clusters of various compositions that appear relatively stable. However, Zn is more easily lost from MgO through evaporation. These phenomena were rationalized by several means of chemical bonding analysis.« less

Fast sintering of silver nanoparticle and flake layers by infrared module assistance in large area roll-to-roll gravure printing system

PubMed Central

Park, Janghoon; Kang, Hyi Jae; Shin, Kee-Hyun; Kang, Hyunkyoo

2016-01-01

We present fast sintering for silver (Ag) nanoparticle (NP) and flake layers printed using roll-to-roll (R2R) gravure printing. An infrared (IR) sintering module was applied to an R2R system to shorten the sintering duration of an R2R gravure-printed Ag layer. IR sintering of the conductive layer was improved by optimising the process condition. After printing of the Ag NP and Ag flake layers, additional IR sintering was performed in the R2R system. The lowest sheet resistance obtained in the Ag NP layer was 0.294 Ω/□, the distance between the substrate and lamp was 50-mm long, the IR lamp power was 500 W, and the sintering time was 5.4 s. The fastest sintering of 0.34 Ω/□ was achieved with 50-mm distance, 1,000-W IR lamp power, and 1.08-s sintering time. In the Ag flake layer, the lowest sheet resistance obtained was 0.288 Ω/□ with a 20-mm distance, 1,000-W IR lamp power, and 10.8-s sintering time. Meanwhile, the fastest sintering was obtained with a 3.83 Ω/□ sheet resistance, 20-mm distance, 1000-W IR lamp, and 1.08-s sintering time. Thus, the IR sintering module can easily be employed in an R2R system to obtain excellent layer sheet resistance. PMID:27713469

CAD/CAM machining Vs pre-sintering in-lab fabrication techniques of Y-TZP ceramic specimens: Effects on their mechanical fatigue behavior.

PubMed

Zucuni, C P; Guilardi, L F; Fraga, S; May, L G; Pereira, G K R; Valandro, L F

2017-07-01

This study evaluated the effects of different pre-sintering fabrication processing techniques of Y-TZP ceramic (CAD/CAM Vs. in-lab), considering surface characteristics and mechanical performance outcomes. Pre-sintered discs of Y-TZP ceramic (IPS e.max ZirCAD, Ivoclar Vivadent) were produced using different pre-sintering fabrication processing techniques: Machined- milling with a CAD/CAM system; Polished- fabrication using a cutting device followed by polishing (600 and 1200 SiC papers); Xfine- fabrication using a cutting machine followed by grinding with extra-fine diamond bur (grit size 30 μm); Fine- fabrication using a cutting machine followed by grinding with fine diamond bur (grit size 46 μm); SiC- fabrication using a cutting machine followed by grinding with 220 SiC paper. Afterwards, the discs were sintered and submitted to roughness (n=35), surface topography (n=2), phase transformation (n=2), biaxial flexural strength (n=20), and biaxial flexural fatigue strength (fatigue limit) (n=15) analyses. No monoclinic-phase content was observed in all processing techniques. It can be observed that obtaining a surface with similar characteristics to CAD/CAM milling is essential for the observation of similar mechanical performance. On this sense, grinding with fine diamond bur before sintering (Fine group) was the best mimic protocol in comparison to the CAD/CAM milling. Copyright © 2017 Elsevier Ltd. All rights reserved.

Lunar in situ resource utilization by activated thermites

NASA Astrophysics Data System (ADS)

Hobosyan, Mkhitar; Martirosyan, Karen

2011-10-01

NASA's anticipated returns to the Moon by 2020, subsequent establishment of lunar in situ resource utilization technologies are essential. The surface of Moon is covered with small eroded particles of regolith called lunar dust that adheres electro-statically to everything coming in contact with it, and is of much concern for future lunar base because of its continual mitigation. The next major concern is the protection of equipment and personnel in long term expeditions from harmful UV radiation, which can be made by constructing protective buildings. For construction of permanent structures it is highly desired to have regular shaped sintered regolith with utilization of local materials and with minimum energy consumption. In this study the concept of sintering of lunar regolith with activated thermite reactions is discussed. The thermodynamic calculations as well as the experimental procedure is provided to prove the effectiveness of activated thermites for regolith sintering using local lunar resources with a low (15 wt. %) concentration of aluminum or magnesium. The thermite method is much more energy efficient than the other sintering methods suggested in literature.

Low temperature processed MnCo2O4 and MnCo1.8Fe0.2O4 as effective protective coatings for solid oxide fuel cell interconnects at 750 °C

NASA Astrophysics Data System (ADS)

Molin, S.; Jasinski, P.; Mikkelsen, L.; Zhang, W.; Chen, M.; Hendriksen, P. V.

2016-12-01

In this study two materials, MnCo2O4 and MnCo1.8Fe0.2O4 are studied as potential protective coatings for Solid Oxide Fuel Cell interconnects working at 750 °C. First powder fabrication by a modified Pechini method is described followed by a description of the coating procedure. The protective action of the coating applied on Crofer 22 APU is evaluated by following the area specific resistance (ASR) of the scale/coating for 5500 h including several thermal cycles. The coating is prepared by brush painting and has a porous structure after deposition. Post mortem microstructural characterization performed on the coated samples shows good protection against chromium diffusion from the chromia scale ensured by a formation of a dense reaction layer. This study shows, that even without high temperature sintering and/or reactive sintering it is possible to fabricate protective coatings based on MnCo spinels.

Niobium-titanium superconductors produced by powder metallurgy having artificial flux pinning centers

DOEpatents

Jablonski, Paul D.; Larbalestier, David C.

1993-01-01

Superconductors formed by powder metallurgy have a matrix of niobium-titanium alloy with discrete pinning centers distributed therein which are formed of a compatible metal. The artificial pinning centers in the Nb-Ti matrix are reduced in size by processing steps to sizes on the order of the coherence length, typically in the range of 1 to 10 nm. To produce the superconductor, powders of body centered cubic Nb-Ti alloy and the second phase flux pinning material, such as Nb, are mixed in the desired percentages. The mixture is then isostatically pressed, sintered at a selected temperature and selected time to produce a cohesive structure having desired characteristics without undue chemical reaction, the sintered billet is reduced in size by deformation, such as by swaging, the swaged sample receives heat treatment and recrystallization and additional swaging, if necessary, and is then sheathed in a normal conducting sheath, and the sheathed material is drawn into a wire. The resulting superconducting wire has second phase flux pinning centers distributed therein which provide enhanced J.sub.ct due to the flux pinning effects.

Efficacy of a Solution-Based Approach for Making Sodalite Waste Forms for an Oxide Reduction Salt Utilized in the Reprocessing of Used Uranium Oxide Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Riley, Brian J.; Pierce, David A.; Frank, Steven M.

2015-04-01

This paper describes various approaches for making sodalite with a LiCl-Li2O oxide reduction salt used to recover uranium from used oxide fuel. The approaches include sol-gel and solution-based synthesis processes. As-made products were mixed with 5 and 10 mass% of a Na2O-B2O3-SiO2 glass binder and these, along with product without a binder, were heated using either a cold-press-and-sinter method or hot uniaxial pressing. The results demonstrate the limitation of sodalite yield due to the fast intermediate reactions between Na+ and Cl- to form halite in solution and Li2O and SiO2 to form lithium silicates (e.g., Li2SiO3 or Li2Si2O5) in themore » calcined and sintered pellets. The results show that pellets can be made with high sodalite fractions (~92 mass%) and low porosities using a solution-based approach and this LiCl-Li2O salt.« less

Parallel Large-Scale Molecular Dynamics Simulation Opens New Perspective to Clarify the Effect of a Porous Structure on the Sintering Process of Ni/YSZ Multiparticles.

PubMed

Xu, Jingxiang; Higuchi, Yuji; Ozawa, Nobuki; Sato, Kazuhisa; Hashida, Toshiyuki; Kubo, Momoji

2017-09-20

Ni sintering in the Ni/YSZ porous anode of a solid oxide fuel cell changes the porous structure, leading to degradation. Preventing sintering and degradation during operation is a great challenge. Usually, a sintering molecular dynamics (MD) simulation model consisting of two particles on a substrate is used; however, the model cannot reflect the porous structure effect on sintering. In our previous study, a multi-nanoparticle sintering modeling method with tens of thousands of atoms revealed the effect of the particle framework and porosity on sintering. However, the method cannot reveal the effect of the particle size on sintering and the effect of sintering on the change in the porous structure. In the present study, we report a strategy to reveal them in the porous structure by using our multi-nanoparticle modeling method and a parallel large-scale multimillion-atom MD simulator. We used this method to investigate the effect of YSZ particle size and tortuosity on sintering and degradation in the Ni/YSZ anodes. Our parallel large-scale MD simulation showed that the sintering degree decreased as the YSZ particle size decreased. The gas fuel diffusion path, which reflects the overpotential, was blocked by pore coalescence during sintering. The degradation of gas diffusion performance increased as the YSZ particle size increased. Furthermore, the gas diffusion performance was quantified by a tortuosity parameter and an optimal YSZ particle size, which is equal to that of Ni, was found for good diffusion after sintering. These findings cannot be obtained by previous MD sintering studies with tens of thousands of atoms. The present parallel large-scale multimillion-atom MD simulation makes it possible to clarify the effects of the particle size and tortuosity on sintering and degradation.

IMPROVED TUBULARS FOR BETTER ECONOMICS IN DEEP GAS WELL DRILLING USING MICROWAVE TECHNOLOGY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dinesh Agrawal; Paul Gigl; Mahlon Dennis

2005-03-01

The main objective of the research program has been to improve the rate-of-penetration in deep hostile environments by improving the life cycle and performance of coiled-tubing, an important component of a deep well drilling system for oil and gas exploration, by utilizing the latest developments in the microwave materials technology. Originally, it was proposed to accomplish this by developing an efficient and economically viable continuous microwave process to sinter continuously formed/extruded steel powder for the manufacture of seamless coiled tubing and other tubular products. However, based on the results and faced with insurmountable difficulties in the extrusion and de-waxing processes,more » the approach of achieving the goals of the program has been slightly changed. In the continuation proposal an approach of microwave sintering combined with Cold Isostatic Press (CIP) and joining (by induction or microwave) is adopted. This process can be developed into a semi-continuous sintering process if the CIP can produce parts fast enough to match the microwave sintering rates. Originally, the entire program was spread over three phases with the following goals: Phase I: Demonstration of the feasibility concept of continuous microwave sintering process for tubular steel products. Phase II: Design, building and testing of a prototype microwave system which shall be combined with a continuous extruder for steel tubular objects. Phase III: Execution of the plan for commercialization of the technology by one of the industrial partners. However, since some of the goals of the phase I were not completed, an extension of nine months was granted and we continued extrusion experiments, designed and built semicontinuous microwave sintering unit.« less

Sintered electrode for solid oxide fuel cells

DOEpatents

Ruka, Roswell J.; Warner, Kathryn A.

1999-01-01

A solid oxide fuel cell fuel electrode is produced by a sintering process. An underlayer is applied to the electrolyte of a solid oxide fuel cell in the form of a slurry, which is then dried. An overlayer is applied to the underlayer and then dried. The dried underlayer and overlayer are then sintered to form a fuel electrode. Both the underlayer and the overlayer comprise a combination of electrode metal such as nickel, and stabilized zirconia such as yttria-stabilized zirconia, with the overlayer comprising a greater percentage of electrode metal. The use of more stabilized zirconia in the underlayer provides good adhesion to the electrolyte of the fuel cell, while the use of more electrode metal in the overlayer provides good electrical conductivity. The sintered fuel electrode is less expensive to produce compared with conventional electrodes made by electrochemical vapor deposition processes. The sintered electrodes exhibit favorable performance characteristics, including good porosity, adhesion, electrical conductivity and freedom from degradation.

Sintered electrode for solid oxide fuel cells

DOEpatents

Ruka, R.J.; Warner, K.A.

1999-06-01

A solid oxide fuel cell fuel electrode is produced by a sintering process. An underlayer is applied to the electrolyte of a solid oxide fuel cell in the form of a slurry, which is then dried. An overlayer is applied to the underlayer and then dried. The dried underlayer and overlayer are then sintered to form a fuel electrode. Both the underlayer and the overlayer comprise a combination of electrode metal such as nickel, and stabilized zirconia such as yttria-stabilized zirconia, with the overlayer comprising a greater percentage of electrode metal. The use of more stabilized zirconia in the underlayer provides good adhesion to the electrolyte of the fuel cell, while the use of more electrode metal in the overlayer provides good electrical conductivity. The sintered fuel electrode is less expensive to produce compared with conventional electrodes made by electrochemical vapor deposition processes. The sintered electrodes exhibit favorable performance characteristics, including good porosity, adhesion, electrical conductivity and freedom from degradation. 4 figs.

Effects of sintering process on wear and mechanical behavior properties of titanium carbide/hexagonal boron nitrid/steel 316L base nanocomposites

NASA Astrophysics Data System (ADS)

Sadooghi, Ali; Payganeh, Gholamhassan

2018-02-01

Powder metallurgy process is one of the approaches to manufacture nanocomposite samples, in which the product quality depends upon the pressure, temperature, and sintering time. In this manuscript, steel is selected as the base material together with 2% carbon-based reinforcing TiC particles, and 2% hBN particles as the self-lubricant material. The powders were mixed for 5 h in high ball milling, and compacted with two pressures of 350 and 450 MPa, sintered in the furnace for 2 and 4 h, and sintering temperatures of 1350 and 1450 °C were utilized. SEM, XRD, and EDX tests are performed to identify the nanocomposite structure, and DTA tests are carried out to specify the temperature graph of the material. Finally, hardness, wear, and bending tests are done to find the corresponding mechanical properties of the samples. As a result, the optimum process parameters, including pressure, temperature and sintering duration is achieved. Results show that adding the reinforcing particles into a steel matrix increase the hardness, as well as flexural strength of the nanocomposite product. Also, coefficient of friction shows a decreases.

Toward Better Personal Ballistic Protection

DTIC Science & Technology

2014-03-04

nanotube-reinforced zirconia-toughened alumina composites prepared by spark plasma sintering , Carbon, Vol 50, Iss 2 (2012), 706-717. [4] Bolduc M...attempt to optimize mechanical properties. The processing approaches investigated were pressureless sintering , hot pressing and hot isostatic...pressing (CIP) and pressureless sintering (PS). Test samples were made with high purity commercially available ceramic powder (over 99.5% for Al2O3). For

Phenomenological model of sintering of oxide nuclear fuel with doping admixtures

NASA Astrophysics Data System (ADS)

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.

Sintering of catalytic nanoparticles: particle migration or Ostwald ripening?

PubMed

Hansen, Thomas W; Delariva, Andrew T; Challa, Sivakumar R; Datye, Abhaya K

2013-08-20

Metal nanoparticles contain the active sites in heterogeneous catalysts, which are important for many industrial applications including the production of clean fuels, chemicals and pharmaceuticals, and the cleanup of exhaust from automobiles and stationary power plants. Sintering, or thermal deactivation, is an important mechanism for the loss of catalyst activity. This is especially true for high temperature catalytic processes, such as steam reforming, automotive exhaust treatment, or catalytic combustion. With dwindling supplies of precious metals and increasing demand, fundamental understanding of catalyst sintering is very important for achieving clean energy and a clean environment, and for efficient chemical conversion processes with atom selectivity. Scientists have proposed two mechanisms for sintering of nanoparticles: particle migration and coalescence (PMC) and Ostwald ripening (OR). PMC involves the mobility of particles in a Brownian-like motion on the support surface, with subsequent coalescence leading to nanoparticle growth. In contrast, OR involves the migration of adatoms or mobile molecular species, driven by differences in free energy and local adatom concentrations on the support surface. In this Account, we divide the process of sintering into three phases. Phase I involves rapid loss in catalyst activity (or surface area), phase II is where sintering slows down, and phase III is where the catalyst may reach a stable performance. Much of the previous work is based on inferences from catalysts that were observed before and after long term treatments. While the general phenomena can be captured correctly, the mechanisms cannot be determined. Advancements in the techniques of in situ TEM allow us to observe catalysts at elevated temperatures under working conditions. We review recent evidence obtained via in situ methods to determine the relative importance of PMC and OR in each of these phases of catalyst sintering. The evidence suggests that, in phase I, OR is responsible for the rapid loss of activity that occurs when particles are very small. Surprisingly, very little PMC is observed in this phase. Instead, the rapid loss of activity is caused by the disappearance of the smallest particles. These findings are in good agreement with representative atomistic simulations of sintering. In phase II, sintering slows down since the smallest particles have disappeared. We now see a combination of PMC and OR, but do not fully understand the relative contribution of each of these processes to the overall rates of sintering. In phase III, the particles have grown large and other parasitic phenomena, such as support restructuring, can become important, especially at high temperatures. Examining the evolution of particle size and surface area with time, we do not see a stable or equilibrium state, especially for catalysts operating at elevated temperatures. In conclusion, the recent literature, especially on in situ studies, shows that OR is the dominant process causing the growth of nanoparticle size. Consequently, this leads to the loss of surface area and activity. While particle migration could be controlled through suitable structuring of catalyst supports, it is more difficult to control the mobility of atomically dispersed species. These insights into the mechanisms of sintering could help to develop sinter-resistant catalysts, with the ultimate goal of designing catalysts that are self-healing.

Processing conditions and microstructural features of porous 316L stainless steel components by DMLS

NASA Astrophysics Data System (ADS)

Gu, Dongdong; Shen, Yifu

2008-12-01

Direct metal laser sintering (DMLS), due to its flexibility in materials and shapes, would be especially interesting to produce complex shaped porous metallic components. In the present work, processing conditions and microstructural characteristics of direct laser sintered porous 316L stainless steel components were studied. It was found that a partial melting mechanism of powders gave a high feasibility in obtaining porous sintered structures possessing porosities of ˜21-˜55%. Linear energy density (LED), which was defined by the ratio of laser power to scan speed, was used to tailor the laser sintering mechanism. A moderate LED of ˜3400-˜6000 J/m and a lower scan speed less than 0.06 m/s proved to be feasible. With the favorable sintering mechanism prevailed, lowering laser power or increasing scan speed, scan line spacing, and powder layer thickness generally led to a higher porosity. Metallurgical mechanisms of pore formation during DMLS were addressed. It showed that the presence of pores was through: (i) the formation of liquid bridges between partially melted particles during laser irradiation; and (ii) the growth of sintering necks during solidification, leaving residual pores between solidified metallic agglomerates.

Process for fabrication of large titanium diboride ceramic bodies

DOEpatents

Moorhead, Arthur J.; Bomar, E. S.; Becher, Paul F.

1989-01-01

A process for manufacturing large, fully dense, high purity TiB.sub.2 articles by pressing powders with a sintering aid at relatively low temperatures to reduce grain growth. The process requires stringent temperature and pressure applications in the hot-pressing step to ensure maximum removal of sintering aid and to avoid damage to the fabricated article or the die.

3500-hour durability testing of ceramic materials for automotive gas turbine engines

NASA Technical Reports Server (NTRS)

Carruthers, W. D.; Richerson, D. W.; Benn, K. W.

1980-01-01

A two-year durability program was performed by AiResearch Phoenix to evaluate four commercially available ceramic materials under simulated automotive gas turbine combustor discharge conditions. These conditions included extended cyclic thermal exposures up to 2500 F and 3500 hr. The four materials selected for evaluation were Norton NCX-34 hot pressed silicon nitride, AiResearch RBN 101 reaction bonded silicon nitride, Carborundum pressureless sintered alpha-SiC and Pure Carbon Co. (British Nuclear Fuels, Ltd.) Refel reaction sintered silicon carbide. These materials were initially exposed to 350 hr/1750 cycles at 1200 and 1370 C. Subsequent exposures to 1050, 2100 and 3500 hr were performed on those materials maintaining 50% of baseline strength after the initial exposure. Additional evaluations of exposed bars included dimensional and weight changes, dye penetrant, specific damping capacity changes, SEM fractography, and X-ray diffraction.

Magnesia tuned multi-walled carbon nanotubes–reinforced alumina nanocomposites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ahmad, Iftikhar, E-mail: ifahmad@ksu.edu.sa; Islam, Mohammad; Dar, Mushtaq Ahmad

2015-01-15

Magnesia tuned alumina ceramic nanocomposites, reinforced with multi-walled carbon nanotubes, were condensed using pressureless and hot-press sintering processes. Densification, microstructure and mechanical properties of the produced nanocomposites were meticulously investigated. Electron microscopy studies revealed the homogenous carbon nanotube dispersion within the alumina matrix and confirmed the retention of carbon nanotubes' distinctive tubular morphology and nanoscale features during the extreme mixing/sintering processes. Pressureless sintered nanocomposites showed meagre mechanical responses due to the poorly-integrated microstructures with a slight improvement upon magnesia addition. Conversely, both the magnesia addition and application of hot-press sintering technique resulted in the nanocomposite formation with near-theoretical densities (~more » 99%), well-integrated microstructures and superior mechanical properties. Hot-press sintered nanocomposites incorporating 300 and 600 ppm magnesia exhibited an increase in hardness (10 and 11%), flexural strength (5 and 10%) and fracture toughness (15 and 20%) with respect to similar magnesia-free samples. Compared to monolithic alumina, a decent rise in fracture toughness (37%), flexural strength (22%) and hardness (20%) was observed in the hot-press sintered nanocomposites tuned with merely 600 ppm magnesia. Mechanically superior hot-press sintered magnesia tailored nanocomposites are attractive for several load-bearing structural applications. - Highlights: • MgO tailored Al{sub 2}O{sub 3}–2 wt.% CNT nanocomposites are presented. • The role of MgO and sintering on nanocomposite structures and properties was studied. • Well-dispersed CNTs maintained their morphology/structure after harsh sintering. • Hot-pressing and MgO led nanocomposites to higher properties/unified structures. • MgO tuned composites showed higher toughness (37%) and strength (22%) than Al{sub 2}O{sub 3}.« less

Optimization of sintering conditions for cerium-doped yttrium aluminum garnet

NASA Astrophysics Data System (ADS)

Cranston, Robert Wesley McEachern

YAG:Ce phosphors have become widely used as blue/yellow light converters in camera projectors, white light emitting diodes (WLEDs) and general lighting applications. Many studies have been published on the production, characterization, and analysis of this optical ceramic but few have been done on determining optimal synthesis conditions. In this work, YAG:Ce phosphors were synthesized through solid state mixing and sintering. The synthesized powders and the highest quality commercially available powders were pressed and sintered to high densities and their photoluminescence (PL) intensity measured. The optimization process involved the sintering temperature, sintering time, annealing temperature and the level of Ce concentration. In addition to the PL intensity, samples were also characterized using particle size analysis, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The PL data was compared with data produced from a YAG:Ce phosphor sample provided by Christie Digital. The peak intensities of the samples were converted to a relative percentage of this industry product. The highest value for the intensity of the commercial powder was measured for a Ce concentration of 0.3 mole% with a sintering temperature of 1540°C and a sintering dwell time of 7 hours. The optimal processing parameters for the in-house synthesized powder were slightly different from those of commercial powders. The optimal Ce concentration was 0.4 mole% Ce, sintering temperature was 1560°C and sintering dwell time was 10 hours. These optimal conditions produced a relative intensity of 94.20% and 95.28% for the in-house and commercial powders respectively. Polishing of these samples resulted in an increase of 5% in the PL intensity.

Efficient sintering of nanocrystalline titanium dioxide films for dye solar cells via raster scanning laser

NASA Astrophysics Data System (ADS)

Mincuzzi, Girolamo; Vesce, Luigi; Reale, Andrea; Di Carlo, Aldo; Brown, Thomas M.

2009-09-01

By identifying the right combination of laser parameters, in particular the integrated laser fluence Φ, we fabricated dye solar cells (DSCs) with UV laser-sintered TiO2 films exhibiting a power conversion efficiency η =5.2%, the highest reported for laser-sintered devices. η is dramatically affected by Φ and a clear trend is reported. Significantly, DSCs fabricated by raster scanning the laser beam to sinter the TiO2 films are made as efficient as those with oven-sintered ones. These results, confirmed on three batches of cells, demonstrate the remarkable potential (noncontact, local, low cost, rapid, selective, and scalable) of scanning laser processing applied to DSC technology.

Sintering Uranium Dioxide of Domestic Production. Report No. 78; SINTERIZACION DE DIOXIDO DE URANIO DE PRODUCCION NACIONAL. Informe No. 78

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carrea, A.J.

1963-01-01

After a brief indication of the uranium- oxygen equilibrium and the methods for the preparation of UO/sub 2/, the sintering of UO/sub 2/ is considered. The effects of various sintering atmospheres on the properties of the product are discussed and tabulated. The method used for the processing of domestic ores for the preparation of UO/sub 2/ and the fabricition of the sintered UO/sub 2/are described. The properties of the product obtained are illustrated graphically. (J.S.R.)

Powder Metallurgy of Uranium Alloy Fuels for TRU-Burning Reactors Final Technical Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

McDeavitt, Sean M

2011-04-29

Overview Fast reactors were evaluated to enable the transmutation of transuranic isotopes generated by nuclear energy systems. The motivation for this was that TRU isotopes have high radiotoxicity and relatively long half-lives, making them unattractive for disposal in a long-term geologic repository. Fast reactors provide an efficient means to utilize the energy content of the TRUs while destroying them. An enabling technology that requires research and development is the fabrication metallic fuel containing TRU isotopes using powder metallurgy methods. This project focused upon developing a powder metallurgical fabrication method to produce U-Zr-transuranic (TRU) alloys at relatively low processing temperatures (500ºCmore » to 600ºC) using either hot extrusion or alpha-phase sintering for charecterization. Researchers quantified the fundamental aspects of both processing methods using surrogate metals to simulate the TRU elements. The process produced novel solutions to some of the issues relating to metallic fuels, such as fuel-cladding chemical interactions, fuel swelling, volatility losses during casting, and casting mold material losses. Workscope There were two primary tasks associated with this project: 1. Hot working fabrication using mechanical alloying and extrusion • Design, fabricate, and assemble extrusion equipment • Extrusion database on DU metal • Extrusion database on U-10Zr alloys • Extrusion database on U-20xx-10Zr alloys • Evaluation and testing of tube sheath metals 2. Low-temperature sintering of U alloys • Design, fabricate, and assemble equipment • Sintering database on DU metal • Sintering database on U-10Zr alloys • Liquid assisted phase sintering on U-20xx-10Zr alloys Appendices Outline Appendix A contains a Fuel Cycle Research & Development (FCR&D) poster and contact presentation where TAMU made primary contributions. Appendix B contains MSNE theses and final defense presentations by David Garnetti and Grant Helmreich outlining the beginning of the materials processing setup. Also included within this section is a thesis proposal by Jeff Hausaman. Appendix C contains the public papers and presentations introduced at the 2010 American Nuclear Society Winter Meeting. Appendix A—MSNE theses of David Garnetti and Grant Helmreich and proposal by Jeff Hausaman A.1 December 2009 Thesis by David Garnetti entitled “Uranium Powder Production Via Hydride Formation and Alpha Phase Sintering of Uranium and Uranium-Zirconium Alloys for Advanced Nuclear Fuel Applications” A.2 September 2009 Presentation by David Garnetti (same title as document in Appendix B.1) A.3 December 2010 Thesis by Grant Helmreich entitled “Characterization of Alpha-Phase Sintering of Uranium and Uranium-Zirconium Alloys for Advanced Nuclear Fuel Applications” A.4 October 2010 Presentation by Grant Helmreich (same title as document in Appendix B.3) A.5 Thesis Proposal by Jeffrey Hausaman entitled “Hot Extrusion of Alpha Phase Uranium-Zirconium Alloys for TRU Burning Fast Reactors” Appendix B—External presentations introduced at the 2010 ANS Winter Meeting B.1 J.S. Hausaman, D.J. Garnetti, and S.M. McDeavitt, “Powder Metallurgy of Alpha Phase Uranium Alloys for TRU Burning Fast Reactors,” Proceedings of 2010 ANS Winter Meeting, Las Vegas, Nevada, USA, November 7-10, 2010 B.2 PowerPoint Presentation Slides from C.1 B.3 G.W. Helmreich, W.J. Sames, D.J. Garnetti, and S.M. McDeavitt, “Uranium Powder Production Using a Hydride-Dehydride Process,” Proceedings of 2010 ANS Winter Meeting, Las Vegas, Nevada, USA, November 7-10, 2010 B.4. PowerPoint Presentation Slides from C.3 B.5 Poster Presentation from C.3 Appendix C—Fuel cycle research and development undergraduate materials and poster presentation C.1 Poster entitled “Characterization of Alpha-Phase Sintering of Uranium and Uranium-Zirconium Alloys” presented at the Fuel Cycle Technologies Program Annual Meeting C.2 April 2011 Honors Undergraduate Thesis by William Sames, Research Fellow, entitled “Uranium Metal Powder Production, Particle Distribution Analysis, and Reaction Rate Studies of a Hydride-Dehydride Process"« less

Formation of nickel and copper ferrites in ceramics: a potential reaction in the reuse of iron-rich sludge incineration ash.

PubMed

Shih, Kaimin

2012-12-01

This study investigates potential solid-state reactions for the stabilization of hazardous metals when reusing the incineration ash from chemically enhanced primary treatment (CEPT) sludge to fabricate ceramic products. Nickel and copper were used as examples of hazardous metals, and the iron content in the reaction system was found to play a major role in incorporating these hazardous metals into their ferrite phases (NiFe2O4 and CuFe2O4). The results from three-hour sintering experiments on NiO + Fe2O3 and CuO + Fe2O3 systems clearly demonstrate the potential for initiating metal incorporation mechanisms using an iron-containing precursor at attainable ceramic sintering temperatures (above 750 degrees C). Both ferrite phases were examined using a prolonged leaching experiment modified from the widely used toxicity characteristic leaching procedure (TCLP) to evaluate their long-term metal leachability. The leaching results indicate that both the NiFe2O4 and the CuFe2O4 products were significantly superior to their oxide forms in immobilizing hazardous metals.

Spark plasma sintering of highly dense fine-grained mineral aggregates

NASA Astrophysics Data System (ADS)

Koizumi, S.; Suzuki, T. S.; Sakka, Y.; Hiraga, T.

2017-12-01

To obtain highly dense and fine-grained mineral aggregates, which are suitable for laboratory measurements of their physical and chemical properties, we applied spark plasma sintering (SPS) to synthetic mineral powders and powders originated from naturally derived crystals. SPS is an emerging consolidation technique which has been applied to various metals and ceramics and rarely to geomaterials (e.g., Guignard et al., 2011). The technique uses spark plasma created by a pulse direct current during heat treatment of powders in a graphite die. It has been found that the technique provides better densification with little grain growth during sintering compared to a conventional sintering technique in many materials. To obtain ideal highly dense fine-grained materials, it is essential to prepare starting powders suitable for the sintering and also to find appropriate sintering conditions of applied uniaxial pressures, pulsed current patterns and heating rates. We prepared synthetic mineral powers through solid state reaction of source powders at high temperature well developed by our group (Koizumi et al. 2010). We also used jet milling at wet condition and subsequent elutriation to prepare olivine powders with sub-micron particle size and equiaxed particle shape. At heating rate of ≦10°C/min and an achievement of highest temperature of 1150°C, Fe-free olivine aggregate with average grain size of 200 nm with porosity of 0.003% was obtained. We also could obtain olivine aggregate, which was sintered from powders of Horoman peridotite, with average grain size of 500 nm and porosity of 0.2%. We will show results of other minerals including major rock forming minerals of the Earth's crust.

Volatile organic compound constituents from an integrated iron and steel facility.

PubMed

Tsai, Jiun-Horng; Lin, Kuo-Hsiung; Chen, Chih-Yu; Lai, Nina; Ma, Sen-Yi; Chiang, Hung-Lung

2008-09-15

This study measured the volatile organic compound (VOC) constituents of four processes in an integrated iron and steel industry; cokemaking, sintering, hot forming, and cold forming. Toluene, 1,2,4-trimethylbenzene, isopentane, m,p-xylene, 1-butene, ethylbenzene, and benzene were the predominant VOC species in these processes. However, some of the chlorinated compounds were high (hundreds ppbv), i.e., trichloroethylene in all four processes, carbon tetrachloride in the hot forming process, chlorobenzene in the cold forming process, and bromomethane in the sintering process. In the sintering process, the emission factors of toluene, benzene, xylene, isopentane, 1,2,4-trimethylbenzene, and ethylbenzene were over 9 g/tonne-product. In the vicinity of the manufacturing plant, toluene, isopentane, 1,2,4-trimethylbenzene, xylene and ethylbenzene were high. Toluene, 1,2,4-trimethylbenzene, xylene, 1-butene and isopentane were the major ozone formation species. Aromatic compounds were the predominant VOC groups, constituting 45-70% of the VOC concentration and contributing >70% to the high ozone formation potential in the stack exhaust and workplace air. The sequence of VOC concentration and ozone formation potential was as follows: cold forming>sintering>hot forming>cokemaking. For the workplace air, cokemaking was the highest producer, which was attributed to the fugitive emissions of the coke oven and working process release.

Effect of Mg(2+) doping on beta-alpha phase transition in tricalcium phosphate (TCP) bioceramics.

PubMed

Frasnelli, Matteo; Sglavo, Vincenzo M

2016-03-01

The beta to alpha transition in tricalcium phosphate (TCP) bioceramics containing different amount of magnesium was studied in the present work. Mg-doped TCP powder was obtained by solid-state reaction starting from pure calcium carbonate, ammonium phosphate dibasic and magnesium oxide powders. The β to α transformation temperature was identified by dilatometric and thermo-differential analyses. Small pellets produced by uniaxial pressing samples were employed to study the influence of Mg(2+) on the transition kinetic, after sintering at 1550°C and subsequent slow or fast cooling down to room temperature. The evolution of β- and α-TCP crystalline phases during each thermal treatment was determined by X-ray powder diffraction analysis combined with Rietveld method-based software An annealing treatment, suitable to reconvert metastable α phase to the more clinically suitable β phase, was also investigated. It is shown that the presence of magnesium within the TCP lattice strongly influences the kinetic of the β⇆α phase transition, promoting the spontaneous α→β reconversion even upon fast cooling, or slowing down the β→α transition during heating. Similarly, it allows the α→β transformation in TCP sintered components by optimized annealing treatment at 850°C. This work concerns the effect of Mg(2+) doping on the β→α phase reconstructive transition in tricalcium phosphate (TCP), one of the most important bio-resorbable materials for bone tissue regeneration. The transition occurs upon the sintering process and is has been shown to be strongly irreversible upon cooling, leading to technological issues such as poor mechanical properties and excessive solubility due to the presence of metastable α-phase. This paper points out the kinetic contribution of Mg(2+) on the spontaneous α→β reconversion also upon fast cooling (i.e. quenching). Moreover, an annealing treatment has been shown to be beneficial to remove the retained α-phase in sintered TCP components, the presence of Mg promoting the reconversion process. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Multielement mapping of alpha-SiC by scanning Auger microscopy

NASA Technical Reports Server (NTRS)

Browning, Ray; Smialek, James L.; Jacobson, Nathan S.

1987-01-01

Fine second-phase particles, numerous in sintered alpha-SiC, were analyzed by scanning Auger microscopy and conventional techniques. The Auger analysis utilized computer-controlled data acquisition, multielement correlation diagrams, and a high spatial resolution of 100 nm. This procedure enabled construction of false color maps and the detection of fine compositional details within these particles. Carbon, silicon oxide, and boron-rich particles (qualitatively as BN or B4C) predominated. The BN particles, sometimes having a carbon core, are believed to result from reaction between B4C additives and nitrogen sintering atmospheres.

Reaction bonded silicon nitride prepared from wet attrition-milled silicon. [fractography

NASA Technical Reports Server (NTRS)

Herball, T. P.; Glasgow, T. K.; Shaw, N. J.

1980-01-01

Silicon powder wet milled in heptane was dried, compacted into test bar shape, helium-sintered, and then reaction bonded in nitrogen-4 volume percent hydrogen. As-nitrided bend strengths averaged approximately 290 MPa at both room temperature and 1400 C. Fracture initiation appeared to be associated with subsurface flaws in high strength specimens and both subsurface and surface flaws in low strength specimens.

Reaction bonded silicon nitride prepared from wet attrition-milled silicon

NASA Technical Reports Server (NTRS)

Herbell, T. P.; Glasgow, T. K.; Shaw, N. J.

1980-01-01

Silicon powder wet milled in heptane was dried, compacted into test bar shape, helium-sintered, and then reaction bonded in nitrogen-4 vol% hydrogen. As-nitrided bend strengths averaged approximately 290 MPa at both room temperature and 1400 C. Fracture initiation appeared to be associated with subsurface flaws in high-strength specimens and both subsurface and surface flaws in low-strength specimens.

Fabrication of a porous material with a porosity gradient by a pulsed electric current sintering process

NASA Astrophysics Data System (ADS)

Suk, Myung-Jin; Choi, Sung-II; Kim, Ji-Soon; Kim, Young Do; Kwon, Young-Soon

2003-12-01

A porous structure with a porosity gradient can be applied to the preparation of continuous FGM, where liquid or chemical vapor of the second phase is infiltrated into the graded pores. It also has applications in skeletal implant materials and ultrafiltration media. An attempt was made to fabricate a porous material with a porosity gradient by means of a pulsed electric current sintering (PECS) process. The present work describes not only the measured value of the temperature difference between the upper and lower part of the specimen, which brings about a gradual change in pore distribution, but also the sintering characteristics of the porous structure obtained by the pressureless PECS process.

Effects of sintering atmosphere on the physical and mechanical properties of modified BOF slag glass

NASA Astrophysics Data System (ADS)

Dai, Wen-bin; Li, Yu; Cang, Da-qiang; Zhou, Yuan-yuan; Fan, Yong

2014-05-01

This study proposes an efficient way to utilize all the chemical components of the basic oxygen furnace (BOF) slag to prepare high value-added glass-ceramics. A molten modified BOF slag was converted from the melting BOF slag by reducing it and separating out iron component in it, and the modified BOF slag was then quenched in water to form glasses with different basicities. The glasses were subsequently sintered in the temperature range of 600-1000°C in air or nitrogen atmosphere for 1 h. The effects of different atmospheres on the physical and mechanical properties of sintered samples were studied by using differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM) and by conducting experiment on evaluating the sintering shrinkage, water absorption and bulk density. It is found that the kinetics of the sintering process is significantly affected by sintering atmosphere. In particular, compared with sintering in air atmosphere, sintering in N2 atmosphere promotes the synergistic growth of pyroxene and melilite crystalline phases, which can contribute to better mechanical properties and denser microstructure.

Processing of uranium dioxide nuclear fuel pellets using spark plasma sintering

NASA Astrophysics Data System (ADS)

Ge, Lihao

Uranium dioxide (UO2), one of the most common nuclear fuels, has been applied in most of the nuclear plant these days for electricity generation. The main objective of this research is to introduce a novel method for UO 2 processing using spark plasma sintering technique (SPS). Firstly, an investigation into the influence of processing parameters on densification of UO2 powder during SPS is presented. A broad range of sintering temperatures, hold time and heating rates have been systematically varied to investigate their influence on the sintered pellet densification process. The results revealed that up to 96% theoretical density (TD) pellets can be obtained at a sintering temperature of 1050 °C for 30s hold time and a total run time of only 10 minutes. A systematic study is performed by varying the sintering temperature between 750°C to 1450°C and hold time between 0.5 min to 20 min to obtain UO2 pellets with a range of densities and grain sizes. The microstructure development in terms of grain size, density and porosity distribution is investigated. The Oxygen/Uranium (O/U) ratio of the resulting pellets is found to decrease after SPS. The mechanical and thermal properties of UO2 are evaluated. For comparable density and grain size, Vickers hardness and Young's modulus are in agreement with the literature value. The thermal conductivity of UO2 increases with the density but the grain size in the investigated range has no significant influence. Overall, the mechanical and thermal properties of UO2 are comparable with the one made using conventional sintering methods. Lastly, the influence of chromium dioxide (Cr2O3) and zirconium diboride (ZrB2) on the grain size of doped UO 2 fuel pellet is performed to investigate the feasibility of producing large-grain-size nuclear fuel using SPS. The benefits of using SPS over the conventional sintering of UO2 are summarized. The future work of designing macro-porous UO2 pellet and thorium dioxide (ThO 2) cored UO2 pellet is also proposed.

Sintering in Ceramics and Solid Oxide Fuel Cells

NASA Astrophysics Data System (ADS)

Hunt, Clay Dale

Nature's propensity to minimize energy, and the change in energy with respect to position, drives diffusion. Diffusion is a means by which mass transport resulting in the bonding of the particles of a powder compact can be achieved without melting. This phenomenon occurs in powdered materials near their melting temperature, and is referred to as "sintering". Because of the extreme melting temperature of some materials, sintering might be the only practical means of processing. The complexity and subtlety of sintering ceramics motivated the evaluation of empirical data and existing sintering models. This project examined polycrystalline cubic-zirconia sintering with and without transition-metal oxide additions that change sintering behavior. This study was undertaken to determine how sintering aids affect the driving force, and activation energy, the energy barrier that must be overcome in order for an atom or ion to diffuse, of the densification occurring during sintering. Examination of commercially-available cubic-zirconia powder sintering behavior was undertaken with dilatometry, which allows monitoring of the length change a material undergoes as it sinters, and with scanning electron microscopy, which facilitates the study of sintered-sample microstructure. MATLAB algorithms quantifying sintering results were developed. Results from this work include proposed definitions of a 26-year-old undefined function of density factor in a well-accepted mathematical model of sintering. These findings suggest activation energy is not changing with density, as is suggested by recent published results. The first numerical integration of the studied sintering model has been performed. With these tools, a measure of the activation energy of densification of cubic-zirconia with and without the addition of cobalt-oxide as a sintering aid has been performed. The resulting MATLAB algorithms can be used in future sintering studies. It is concluded that sintering enhancement achieved with cobalt-oxide addition comes from reduction in activation energy of densification of cubic-zirconia. Further, it is suggested that the activation energy of densification does not change with material density. This conclusion is supported by the sensitivity of the numerical integration of the aforementioned sintering model to changes in activation energy.

Mathematical modeling of phase change electrodes and application to a novel titanium extraction process

NASA Astrophysics Data System (ADS)

Kar, Pritish

Titanium and its alloys have excellent engineering properties but their applications are limited because they are expensive and a good percentage of this cost results from the extraction process. The national agencies of many countries around the world have invested a lot of resources to develop a more cost-effective titanium extraction process. A result of one such research efforts is the Fray-Farthing-Chen (FFC) process in which pellets of titanium dioxide are made the cathode in an electrochemical cell with a graphite anode and an electrolyte of molten CaCl2 at 900°C. After electro-deoxidation, the pellets are reduced to titanium with oxygen in solid solution. From this short description, this one step process provides distinct advantages over the current process of extracting titanium known as the Kroll process that takes several days to complete. For investigation of the FFC process theoretically, a coupled electrochemical and diffusion based model was set-up to simulate the linear sweep voltammograms that was developed by collaborators working on lab-scale experiments on the FCC process. Using this model, a parameter called "deltadc" (that is the product of diffusion coefficients of oxygen in the phases, Ti3O5 and Ti2O3 and the stoichiometric range of these phases) was determined. The results suggest a reaction of first-order in the concentration of oxygen in the solid phase. For modeling the reaction of an individual sintered pellet of TiO 2 as it undergoes electro-deoxidation in a molten salt bath of CaCl 2, a similarity of this process with the operation of a lithium ion battery was exploited. Using the model, a number of parameters of physical importance, namely thickness of the sintered pellets, porosity of the pellets and the radius of the particles making up the pellets and the optimum values for the these parameters were proposed based on the simulation data. It is also shown that if the reduction is started with a pellet of partially reduced titanium dioxide (such as by reducing with hydrogen), one can avoid titanate formation. The work described in this dissertation will hopefully help in the development of a more cost-effective titanium extraction process.

Metal stabilization mechanism of incorporating lead-bearing sludge in kaolinite-based ceramics.

PubMed

Lu, Xingwen; Shih, Kaimin

2012-02-01

The feasibility and mechanism of incorporating simulated lead-laden sludge into low-cost ceramic products was investigated by observing the reaction of lead with two kaolinite-based precursors under sintering conditions. To investigate the phase transformation process of lead, lead oxide (PbO) mixed with a kaolinite or mullite precursor were fired at 500-950°C for 3h. Detailed X-ray diffraction analysis of sintered products revealed that both precursors had crystallochemically incorporated lead into the lead feldspar (PbAl(2)Si(2)O(8)) crystalline structure. By mixing lead oxide with kaolinite, lead feldspar begins to crystallize at 700°C; maximum incorporation of lead into this structure occurred at 950°C. However, two intermediate phases, Pb(4)Al(4)Si(3)O(16) and a polymorph of lead feldspar, were detected at temperatures between 700 and 900°C. By sintering lead oxide with the mullite precursor, lead feldspar was detected at temperatures above 750°C, and an intermediate phase of Pb(4)Al(4)Si(3)O(16) was observed in the temperature range of 750-900°C. This study compared the lead leachabilities of PbO and lead feldspar using a prolonged leaching test (at pH 2.9 for 23d) modified from the toxicity characteristic leaching procedure. The results indicate the superiority of lead feldspar in stabilizing lead and suggest a promising and reliable strategy to stabilize lead in ceramic products. Copyright © 2011 Elsevier Ltd. All rights reserved.

Nickel stabilization efficiency of aluminate and ferrite spinels and their leaching behavior.

PubMed

Shih, Kaimin; White, Tim; Leckie, James O

2006-09-01

Stabilization efficiencies of spinel-based construction ceramics incorporating simulated nickel-laden waste sludge were evaluated and the leaching behavior of products investigated. To simulate the process of immobilization, nickel oxide was mixed alternatively with gamma-alumina, kaolinite, and hematite. These tailoring precursors are commonly used to prepare construction ceramics in the building industry. After sintering from 600 to 1480 degrees C at 3 h, the nickel aluminate spinel (NiAl204) and the nickel ferrite spinel (NiFe204) crystallized with the ferrite spinel formation commencing about 200-300 degrees C lower than for the aluminate spinel. All the precursors showed high nickel incorporation efficiencies when sintered at temperatures greater than 1250 degrees C. Prolonged leach tests (up to 26 days) of product phases were carried out using a pH 2.9 acetic acid solution, and the spinel products were invariably superior to nickel oxide for immobilization over longer leaching periods. The leaching behavior of NiAl2O4 was consistent with congruent dissolution without significant reprecipitation, but for NiFe2O4, ferric hydroxide precipitation was evident. The major leaching reaction of sintered kaolinite-based products was the dissolution of cristobalite rather than NiAl2O4. This study demonstrated the feasibility of transforming nickel-laden sludge into spinel phases with the use of readily available and inexpensive ceramic raw materials, and the successful reduction of metal mobility under acidic environments.

Microwave dielectric properties of CaCu3Ti4O12-Al2O3 composite

NASA Astrophysics Data System (ADS)

Rahman, Mohd Fariz Ab; Abu, Mohamad Johari; Karim, Saniah Ab; Zaman, Rosyaini Afindi; Ain, Mohd Fadzil; Ahmad, Zainal Arifin; Mohamed, Julie Juliewatty

2016-07-01

(1-x)CaCu3Ti4O12 + (x)Al2O3 composite (0 ≤ x ≤0.25) was prepared via conventional solid-state reaction method. The fabrication of sample was started with synthesizing stoichiometric CCTO from CaCO3, CuO and TiO2 powders, then wet-mixed in deionized water for 24 h. The process was continued with calcined CCTO powder at 900 °C for 12 h before sintered at 1040 °C for 10 h. Next, the calcined CCTO powder with different amount of Al2O3 were mixed for 24 h, then palletized and sintered at 1040 °C for 10. X-ray diffraction analysis on the sintered samples showed that CCTO powder was in a single phase, meanwhile the trace of secondary peaks which belong to CaAl2O4 and Corundum (Al2O3) could be observed in the other samples Scanning electron microscopy analysis showed that the grain size of the sample is firstly increased with addition of Al2O3 (x = 0.01), then become smaller with the x > 0.01. Microwave dielectric properties showed that the addition of Al2O3 (x = 0.01) was remarkably reduced the dielectric loss while slightly increased the dielectric permittivity. However, further addition of Al2O3 was reduced both dielectric loss and permittivity at least for an order of magnitude.

New nano-sized Al2O3-BN coating 3Y-TZP ceramic composites for CAD/CAM-produced all-ceramic dental restorations. Part I. Fabrication of powders.

PubMed

Yang, Se Fei; Yang, Li Qiang; Jin, Zhi Hao; Guo, Tian Wen; Wang, Lei; Liu, Hong Chen

2009-06-01

Partially sintered 3 mol % yttria-stabilized tetragonal zirconium dioxide (ZrO(2), zirconia) polycrystal (3Y-TZP) ceramics are used in dental posterior restorations with computer-aided design-computer-aided manufacturing (CAD/CAM) techniques. High strength is acquired after sintering, but shape distortion of preshaped compacts during their sintering is inevitable. The aim of this study is to fabricate new machinable ceramic composites with strong mechanical properties that are fit for all-ceramic dental restorations. Aluminum oxide (Al(2)O(3))-coated 3Y-TZP powders were first prepared by the heterogeneous precipitation method starting with 3Y-TZP, Al(NO(3))(3) . 9H(2)O, and ammonia, then amorphous boron nitride (BN) was produced and the as-received composite powders were coated via in situ reaction with boric acid and urea. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) were used to analyze the status of Al(2)O(3)-BN on the surface of the 3Y-TZP particles. TEM micrographs show an abundance of Al(2)O(3) particles and amorphous BN appearing uniformly on the surface of the 3Y-TZP particles after the coating process. The size of the Al(2)O(3) particles is about 20 nm. The XRD pattern shows clearly the peak of amorphous BN among the peaks of ZrO(2).

Fabrication of Titanium Oxide-Based Composites by Reactive SPS Sintering and Their Thermoelectric Properties

NASA Astrophysics Data System (ADS)

Fuda, K.; Shoji, T.; Kikuchi, S.; Kunihiro, Y.; Sugiyama, S.

2013-07-01

Titanium oxide-based composites containing (1) Nb, (2) Nb and Sr, and (3) Sr and La were fabricated by a combination of wet processing and reactive spark plasma sintering in which the metal oxide components were reduced by reaction with titanium nitride. If only TiO2 was used as the starting material, several Magneli-type phases of oxygen-deficient titanium oxides were obtained. When mixed with Nb ions with Ti:Nb = 0.9:0.1, microsegregation of Nb ions was observed (case 1). If Sr was added, a perovskite, SrTiO3 (STO) phase occurred (case 2), which contained La ions in the case of La addition (case 3). The sintered compacts consisted largely of grains of about 1 μm in size. In the case of Ti-Nb combination (case 1), a unique stripe pattern also appeared inside the grains. The electrical conductivity increased monotonically with increasing temperature in the case of the pure Magneli phases and the Nb-containing composite, whereas bow-shaped temperature dependences with a maximum were observed in the case of the composites containing STO phases. The Seebeck coefficients were commonly negative, and the absolute values increased with temperature. The thermal conductivity was between 2 W m-1 K-1 and 4 W m-1 K-1 in the temperature range from room temperature to 800°C. A maximum ZT of 0.34 was achieved at 800°C (case 2).

Development of Bulk Nanocrystalline Tungsten Alloys for Fusion Reactor Structures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fang, Zhigang Zak

This project developed a technology for manufacturing bulk ultrafine tungsten materials that are at or near full density for fusion reactor structural applications, aiming to improve ductility and toughness of tungsten before and after irradiation. The project involved the development of fabrication processes for making bulk ultrafine grained W, the development of new alloys of ultrafine grained W and evaluations of properties of these specific materials. The goal of this fabrication process is to produce fully dense bulk W with ultrafine grain sizes, with uniform distributions of grain size and additives. To date there is no known process that couldmore » be used to make ultrafine grained tungsten in a fully dense state and in a cost-acceptable fashion. The specific technology described in this proposal for making ultrafine grained tungsten involves a suite of nano-particle processing and sintering techniques. The program also developed new alloys of ultrafine grained W, e.g. W-(Ta,V,Ti)-TiC alloys to improve ductility and toughness before and after irradiation. By completing this project, we achieved the following objectives: • Demonstrated experimentally the feasibility of producing bulk ultrafine grained tungsten alloys (at or near 100% dense, <1000 nm grain size) using the proposed process • Demonstrated the proposed ultrafine grained W alloys, namely, W-(Ta, V, Ti)-TiC, can indeed be made using the proposed process • Demonstrated that the properties of nano tungsten alloys meet the requirements for fusion reactor applications. The overall goal was to harness the potential of ultrafine grained W produced using the proposed processes as the core structural materials for future fusion reactors. The project was very successful overall, meeting all milestones and surpassing project goals in terms of process development and material’s blistering resistance properties. A novel process similar to the conventional press-and-sinter powder metallurgy method was developed for producing ultrafine grain tungsten from nanosize tungsten powders. Grain growth was significantly controlled during sintering by certain alloy compositions, particularly Ti, and most compositions sintered to maximum densification. To optimize this process, the effect of processing parameters on the densification and grain growth of nano-W powders was investigated. Near-fully densified tungsten was obtained at sintering temperatures between 1100 and 1300 °C, and both Ar and H2 sintering atmospheres were investigated. The Ar sintering atmosphere was determined to more favorably promote densification and minimize grain growth. The nanosized tungsten powder compacts were subjected to reduction in H2 as a part of the sintering cycle. The reduction temperature was found to have significant effects on the sintering of nano-W powder, primarily as a result of grain coarsening, which was seen at temperatures as low as 700 °C. In an effort to inhibit grain growth, the effect of Ti-based additives on the densification and grain growth of nano-W powders was investigated in this project. The addition of 1 wt.% Ti into tungsten led to more than a 63% decrease in average grain size of sintered samples at comparable density levels. Compared to conventional high temperature sintering, a lower temperature sintering cycle for a longer hold time resulted in both near-full density and fine grain size. The roles of the Ti additives include not only the inhibition of grain growth, but also the potential absorption of oxygen from W particles. The project has resulted in the publication; thus far, of six peer reviewed journal articles and seven conference presentations, as well as a master’s thesis. Two additional journal articles are currently in preparation. Presentations and articles were a particular focus of the second half of the project, once significant experimentation had been performed and analyzed. As part of our efforts to disseminate information of our results, the W research teams with Prof. Fang had a strong presence at multiple international conferences during 2015 and 2016. Several research groups in the US are now performing experiments using the ultrafine grained W materials.« less

Consolidation of materials by pulse-discharge processes

NASA Astrophysics Data System (ADS)

Strizhakov, E. L.; Nescoromniy, S. V.

2017-07-01

The article presents the research and the analysis of the pulse-discharge processes of capacitor discharge sintering: CD Stud Welding, capacitor discharge percussion welding (CDPW), high-voltage capacitor welding with an inductive-dynamic drive (HVCW with IDD), pulse electric current sintering (PECS) of powders. The comparative analysis of the impact parameter is presented.

Structural properties and gas sensing behavior of sol-gel grown nanostructured zinc oxide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rajyaguru, Bhargav; Gadani, Keval; Kansara, S. B.

2016-05-06

In this communication, we report the results of the studies on structural properties and gas sensing behavior of nanostructured ZnO grown using acetone precursor based modified sol-gel technique. Final product of ZnO was sintered at different temperatures to vary the crystallite size while their structural properties have been studied using X-ray diffraction (XRD) measurement performed at room temperature. XRD results suggest the single phasic nature of all the samples and crystallite size increases from 11.53 to 20.96 nm with increase in sintering temperature. Gas sensing behavior has been studied for acetone gas which indicates that lower sintered samples are moremore » capable to sense the acetone gas and related mechanism has been discussed in the light of crystallite size, crystal boundary density, defect mechanism and possible chemical reaction between gas traces and various oxygen species.« less

Improved silicon carbide for advanced heat engines

NASA Technical Reports Server (NTRS)

Whalen, Thomas J.; Mangels, J. A.

1986-01-01

The development of silicon carbide materials of high strength was initiated and components of complex shape and high reliability were formed. The approach was to adapt a beta-SiC powder and binder system to the injection molding process and to develop procedures and process parameters capable of providing a sintered silicon carbide material with improved properties. The initial effort was to characterize the baseline precursor materials, develop mixing and injection molding procedures for fabricating test bars, and characterize the properties of the sintered materials. Parallel studies of various mixing, dewaxing, and sintering procedures were performed in order to distinguish process routes for improving material properties. A total of 276 modulus-of-rupture (MOR) bars of the baseline material was molded, and 122 bars were fully processed to a sinter density of approximately 95 percent. Fluid mixing techniques were developed which significantly reduced flaw size and improved the strength of the material. Initial MOR tests indicated that strength of the fluid-mixed material exceeds the baseline property by more than 33 percent. the baseline property by more than 33 percent.

Sintered Intermetallic Reinforced 434L Ferritic Stainless Steel Composites

NASA Astrophysics Data System (ADS)

Upadhyaya, A.; Balaji, S.

2009-03-01

The present study examines the effect of aluminide (Ni3Al, Fe3Al) additions on the sintering behavior of ferritic 434L stainless steels during solid-state sintering (SSS) and supersolidus liquid-phase sintering (SLPS). 434L stainless steel matrix composites containing 5 and 10 wt pct of each aluminide were consolidated at 1200 °C (SSS) and 1400 °C (SLPS). The effects of sintering and aluminide additions on the densification, microstructural evolution, mechanical, tribological, and corrosion behavior of sintered ferritic (434L) stainless steels were investigated. The performances of the 434L-aluminide composites were compared with the straight 434L stainless steels processed at similar conditions. Supersolidus sintering resulted in significant improvement in densification, mechanical, wear, and corrosion resistance in both straight 434L and 434L-aluminide composites. Fe3Al additions to 434L stainless steels result in improved wear resistance without significant degradation of corrosion resistance in 3.56 wt pct NaCl solution.

Taguchi Analysis on the Effect of Process Parameters on Densification During Spark Plasma Sintering of HfB2-20SiC (Preprint)

DTIC Science & Technology

2011-11-01

30 kN pressure and heating rate of 100 K/min. Introduction Boride , carbides and nitrides of the group IVB and VB transition metals are considered...10. Sciti D., Silvestroni L., Nygren M. Spark plasma sintering of Zr- and Hf- borides with decreasing amounts of MoSi2 as sintering aid Journal of

Reactive solid surface morphology variation via ionic diffusion.

PubMed

Sun, Zhenchao; Zhou, Qiang; Fan, Liang-Shih

2012-08-14

In gas-solid reactions, one of the most important factors that determine the overall reaction rate is the solid morphology, which can be characterized by a combination of smooth, convex and concave structures. Generally, the solid surface structure varies in the course of reactions, which is classically noted as being attributed to one or more of the following three mechanisms: mechanical interaction, molar volume change, and sintering. Here we show that if a gas-solid reaction involves the outward ionic diffusion of a solid-phase reactant then this outward ionic diffusion could eventually smooth the surface with an initial concave and/or convex structure. Specifically, the concave surface is filled via a larger outward diffusing surface pointing to the concave valley, whereas the height of the convex surface decreases via a lower outward diffusion flux in the vertical direction. A quantitative 2-D continuum diffusion model is established to analyze these two morphological variation processes, which shows consistent results with the experiments. This surface morphology variation by solid-phase ionic diffusion serves to provide a fourth mechanism that supplements the traditionally acknowledged solid morphology variation or, in general, porosity variation mechanisms in gas-solid reactions.

The Preparation and Characterization of Materials.

ERIC Educational Resources Information Center

Wold, Aaron

1980-01-01

Presents several examples illustrating different aspects of materials problems, including problems associated with solid-solid reactions, sintering and crystal growth, characterization of materials, preparation and characterization of stoichiometric ferrites and chromites, copper-sulfur systems, growth of single crystals by chemical vapor…

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, I-Wei

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 densemore » 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 of flash sintering, which is a rapid sintering process initiated by a large electrical loading.« less

Grain refinement in heavy rare earth element-free sintered Nd–Fe–B magnets by addition of a small amount of molybdenum

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Jin Woo; Lee, Won Suk; Byun, Jong Min

2015-05-07

We employed a modified refractory-metal-addition method to achieve higher coercivity and remanence in heavy rare earth element (HREE)-free Nd–Fe–B sintered magnets. This process involved inducing the formation of a homogeneous secondary phase at the grain boundaries during sintering, making it possible to control the intergrain diffusion by adding small amounts of Mo, a refractory metal. To control the microstructure of the secondary phase effectively, a metal organic compound of the refractory metal was coated on the surfaces of the particles of an HREE-free Nd–Fe–B powder. The average grain size after this process was 5.60 μm, which was approximately 1.8 μm smaller thanmore » that of the HREE-free sintered Nd–Fe–B magnets (7.4 μm). The coercivity of the magnets prepared through this process could be increased from 11.88 kOe to 13.91 kOe without decreasing their remanence.« less

Copper indium gallium selenide (CIGS) photovoltaic devices made using multistep selenization of nanocrystal films.

PubMed

Harvey, Taylor B; Mori, Isao; Stolle, C Jackson; Bogart, Timothy D; Ostrowski, David P; Glaz, Micah S; Du, Jiang; Pernik, Douglas R; Akhavan, Vahid A; Kesrouani, Hady; Vanden Bout, David A; Korgel, Brian A

2013-09-25

The power conversion efficiency of photovoltaic devices made with ink-deposited Cu(InxGa1-x)Se2 (CIGS) nanocrystal layers can be enhanced by sintering the nanocrystals with a high temperature selenization process. This process, however, can be challenging to control. Here, we report that ink deposition followed by annealing under inert gas and then selenization can provide better control over CIGS nanocrystal sintering and yield generally improved device efficiency. Annealing under argon at 525 °C removes organic ligands and diffuses sodium from the underlying soda lime glass into the Mo back contact to improve the rate and quality of nanocrystal sintering during selenization at 500 °C. Shorter selenization time alleviates excessive MoSe2 formation at the Mo back contact that leads to film delamination, which in turn enables multiple cycles of nanocrystal deposition and selenization to create thicker, more uniform absorber films. Devices with power conversion efficiency greater than 7% are fabricated using the multiple step nanocrystal deposition and sintering process.

Co-melting technology in resource recycling of sludge derived from stone processing.

PubMed

Hu, Shao-Hua; Hu, Shen-Chih; Fu, Yen-Pei

2012-12-01

Stone processing sludge (SPS) is a by-product of stone-processing wastewater treatment; it is suitable for use as a raw material for making artificial lightweight aggregates (ALWAs). In this study, boric acid was utilized as a flux to lower sintering temperature. The formation of the viscous glassy phase was observed by DTA curve and changes in XRD patterns. Experiments were conducted to find the optimal combination of sintering temperature, sintering time, and boric acid dosage to produce an ALWA of favorable characteristics in terms of water absorption, bulk density, apparent porosity, compressive strength and weight loss to satisfy Taiwan's regulatory requirements for construction and insulation materials. Optimal results gave a sintering temperature of 850 degrees C for 15 min at a boric acid dosage of 15% by weight of SPS. Results for ALWA favorable characteristics were: 0.21% (water absorption), 0.35% (apparent porosity), 1.67 g/cm3 (bulk density), 66.94 MPa (compressive strength), and less than 0.1% (weight loss).

Co-melting technology in resource recycling of sludge derived from stone processing.

PubMed

Hu, Shao-Hua; Hu, Shen-Chih; Fu, Yen-Pei

2012-12-01

Stone processing sludge (SPS) is a by-product of stone-processing wastewater treatment; it is suitable for use as a raw material for making artificial lightweight aggregates (ALWAs). In this study, boric acid was utilized as a flux to lower sintering temperature. The formation of the viscous glassy phase was observed by DTA curve and changes in XRD patterns. Experiments were conducted to find the optimal combination of sintering temperature, sintering time, and boric acid dosage to produce an ALWA of favorable characteristics in terms of water absorption, bulk density, apparent porosity, compressive strength and weight loss to satisfy Taiwan's regulatory requirements for construction and insulation materials. Optimal results gave a sintering temperature of 850 °C for 15 min at a boric acid dosage of 15 % by weight of SPS. Results for ALWA favorable characteristics were: 0.21 % (water absorption), 0.35 %(apparent porosity), 1.67 g/cm3 (bulk density), 66.94 MPa (compressive strength), and less than 0.1% (weight loss). [Box: see text].

Processing of solid solution, mixed uranium/refractory metal carbides for advanced space nuclear power and propulsion systems

NASA Astrophysics Data System (ADS)

Knight, Travis Warren

Nuclear thermal propulsion (NTP) and space nuclear power are two enabling technologies for the manned exploration of space and the development of research outposts in space and on other planets such as Mars. Advanced carbide nuclear fuels have been proposed for application in space nuclear power and propulsion systems. This study examined the processing technologies and optimal parameters necessary to fabricate samples of single phase, solid solution, mixed uranium/refractory metal carbides. In particular, the pseudo-ternary carbide, UC-ZrC-NbC, system was examined with uranium metal mole fractions of 5% and 10% and corresponding uranium densities of 0.8 to 1.8 gU/cc. Efforts were directed to those methods that could produce simple geometry fuel elements or wafers such as those used to fabricate a Square Lattice Honeycomb (SLHC) fuel element and reactor core. Methods of cold uniaxial pressing, sintering by induction heating, and hot pressing by self-resistance heating were investigated. Solid solution, high density (low porosity) samples greater than 95% TD were processed by cold pressing at 150 MPa and sintering above 2600 K for times longer than 90 min. Some impurity oxide phases were noted in some samples attributed to residual gases in the furnace during processing. Also, some samples noted secondary phases of carbon and UC2 due to some hyperstoichiometric powder mixtures having carbon-to-metal ratios greater than one. In all, 33 mixed carbide samples were processed and analyzed with half bearing uranium as ternary carbides of UC-ZrC-NbC. Scanning electron microscopy, x-ray diffraction, and density measurements were used to characterize samples. Samples were processed from powders of the refractory mono-carbides and UC/UC 2 or from powders of uranium hydride (UH3), graphite, and refractory metal carbides to produce hypostoichiometric mixed carbides. Samples processed from the constituent carbide powders and sintered at temperatures above the melting point of UC showed signs of liquid phase sintering and were shown to be largely solid solutions. Pre-compaction of mixed carbide powders prior to sintering was shown to be necessary to achieve high densities. Hypostoichiometric, samples processed at 2500 K exhibited only the initial stage of sintering and solid solution formation. Based on these findings, a suggested processing methodology is proposed for producing high density, solid solution, mixed carbide fuels. Pseudo-binary, refractory carbide samples hot pressed at 3100 K and 6 MPa showed comparable densities (approximately 85% of the theoretical value) to samples processed by cold pressing and sintering at temperatures of 2800 K.

Processing of U-2.5Zr-7.5Nb and U-3Zr-9Nb alloys by sintering process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dos Santos, A. M. M.; Ferraz, W. B.; Lameiras, F. S.

2012-07-01

To minimize the risk of nuclear proliferation, there is worldwide interest in reducing fuel enrichment of research and test reactors. To achieve this objective while still guaranteeing criticality and cycle length requirements, there is need of developing high density uranium metallic fuels. Alloying elements such as Zr, Nb and Mo are added to uranium to improve fuel performance in reactors. In this context, the Centro de Desenvolvimento da Tecnologia Nuclear (CDTN) is developing the U-2.5Zr-7.5Nb and U-3Zr-9Nb (weight %) alloys by the innovative process of sintering that utilizes raw materials in the form of powders. The powders were pressed atmore » 400 MPa and then sintered under a vacuum of about 1x10{sup -4} Torr at temperatures ranging from 1050 deg. to 1500 deg.C. The densities of the alloys were measured geometrically and by hydrostatic method and the phases identified by X ray diffraction (XRD). The microstructures of the pellets were observed by scanning electron microscopy (SEM) and the alloying elements were analyzed by energy dispersive X-ray spectroscopy (EDS). The results obtained showed the fuel density to slightly increase with the sintering temperature. The highest density achieved was approximately 80% of theoretical density. It was observed in the pellets a superficial oxide layer formed during the sintering process. (authors)« less

Transformation of sintered CsPbBr 3 nanocrystals to cubic CsPbI 3 and gradient CsPbBr xI 3–x through halide exchange

DOE PAGES

Hoffman, Jacob B.; Schleper, A. Lennart; Kamat, Prashant V.

2016-06-20

All-inorganic cesium lead halide (CsPbX 3, X = Br –, I –) perovskites could potentially provide comparable photovoltaic performance with enhanced stability compared to organic–inorganic lead halide species. However, small-bandgap cubic CsPbI3 has been difficult to study due to challenges forming CsPbI 3 in the cubic phase. Here, a low-temperature procedure to form cubic CsPbI 3 has been developed through a halide exchange reaction using films of sintered CsPbBr 3 nanocrystals. The reaction was found to be strongly dependent upon temperature, featuring an Arrhenius relationship. Additionally, film thickness played a significant role in determining internal film structure at intermediate reactionmore » times. Thin films (50 nm) showed only a small distribution of CsPbBr xI 3–x species, while thicker films (350 nm) exhibited much broader distributions. Furthermore, internal film structure was ordered, featuring a compositional gradient within film. Transient absorption spectroscopy showed the influence of halide exchange on the excited state of the material. In thicker films, charge carriers were rapidly transferred to iodide-rich regions near the film surface within the first several picoseconds after excitation. Furthermore, this ultrafast vectorial charge-transfer process illustrates the potential of utilizing compositional gradients to direct charge flow in perovskite-based photovoltaics.« less

Recent developments in melt processed Gd-123 and MgB2 materials at RTRI

NASA Astrophysics Data System (ADS)

Muralidhar, M.; Fukumoto, Y.; Ishihara, A.; Suzuki, K.; Tomita, M.; Koblischka, M. R.; Yamamoto, A.; Kishio, K.

2014-01-01

In this contribution we will report on the current status, recent developments in GdBa2Cu3Oy "Gd-123" and MgB2 material processing, characterization, and applications at the Railway Technical Research Institute (RTRI). Batch-processing of Gd-123 bulk material grown in air was performed using novel thin film Nd-123 seeds grown on MgO crystals. In this way, we are able to fabricate materials with good quality, and uniform performance. We examined the technology of the uniform performance of the large 45 mm diameter, single grain Gd-123 bulks for use in application of NMR. For this purpose, four 5 mm thick pieces are cut vertically from a single grain Gd-123 material and the magnetic field distribution is measured using a scanning hall sensor. We found that all four pieces are single domain and exhibit a quite uniform field distribution. Furthermore, the batch-processed bulk materials are used for the construction of a chilled Maglev vehicle. On the other hand, to optimize the trapped field performance of bulk MgB2 material, several samples were prepared by solid state reaction at different temperatures ranging from 750 to 950 °C in pure argon atmosphere. X-ray diffraction results indicated that single phase and homogenous MgB2 bulks are produced when sintering them around 775 °C. Further, atomic force microscopy (AFM) and scanning electron microscopy (SEM) indicated that an uniform grain size results by controlling the processing temperature. So, higher trapped fields can be achieved in sintered MgB2 material.

Direct laser sintered WC-10Co/Cu nanocomposites

NASA Astrophysics Data System (ADS)

Gu, Dongdong; Shen, Yifu

2008-04-01

In the present work, the direct metal laser sintering (DMLS) process was used to prepare the WC-Co/Cu nanocomposites in bulk form. The WC reinforcing nanoparticles were added in the form of WC-10 wt.% Co composite powder. The microstructural features and mechanical properties of the laser-sintered sample were characterized by X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscope (SEM), energy dispersive X-ray spectroscope (EDX), and nanoindentation tester. It showed that the original nanometric nature of the WC reinforcing particulates was well retained without appreciable grain growth after laser processing. A homogeneous distribution of the WC reinforcing nanoparticles with a coherent particulate/matrix interfacial bonding was obtained in the laser-sintered structure. The 94.3% dense nanocomposites have a dynamic nanohardness of 3.47 GPa and a reduced elastic modulus of 613.42 GPa.

Powder metallurgy preparation of Mg-Ca alloy for biodegradable implant application

NASA Astrophysics Data System (ADS)

Annur, D.; Suhardi, A.; Amal, M. I.; Anwar, M. S.; Kartika, I.

2017-04-01

Magnesium and its alloys is a promising candidate for implant application especially due to its biodegradability. In this study, Mg-7Ca alloys (in weight %) were processed by powder metallurgy from pure magnesium powder and calcium granule. Milling process was done in a shaker mill using stainless steel balls in various milling time (3, 5, and 8 hours) followed by compaction and sintering process. Different sintering temperatures were used (450°C and 550°C) to examine the effect of sintering temperature on mechanical properties and corrosion resistance. Microstructure evaluation was characterized by X-ray diffraction, scanning electron microscope and energy dispersive X-ray spectroscopy. Mechanical properties and corrosion behavior were examined through hardness testing and electrochemical testing in Hank’s solution (simulation body fluid). In this report, a prolonged milling time reduced particle size and later affected mechanical properties of Mg alloy. Meanwhile, the phase analysis showed that α Mg, Mg2Ca, MgO phases were formed after the sintering process. Further, this study showed that Mg-Ca alloy with different powder metallurgy process would have different corrosion rate although there were no difference of Ca content in the alloy.

Fabrication, strength and oxidation of molybdenum-silicon-boron alloys from reaction synthesis

NASA Astrophysics Data System (ADS)

Middlemas, Michael Robert

Mo-Si-B alloys are a leading candidate for the next generation of jet turbine engine blades and have the potential to raise the operating temperatures by 300-400°C, which would dramatically increase power and efficiency. The alloys of interest are a three-phase mixture of the molybdenum solid solution (Moss) and two intermetallic phases, Mo3Si (A15) and Mo5SiB2 (T2). A novel powder metallurgical method was developed which uses the reaction of molybdenum, silicon nitride (Si3N4) and boron nitride (BN) powders to synthesize a fine dispersion of the intermetallic phases in a Moss matrix. The covalent nitrides are stable in oxidizing environments up to 1000ºC, allowing for fine particle processing without the formation of silicon and boron oxides. The process developed uses standard powder processing techniques to create Mo-Si-B alloys in a less complex and expensive manner than previously demonstrated. The formation of the intermetallic phases was examined by thermo-gravimetric analysis and x-ray diffraction. The start of the reactions to form the T2 and A15 phases were observed at 1140°C and 1193°C and the reactions have been demonstrated to be complete in as little as two hours at 1300°C. This powder metallurgy approach yields a fine dispersion of intermetallics in the Moss matrix, with average grain sizes of 2-4mum. Densities up to 95% of theoretical were attained from pressureless sintering at 1600°C and full theoretical density was achieved by hot-isostatic pressing (HIP). Low temperature sintering and HIPing was attempted to limit grain growth and to reduce the equilibrium silicon concentration in the Moss matrix. Sintering and HIPing at 1300°C reduced the grain sizes of all three phases by over a factor of two. Powder metallurgy provides an opportunity for microstructure control through changes in raw materials and processing parameters. Microstructure examination by electron back-scatter diffraction (EBSD) imaging was used to precisely define the location of all three phases and to measure the volume fractions and grain size distributions. Microstructural quantification techniques including two-point correlation functions were used to quantify microstructural features and correlate the BN powder size and morphology to the distribution of the intermetallic phases. High-temperature tensile tests were conducted and yield strengths of 580MPa at 1100°C and 480MPa at 1200°C were measured for the Mo-2Si-1B wt.% alloy. The yield strength of the Mo-3Si-1B wt.% alloy was 680MPa at 1100°C and 420MPa at 1300°C. A review of the pertinent literature reveals that these are among the highest yield strengths measured for these compositions. The oxidation resistance in air at 1000 and 1100°C was found to be comparable to the best values reported in the literature. The protective borosilicate surface layer was formed quickly due to the close spacing of intermetallic particles and pre-oxidation treatment was developed to further limit the transient oxidation behavior. An oxidation model was developed which factors in the different stages of oxidation to predict compositions which minimize the total metal recession due to oxidation.

Continuum simulation of heat transfer and solidification behavior of AlSi10Mg in Direct Metal Laser Sintering Process

NASA Astrophysics Data System (ADS)

Ojha, Akash; Samantaray, Mihir; Nath Thatoi, Dhirendra; Sahoo, Seshadev

2018-03-01

Direct Metal Laser Sintering (DMLS) process is a laser based additive manufacturing process, which built complex structures from powder materials. Using high intensity laser beam, the process melts and fuse the powder particles makes dense structures. In this process, the laser beam in terms of heat flux strikes the powder bed and instantaneously melts and joins the powder particles. The partial solidification and temperature distribution on the powder bed endows a high cooling rate and rapid solidification which affects the microstructure of the build part. During the interaction of the laser beam with the powder bed, multiple modes of heat transfer takes place in this process, that make the process very complex. In the present research, a comprehensive heat transfer and solidification model of AlSi10Mg in direct metal laser sintering process has been developed on ANSYS 17.1.0 platform. The model helps to understand the flow phenomena, temperature distribution and densification mechanism on the powder bed. The numerical model takes into account the flow, heat transfer and solidification phenomena. Simulations were carried out for sintering of AlSi10Mg powders in the powder bed having dimension 3 mm × 1 mm × 0.08 mm. The solidification phenomena are incorporated by using enthalpy-porosity approach. The simulation results give the fundamental understanding of the densification of powder particles in DMLS process.

Study on selective laser sintering of glass fiber reinforced polystyrene

NASA Astrophysics Data System (ADS)

Yang, Laixia; Wang, Bo; Zhou, Wenming

2017-12-01

In order to improve the bending strength of Polystyrene (PS) sintered parts by selective laser sintering, Polystyrene/glass fiber (PS/GF) composite powders were prepared by mechanical mixing method. The size distribution of PS/GF composite powders was characterized by laser particle size analyzer. The optimum ratio of GF was determined by proportioning sintering experiments. The influence of process parameters on the bending strength of PS and PS/GF sintered parts was studied by orthogonal test. The result indicates that the particle size of PS/GF composite powder is mainly distributed in 24.88 μm~139.8 μm. When the content of GF is 10%, it has better strengthen effect. Finally, the article used the optimum parameter of the two materials to sinter prototype, it is found that the PS/GF prototype has the advantages of good accuracy and high strength.

Reduction behavior and kinetics of vanadium-titanium sinters under high potential oxygen enriched pulverized coal injection

NASA Astrophysics Data System (ADS)

Ma, Jin-fang; Wang, Guang-wei; Zhang, Jian-liang; Li, Xin-yu; Liu, Zheng-jian; Jiao, Ke-xin; Guo, Jian

2017-05-01

In this work, the reduction behavior of vanadium-titanium sinters was studied under five different sets of conditions of pulverized coal injection with oxygen enrichment. The modified random pore model was established to analyze the reduction kinetics. The results show that the reduction rate of sinters was accelerated by an increase of CO and H2 contents. Meanwhile, with the increase in CO and H2 contents, the increasing range of the medium reduction index (MRE) of sinters decreased. The increasing oxygen enrichment ratio played a diminishing role in improving the reduction behavior of the sinters. The reducing process kinetic parameters were solved using the modified random role model. The results indicated that, with increasing oxygen enrichment, the contents of CO and H2 in the reducing gas increased. The reduction activation energy of the sinters decreased to between 20.4 and 23.2 kJ/mol.

In vitro biodegradation testing of Mg-alloy EZK400 and manufacturing of implant prototypes using PM (powder metallurgy) methods.

PubMed

Wolff, M; Luczak, M; Schaper, J G; Wiese, B; Dahms, M; Ebel, T; Willumeit-Römer, R; Klassen, T

2018-09-01

The study is focussing towards Metal Injection Moulding (MIM) of Mg-alloys for biomedical implant applications. Especially the influence of the sintering processing necessary for the consolidation of the finished part is in focus of this study. In doing so, the chosen high strength EZK400 Mg-alloy powder material was sintered using different sintering support bottom plate materials to evaluate the possibility of iron impurity pick up during sintering. It can be shown that iron pick up took place from the steel bottom plate into the specimen. Despite the fact that a separating boron nitrite (BN) barrier layer was used and the Mg-Fe phase diagram is not predicting any significant solubility to each other. As a result of this study a new bottom plate material not harming the sintering and the biodegradation performance of the as sintered material, namely a carbon plate material, was found.

Evaluation of Microstructure and Mechanical Properties of Al-TiC Metal Matrix Composite Prepared by Conventional, Microwave and Spark Plasma Sintering Methods

PubMed Central

Ghasali, Ehsan; Fazili, Ali; Alizadeh, Masoud; Shirvanimoghaddam, Kamyar; Ebadzadeh, Touradj

2017-01-01

In this research, the mechanical properties and microstructure of Al-15 wt % TiC composite samples prepared by spark plasma, microwave, and conventional sintering were investigated. The sintering process was performed by the speak plasma sintering (SPS) technique, microwave and conventional furnaces at 400 °C, 600 °C, and 700 °C, respectively. The results showed that sintered samples by SPS have the highest relative density (99% of theoretical density), bending strength (291 ± 12 MPa), and hardness (253 ± 23 HV). The X-ray diffraction (XRD) investigations showed the formation of TiO2 from the surface layer decomposition of TiC particles. Scanning electron microscopy (SEM) micrographs demonstrated uniform distribution of reinforcement particles in all sintered samples. The SEM/EDS analysis revealed the formation of TiO2 around the porous TiC particles. PMID:29088114

Development of high strength, high temperature ceramics

NASA Technical Reports Server (NTRS)

Hall, W. B.

1982-01-01

Improvement in the high-pressure turbopumps, both fuel and oxidizer, in the Space Shuttle main engine were considered. The operation of these pumps is limited by temperature restrictions of the metallic components used in these pumps. Ceramic materials that retain strength at high temperatures and appear to be promising candidates for use as turbine blades and impellers are discussed. These high strength materials are sensitive to many related processing parameters such as impurities, sintering aids, reaction aids, particle size, processing temperature, and post thermal treatment. The specific objectives of the study were to: (1) identify and define the processing parameters that affect the properties of Si3N4 ceramic materials, (2) design and assembly equipment required for processing high strength ceramics, (3) design and assemble test apparatus for evaluating the high temperature properties of Si3N4, and (4) conduct a research program of manufacturing and evaluating Si3N4 materials as applicable to rocket engine applications.

Improved silicon carbide for advanced heat engines. II - Pressureless sintering and mechanical properties of injection molded silicon carbide

NASA Technical Reports Server (NTRS)

Whalen, Thomas J.; Baer, J. R.

1989-01-01

The influence on density and strength of pressureless sintering in vacuum and argon environments has been evaluated with injection molded SiC materials. Main effects and two factor interactions of sintering (cycle variables temperature, time, heating rate, and atmosphere) were assessed. An improved understanding of the influence of the processing flaws and sintering conditions has been obtained. Strength and density have improved from a baseline level of 299 MPa (43.3 Ksi) and 94 pct of theoretical density to values greater than 483 MPa (70 Ksi) and 97 pct.

Novel Routes for Sintering of Ultra-high Temperature Ceramics and their Properties

DTIC Science & Technology

2014-10-31

UHTCs charge (zirconium and hafnium borides , SiC) with additives (chromium carbide, nickel, chromium, etc.), which activate sintering process, is...temperature phases in a form of carboborides of zirconium and bi borides of zirconium or chromium. Elevation of densification rate of sintered borides is...superplasticity under the slip mechanism of zirconium boride and silica carbide grains on grain boundary interlayers with nanocrystalline grains of carbon

Synthesis of submicron CaZrO{sub 3} in combustion reactions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khaliullin, Sh. M., E-mail: khaliullin@ihim.uran.ru; Zhuravlev, V. D.; Bamburov, V. G.

Submicron CaZrO{sub 3} powder is obtained in combustion reactions (solution combustion synthesis—SCS) with glycine. It is found that SCS reduces the sintering temperature of CaZrO{sub 3} powders. The dielectric properties of calcium zirconate ceramics are studied by the electrochemical impedance method. It is shown that a ceramics of powders obtained by the SCS method has high dielectric characteristics.

Sinterable Powders from Laser Driven Reactions

DTIC Science & Technology

1982-03-01

using several shaping techniques. The Si powders were densified to precisely controlled levels designed to yield high density reaction bonded silicon...nitride (RBSN). -Nitriding kinetics were rapid at low temperatures because of the small particle sizes. Characteristic dimensions of RBSN micro ...b. Dispersion Test 90 c. Contact Angle Measurements 94 vi TABLE OF C014E1TS (cont.) PAGE 2. Results of Dispersion Test 94 a. Screening Tests 94 b

Microstructural evolution during sintering of copper particles studied by laboratory diffraction contrast tomography (LabDCT).

PubMed

McDonald, S A; Holzner, C; Lauridsen, E M; Reischig, P; Merkle, A P; Withers, P J

2017-07-12

Pressureless sintering of loose or compacted granular bodies at elevated temperature occurs by a combination of particle rearrangement, rotation, local deformation and diffusion, and grain growth. Understanding of how each of these processes contributes to the densification of a powder body is still immature. Here we report a fundamental study coupling the crystallographic imaging capability of laboratory diffraction contrast tomography (LabDCT) with conventional computed tomography (CT) in a time-lapse study. We are able to follow and differentiate these processes non-destructively and in three-dimensions during the sintering of a simple copper powder sample at 1050 °C. LabDCT quantifies particle rotation (to <0.05° accuracy) and grain growth while absorption CT simultaneously records the diffusion and deformation-related morphological changes of the sintering particles. We find that the rate of particle rotation is lowest for the more highly coordinated particles and decreases during sintering. Consequently, rotations are greater for surface breaking particles than for more highly coordinated interior ones. Both rolling (cooperative) and sliding particle rotations are observed. By tracking individual grains the grain growth/shrinkage kinetics during sintering are quantified grain by grain for the first time. Rapid, abnormal grain growth is observed for one grain while others either grow or are consumed more gradually.

Formability and mechanical properties of porous titanium produced by a moldless process.

PubMed

Naito, Yoshihito; Bae, Jiyoung; Tomotake, Yoritoki; Hamada, Kenichi; Asaoka, Kenzo; Ichikawa, Tetsuo

2013-08-01

Tailor-made porous titanium implants show great promise in both orthopedic and dental applications. However, traditional powder metallurgical processes require a high-cost mold, making them economically unviable for producing unique devices. In this study, a mixture of titanium powder and an inlay wax binder was developed for moldless forming and sintering. The formability of the mixture, the dimensional changes after sintering, and the physical and mechanical properties of the sintered porous titanium were evaluated. A 90:10 wt % mixture of Ti powder and wax binder was created manually at 70°C. After debindering, the specimen was sintered in Ar at 1100°C without any mold for 1, 5, and 10 h. The shrinkage, porosity, absorption ratio, bending and compressive strength, and elastic modulus were measured. The bending strength (135-356 MPa), compression strength (178-1226 MPa), and elastic modulus (24-54 GPa) increased with sintering time; the shrinkage also increased, whereas the porosity (from 37.1 to 29.7%) and absorption ratio decreased. The high formability of the binder/metal powder mixture presents a clear advantage for fabricating tailor-made bone and hard tissue substitution units. Moreover, the sintered compacts showed high strength and an elastic modulus comparable to that of cortical bone. Copyright © 2013 Wiley Periodicals, Inc.

Preparation of micro-porous bioceramic containing silicon-substituted hydroxyapatite and beta-tricalcium phosphate.

PubMed

Fuh, Lih-Jyh; Huang, Ya-Jing; Chen, Wen-Cheng; Lin, Dan-Jae

2017-06-01

Dimensional instability caused by sintering shrinkage is an inevitable drawback for conventional processing of hydroxyapatite (HA). A new preparation method for biphasic calcium phosphates was developed to increase micro pores and biodegradation without significant dimensional change. Powder pressed HA discs, under 100MPa, were immersed in a colloidal mixture of tetraethoxysilane (TEOS) and ammonium hydroxide for 10min, followed by drying, and then were sintered at 900°C, 1050°C, and 1200°C, respectively. Comparing with pure HA discs, the newly prepared product sintered up to 1200°C contained silicon substituted HA, beta-tricalcium phosphate, and calcium silicate with better micro-porosity, high specific surface area, less sintering shrinkage and the strength maintained. The cytocompatibility test demonstrated a better viability for D1 mice stem cells cultured on TEOS treated HA for 14days compared to the pure HA. This simple TEOS sol-gel pretreatment has the potential to be applied to any existing manufacturing process of HA scaffold for better control of sintering shrinkage, create micropores, and increase biodegradation. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of NASA's Sample Cartridge Assembly: Summary of GEDS Design, Development Testing, and Thermal Analyses

NASA Technical Reports Server (NTRS)

O'Connor, Brian; Hernandez, Deborah; Hornsby, Linda; Brown, Maria; Horton-Mullins, Kathryn

2017-01-01

Outline: Background of ISS (International Space Station) Material Science Research Rack; NASA SCA (Sample Cartridge Assembly) Design; GEDS (Gravitational Effects in Distortion in Sintering) Experiment Ampoule Design; Development Testing Summary; Thermal Modeling and Analysis. Summary: GEDS design development challenging (GEDS Ampoule design developed through MUGS (Microgravity) testing; Short duration transient sample processing; Unable to measure sample temperatures); MUGS Development testing used to gather data (Actual LGF (Low Gradient Furnace)-like furnace response; Provided sample for sintering evaluation); Transient thermal model integral to successful GEDS experiment (Development testing provided furnace response; PI (Performance Indicator) evaluation of sintering anchored model evaluation of processing durations; Thermal transient model used to determine flight SCA sample processing profiles).

Pressure-assisted low-temperature sintering for paper-based writing electronics.

PubMed

Xu, L Y; Yang, G Y; Jing, H Y; Wei, J; Han, Y D

2013-09-06

With the aim of preparing paper-based writing electronics, a kind of conductive pen was made with nano-silver ink as the conductive component and a rollerball pen as the writing implement. This was used to direct-write conductive patterns on Epson photo paper. In order to decrease the sintering temperature, pressure was introduced to enhance the driving forces for sintering. Compared with hot sintering without pressure, hot-pressure can effectively improve the conductivity of silver coatings, reduce the sintering time and thus improve productivity. Importantly, pressure can achieve a more uniform and denser microstructure, which increases the connection strength of the silver coating. At the optimum hot-pressure condition (sintering temperature 120 ° C/sintering pressure 25 MPa/sintering time 15 min), a typical measured resistivity value was 1.43 × 10⁻⁷ Ω m, nine greater than that of bulk silver. This heat treatment process is compatible with paper and does not cause any damage to the paper substrates. Even after several thousand bending cycles, the resistivity values of writing tracks by hot-pressure sintering stay almost the same (from 1.43 × 10⁻⁷ to 1.57 × 10⁻⁷ Ω m). The stability and flexibility of the writing circuits are good, which demonstrates the promising future of writing electronics.

Cryomilled and spark plasma sintered titanium: the evolution of microstructure

NASA Astrophysics Data System (ADS)

Kozlík, Jiří; Becker, Hanka; Harcuba, Petr; Stráský, Josef; Janeček, Milos

2017-05-01

Bulk ultra-fine grained (UFG) commercially pure Ti was prepared by cryogenic milling in liquid argon and subsequent spark plasma sintering (SPS). During cryogenic milling, individual powder particles are repetitively severely deformed by attrition forces. Powder particles were not significantly refined, but due to severe repetitive plastic deformation, ultra-fine grained microstructure emerges within each powder particle. Cryogenic milling can be therefore considered as a specific severe plastic deformation (SPD) method. Compactization of cryomilled powder by SPS technique (also referred to as field assisted sintering technique - FAST) requires significantly lower sintering temperatures and shorter sintering times for successful compaction when compared to any other sintering technique. This is crucial for maintaining the UFG microstructure due to its limited thermal stability. Several specimens were prepared by varying processing parameters, in particular the sintering temperature. The microstructure of powders and compacted samples was observed by scanning electron microscopy (SEM). Increased sintering temperature results in recrystallization and grain growth. A trade-off relationship between the density of compacted material and grain size was identified. Microhardness of the material was found to depend on residual porosity rather than grain size. This contribution presents cryogenic milling and spark plasma sintering as a viable alternative for achieving UFG microstructure in commercially pure Ti.

Development of a Cr-Based Hard Composite Processed by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

García-Junceda, A.; Sáez, I.; Deng, X. X.; Torralba, J. M.

2018-04-01

This investigation analyzes the feasibility of processing a composite material comprising WC particles randomly dispersed in a matrix in which Cr is the main metallic binder. Thus, a new composite material is processed using a commercial, economic, and easily available Cr-based alloy, assuming that there is a certain Cr solubility in the WC particles acting as reinforcement. The processing route followed includes mechanical milling of the powders and consolidation by spark plasma sintering.

Effects of chemical states of carbon on deuterium retention in carbon-containing materials

NASA Astrophysics Data System (ADS)

Oyaidzu, Makoto; Kimura, Hiromi; Nakahata, Toshihiko; Nishikawa, Yusuke; Tokitani, Masayuki; Oya, Yasuhisa; Iwakiri, Hirotomo; Yoshida, Naoaki; Okuno, Kenji

2007-08-01

Deuterium retention behavior in highly oriented pyrolytic graphite (HOPG), poly-crystalline diamond, poly-crystalline SiC, sintered WC, and converted B 4C were investigated to reveal tritium behavior in re-deposition and co-deposition layers. Such layers would contain carbon, when the first wall and/or divertor were made of graphite or carbon-containing materials. Furthermore, the employment of other materials such as tungsten, and first wall conditioning such as boronization would complicate the layers. No different deuterium trapping sites due to carbon from those in HOPG were found in all the samples, where two deuterium trapping processes were observed: hot atom chemical trapping of energetic deuterium by a dangling bond of carbon and thermochemical trapping of thermalized deuterium in a constituent atom vacancy surrounded by carbons. Additionally, the latter reaction could be easily counteracted by or competed with the other deuterium trapping reactions by constituent atoms.

The effect of B{sub 2}O{sub 3} flux on growth NLBCO superconductor by solid state reaction and wet-mixing methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Suharta, W. G., E-mail: wgsuharta@gmail.com; Wendri, N.; Ratini, N.

The synthesis of B{sub 2}O{sub 3} flux substituted NLBCO superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} has been done using solid state reaction and wet-mixing methods in order to obtain homogeneous crystals and single phase. From DTA/TGA characteritations showed the synthesis process by wet-mixing requires a lower temperature than the solid state reaction in growing the superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂}. Therefore, in this research NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} sample calcinated at 650°C for wet-mixing method and 820°C for solid state reaction methods. The all samples was sintered at 950°C for ten hours. Crystallinity of the sample was confirmedmore » using X-ray techniques and generally obtained sharp peaks that indicates the sample already well crystallized. Search match analyses for diffraction data gave weight fractions of impurity phase of the solid state reaction method higher than wet-mixing method. In this research showed decreasing the price of the lattice parameter about 1% with the addition of B{sub 2}O{sub 3} flux for the both synthesis process and 2% of wet mixing process for all samples. Characterization using scanning electron microscopy (SEM) showed the distribution of crystal zise for wet-mixing method more homogeneous than solid state reaction method, with he grain size of samples is around 150–250 nm. The results of vibrating sample magnetometer (VSM) showed the paramagnetic properties for all samples.« less

The development and characterization of a novel aluminum-copper-magnesium P/M alloy

NASA Astrophysics Data System (ADS)

Boland, Christopher Daniel

Powder metallurgy (P/M) is a metal fabrication process that is characterized by high yield and ability to be automated, as well as the resultant part complexity and reproducibility. This press and sinter process is favoured by the automotive industry. Aluminum alloy P/M parts are particularly attractive because they have a high strength to weight ratio and they can be made to have high corrosion and wear resistance. There are few commercial Al P/M alloys currently in use and they occupy a small portion of the market. To expand the use of aluminum in the industry a new alloy was created, modeled after the wrought AC2024 family of alloys. P/M 2324, with a nominal composition of Al-4.4Cu-1.5Mg, was assessed using physical, chemical and mechanical methods to help maximize alloy properties through processing. The objective of this work was to develop a viable industrial alloy. The investigation of 2324 included the evaluation of starting powders, starting composition, processing methods, secondary treatments, and industrial response. All blending and compacting was completed at Dalhousie University, while sintering was undertaken at Dalhousie and GKN Sinter Metals. The green alloy was assessed for best compaction pressure using green density and strength. The sintered alloy was assessed to determine the best press and sinter variables, using dimensional change, sintered density, apparent hardness, tensile properties and microscopy. These same sintered properties were tested to determine if sintering done on a laboratory scale could be replicated industrially. The viability of heat treatment was tested using differential scanning calorimetry, hardness and tensile properties. The alloy was also subject to modifications of Cu and Mg amounts, as well as to the addition of tin to the base composition. It was determined that compaction at 400MPa and sintering at 600°C for 20min produced the best properties for the sintered bodies. The resultant mechanical properties were attributed to a high sintered density (2.68g/cm 3 or 97% of theoretical) and strengthening mechanisms present in the Al-Cu-Mg system. These mechanisms included possible secondary phases formed in the alloy seen using microscopy and differential scanning calorimetry analyses. A T6 heat treatment of solutionizing at 495°C for 1.5h, water quench and aging for 10h was found to improve the properties of 2324. Modifications to Cu and Mg alloying additions produced few gains. However, the presence of 0.2Sn (w/o) was found to enhance the alloy. Resultant properties of the optimal alloy included an apparent hardness of 76.6HRE and an ultimate tensile strength of 367MPa. Also studied was the discrepancy observed in sintering at GKN and Dalhousie and the mechanisms at work with the addition of Sn. 2324 was adapted successfully to P/M applications. It was capable of performing against an established Al P/M industry standard, and with further testing its uses can undoubtedly be expanded.

Improved magnetic properties and growth anisotropy of chemically modified Sr ferrites

NASA Astrophysics Data System (ADS)

Lee, Jung W.; Cho, Yong S.; Amarakoon, Vasantha R. W.

1999-04-01

Magnetic properties and microstructural characteristics of SrOṡ5.9Fe2O3 chemically modified with Si and Ca were investigated by changing experimental parameters such as additive composition, the ratio of Ca/Si, and sintering condition. A novel particulate coating method utilizing sol-gel reactions was used to uniformly incorporate the additives of Si and Ca. This method was very successful in obtaining homogeneous grain growth and fine grains. A sample containing the gel additives of 0.6 wt % SiO2 and 0.7 wt % CaO and sintered at 1200 °C for 4 h was found to significantly suppress abnormal grain growth, resulting in submicron-sized grains and high density. A distinct grain boundary phase containing Si and Ca was observed by increasing the sintering temperature to 1250 °C. The resultant microstructural characteristics favorably affected magnetic properties. For example, the chemically modified sample exhibited a higher coercivity of 3530 Oe compared to a value of 2050 Oe obtained for the sample without the additives. On the other hand, an increase in the ratio of Ca/Si or in sintering temperature tended to induce a large anisotropy during grain growth.

Preparation and evaluation of silicon nitride matrices for silicon nitride-SiC fiber composites. M.S. Thesis Final Technical Report

NASA Technical Reports Server (NTRS)

Axelson, Scott R.

1988-01-01

Continuous silicon carbide (SiC) fiber was added to three types of silicon nitride (Si3N4) matrices. Efforts were aimed at producing a dense Si3N4 matrix from reaction-bonded silicon nitride (RBSN) by hot-isostatic-pressing (HIP) and pressureless sintering, and from Si3N4 powder by hot-pressing. The sintering additives utilized were chosen to allow for densification, while not causing severe degradation of the fiber. The ceramic microstructures were evaluated using scanning optical microscopy. Vickers indentation was used to determine the microhardness and fracture toughness values of the matrices. The RBSN matrices in this study did not reach more than 80 percent of theoretical density after sintering at various temperatures, pressures, and additive levels. Hot-pressing Si3N4 powder produced the highest density matrices; hardness and toughness values were within an order of magnitude of the best literature values. The best sintering aid composition chosen included Y2O3, SiO2, and Al2O3 or AlN. Photomicrographs demonstrate a significant reduction of fiber attack by this additive composition.

Stable solidification of silica-based ammonium molybdophosphate by allophane: Application to treatment of radioactive cesium in secondary solid wastes generated from fukushima.

PubMed

Wu, Yan; Lee, Chuan-Pin; Mimura, Hitoshi; Zhang, Xiaoxia; Wei, Yuezhou

2018-01-05

Silica-based ammonium molybdophosphate (AMP/SiO 2 ) is an absorbent material that can effectively remove Cs from radioactive-contaminated wastewater (RCW) generated by Fukushima nuclide accident. Pressing/sintering method was used for final disposal of secondary waste (spent absorbent) to achieve the volume reduction of AMP-Cs/SiO 2 (AMP/SiO 2 saturation adsorption of Cs) and stable solidification of Cs by adding natural allophane. The structure of AMP-Cs completely collapsed at approximately 700°C, and most Mo and P species in AMP sublimed. The optimal sintering temperature was estimated as 900°C. The stable crystalline phase of Cs 4 Al 4 Si 20 O 48 was recrystallized by the reaction of Cs 2 O, Al 2 O 3 , and SiO 2 , and the immobilization ratio of Cs was approximately 100%. The leachability of Cs from the sintered product in distilled water was approximately 0.41%. The high immobilization and low leachability of Cs were attributed to the excellent solidification properties of the sintered products of AMP-Cs/SiO 2 -allophane. Copyright © 2017 Elsevier B.V. All rights reserved.

Particle morphology influence on mechanical and biocompatibility properties of injection molded Ti alloy powder.

PubMed

Gülsoy, H Özkan; Gülsoy, Nagihan; Calışıcı, Rahmi

2014-01-01

Titanium and Titanium alloys exhibits properties that are excellent for various bio-applications. Metal injection molding is a processing route that offers reduction in costs, with the added advantage of near net-shape components. Different physical properties of Titanium alloy powders, shaped and processed via injection molding can achieve high complexity of part geometry with mechanical and bioactivity properties, similar or superior to wrought material. This study describes that the effect of particle morphology on the microstructural, mechanical and biocompatibility properties of injection molded Ti-6Al-4V (Ti64) alloy powder for biomaterials applications. Ti64 powders irregular and spherical in shape were injection molded with wax based binder. Binder debinding was performed in solvent and thermal method. After debinding the samples were sintered under high vacuum. Metallographic studies were determined to densification and the corresponding microstructural changes. Sintered samples were immersed in a simulated body fluid (SBF) with elemental concentrations that were comparable to those of human blood plasma for a total period of 15 days. Both materials were implanted in fibroblast culture for biocompatibility evaluations were carried out. The results show that spherical and irregular powder could be sintered to a maximum theoretical density. Maximum tensile strength was obtained for spherical shape powder sintered. The tensile strength of the irregular shape powder sintered at the same temperature was lower due to higher porosity. Finally, mechanical tests show that the irregular shape powder has lower mechanical properties than spherical shape powder. The sintered irregular Ti64 powder exhibited better biocompatibility than sintered spherical Ti64 powder. Results of study showed that sintered spherical and irregular Ti64 powders exhibited high mechanical properties and good biocompatibility properties.

Thermoelectric properties of a doped LaNiO3 perovskite system prepared using a spark-plasma sintering process

NASA Astrophysics Data System (ADS)

Tak, Jang-Yeul; Choi, Soon-Mok; Seo, Won-Seon; Cho, Hyung Koun

2013-07-01

Both perovskites LaNiO3 and LaCuO3 have a limitation associated with phase transitions for high-temperature thermoelectric applications. The optimized conditions were investigated to obtain the LaNi1- x Cu x O3- δ perovskite single phase showing a Cu-doping effect into Ni sites against unintended deoxidized phases. Three advantages of synergetic effects due to the simultaneous presence of nickel and copper were investigated: a low melting temperature of CuO as compared to that of NiO, the absence of intermediated deoxidized phases in the LaCuO3 system, and the Cu doping effect, which suppresses the formation of intermediate secondary phases. A solid solution was also fabricated using a spark-plasma sintering (SPS) process for the purpose of sintering LaNi1- x Cu x O3- δ compositions at a low sintering temperature.

Computer simulation of low-temperature composites sintering processes for additive technologies

NASA Astrophysics Data System (ADS)

Tovpinets, A. O.; Leytsin, V. N.; Dmitrieva, M. A.

2017-12-01

This is impact research of mixture raw components characteristics on the low-temperature composites structure formation during the sintering process. The obtained results showed that the structure determination of initial compacts obtained after thermal destruction of the polymer binder lets quantify the concentrations of main components and the refractory crystalline product of thermal destruction. Accounting for the distribution of thermal destruction refractory product allows us to refine the forecast of thermal stresses in the matrix of sintered composite. The presented results can be considered as a basis for optimization of initial compositions of multilayer low-temperature composites obtained by additive technologies.

Sinterless Fabrication Of Contact Pads On InP Devices

NASA Technical Reports Server (NTRS)

Weizer, Victor G.; Fatemi, Navid S.; Korenyi-Both, Andras L.

1995-01-01

Research has shown that with proper choice of material, low-resistance contact pads deposited on solar cells and other devices by improved technique that does not involve sintering. Research directed at understanding mechanisms involved in contact-sintering process has resulted in identification of special group of materials that includes phosphides of gold, silver, and nickel; specifically, Au(2)P(3), AgP(2), and Ni(3)P. Incorporation of phosphide interlayer substantially reduces resistivity between gold current-carrying layer and indium phosphide substrate. Further research indicated only very thin interlayer of any of these compounds needed to obtain low contact resistance, without subjecting contact to destructive sintering process.

Improved efficiency of hybrid organic photovoltaics by pulsed laser sintering of silver nanowire network transparent electrode.

PubMed

Spechler, Joshua A; Nagamatsu, Ken A; Sturm, James C; Arnold, Craig B

2015-05-20

In this Research Article, we demonstrate pulsed laser processing of a silver nanowire network transparent conductor on top of an otherwise complete solar cell. The macroscopic pulsed laser irradiation serves to sinter nanowire-nanowire junctions on the nanoscale, leading to a much more conductive electrode. We fabricate hybrid silicon/organic heterojunction photovoltaic devices, which have ITO-free, solution processed, and laser processed transparent electrodes. Furthermore, devices which have high resistive losses show up to a 35% increase in power conversion efficiency after laser processing. We perform this study over a range of laser fluences, and a range of nanowire area coverage to investigate the sintering mechanism of nanowires inside of a device stack. The increase in device performance is modeled using a simple photovoltaic diode approach and compares favorably to the experimental data.

CONTINUOUS PROCESS FOR PREPARING URANIUM HEXAFLUORIDE FROM URANIUM TETRAFLUORIDE AND OXYGEN

DOEpatents

Adams, J.B.; Bresee, J.C.; Ferris, L.M.

1961-11-21

A process for preparing UF/sub 6/ by reacting UF/sub 4/ and oxygen is described. The UF/sub 4/ and oxygen are continuously introduced into a fluidized bed of UO/sub 2/F/sub 2/ at a temperature of 600 to 900 deg C. The concentration of UF/sub 4/ in the bed is maintained below 25 weight per cent in order to avoid sintering and intermediate compound formation. By-product U0/sub 2/F/sub 2/ is continuously removed from the top of the bed recycled. In an alternative embodiment heat is supplied to the reaction bed by burning carbon monoxide in the bed. The product UF/sub 6/ is filtered to remove entrained particles and is recovered in cold traps and chemical traps. (AEC)

Sintering, properties and fabrication of Si3N4 + Y2O3 based ceramics

NASA Technical Reports Server (NTRS)

Quackenbush, C. L.; Smith, J. T.; Neil, J. T.; French, K. W.

1983-01-01

Pure silicon nitride shows a remarkable resistance to sintering without the use of densification additives. The present investigation is concerned with results which show the effect of chemical content on sinterability, taking into account the composition, raw material impurities, and processing contaminants. Aspects of sintering are discussed along with strength characteristics, and oxidation relations. Attention is given to phase field I and II materials, phase field III and IV materials, tungsten carbide and oxidation at 600 C, and studies involving shape fabrication by injection molding. It was found that in sintering Si3N4 + Y2O3 an increase in the amount of Y2O3 and, in particular, the addition of Al2O3 enhances the fluidity of the liquid phase.

Casting of particle-based hollow shapes

DOEpatents

Menchhofer, P.

1997-09-09

A method is disclosed for the production of hollow articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with one aspect of the invention, a thermally settable slurry containing a relatively high concentration of the particles is coated onto a prewarmed continuous surface in a relatively thin layer so that the slurry is substantially uniformly coated on the surface. The heat of the prewarmed surface conducts to the slurry to initiate a reaction which causes the slurry to set or harden in a shape conforming to the surface. The hardened configurations may then be sintered to consolidate the particles and provide a high density product. 9 figs.

Casting of particle-based hollow shapes

DOEpatents

Menchhofer, P.

1995-05-30

A method is disclosed for the production of hollow articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with one aspect of the invention, a thermally settable slurry containing a relatively high concentration of the particles is coated onto a prewarmed continuous surface in a relatively thin layer so that the slurry is substantially uniformly coated on the surface. The heat of the prewarmed surface conducts to the slurry to initiate a reaction which causes the slurry to set or harden in a shape conforming to the surface. The hardened configurations may then be sintered to consolidate the particles and provide a high density product. 9 figs.

Casting of particle-based hollow shapes

DOEpatents

Menchhofer, Paul

1997-01-01

A method for the production of hollow articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with one aspect of the invention, a thermally settable slurry containing a relatively high concentration of the particles is coated onto a prewarmed continuous surface in a relatively thin layer so that the slurry is substantially uniformly coated on the surface. The heat of the prewarmed surface conducts to the slurry to initiate a reaction which causes the slurry to set or harden in a shape conforming to the surface. The hardened configurations may then be sintered to consolidate the particles and provide a high density product.

Casting of particle-based hollow shapes

DOEpatents

Menchhofer, Paul

1995-01-01

A method for the production of hollow articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with one aspect of the invention, a thermally settable slurry containing a relatively high concentration of the particles is coated onto a prewarmed continuous surface in a relatively thin layer so that the slurry is substantially uniformly coated on the surface. The heat of the prewarmed surface conducts to the slurry to initiate a reaction which causes the slurry to set or harden in a shape conforming to the surface. The hardened configurations may then be sintered to consolidate the particles and provide a high density product.

Morphology and phase identification of micron to nanosized manganese oxide (MnO) with variations in sintering time

NASA Astrophysics Data System (ADS)

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

2017-09-01

Manganese oxide (MnO) occurs in many rock types and may take the form of minerals. MnO has its drawbacks, namely highly reactive oxidizing species classified as dangerous and explosive at temperatures above 55 °C. Despite this,MnO has excellent magnetic, electrochemical, and conductivity properties, which should be reduced to nano-size to maximize their use and improve the properties of MnO. Phase and morphology characterization of powder this research aims to reduce the grain size of the MnO from micro to nano using the sol-gel method with various sintering times. Sol-gel is a simple synthesis method that has been proven capable of synthesizing a wide variety of micro-sized oxide materials into nano. Sintering time is a technique performed in the synthesis process to dry the material to a temperature above the normal temperature. The temperature used for sintering starting from 600 °C to 1000 °C. Characterizations were done using XRD, SEM, EDX, and FTIR machines. The sintering processes in this study used a temperature of 600 °C with different sintering periods of 30, 60 and 90 minutes. The XRD characterization with a 30-minute sintering time resulted in the smallest MnO in the form crystalline powder of 47.3 nm. The highest intensity (degree of crystallinity) found in MnO sintered for 90 minutes. The results of the morphological characterization of SEM showed a morphological change in MnO from micro-sized triangular to nano-sized spherical shape. The EDX characterization results indicated that the 30-minute sintering caused the lowest change in Mn and the highest change in O. The results of FTIR characterization showed a shift in C-H and Mn-O followed by an increase in the group of N-H, C=O and Mn-O.

Effect of graphite addition into mill scale waste as a potential bipolar plates material of proton exchange membrane fuel cells

NASA Astrophysics Data System (ADS)

Khaerudini, D. S.; Prakoso, G. B.; Insiyanda, D. R.; Widodo, H.; Destyorini, F.; Indayaningsih, N.

2018-03-01

Bipolar plates (BPP) is a vital component of proton exchange membrane fuel cells (PEMFC), which supplies fuel and oxidant to reactive sites, remove reaction products, collects produced current and provide mechanical support for the cells in the stack. This work concerns the utilization of mill scale, a by-product of iron and steel formed during the hot rolling of steel, as a potential material for use as BPP in PEMFC. On the other hand, mill scale is considered a very rich in iron source having characteristic required such as for current collector in BPP and would significantly contribute to lower the overall cost of PEMFC based fuel cell systems. In this study, the iron reach source of mill scale powder, after sieving of 150 mesh, was mechanically alloyed with the carbon source containing 5, 10, and 15 wt.% graphite using a shaker mill for 3 h. The mixed powders were then pressed at 300 MPa and sintered at 900 °C for 1 h under inert gas atmosphere. The structural changes of powder particles during mechanical alloying and after sintering were studied by X-ray diffractometry, optical microscopy, scanning electron microscopy, and microhardness measurement. The details of the presence of iron, carbon, and iron carbide (Fe-C) as the products of reactions as well as sufficient mechanical strength of the sintered materials were presented in this report.

Industrial production of 131I by neutron irradiation and melting of sintered TeO2

NASA Astrophysics Data System (ADS)

Alanis, Jose; Navarrete, Manuel

2001-07-01

Optimal conditions of temperature and reaction rate have been settled to produce high purity TeO2 by the chemical reaction between Te and HNO3. Also, heating and time conditions for sintering this product have been found, in order to create cavities in the crystal inside, where a gaseous element such as iodine can be adsorbed with minimal leaking. In this way it is fabricated a suitable target to be irradiated with thermal neutrons for obtaining 131Te(t1/2=24.8 m) and 131mTe(t1/2=30 h) by (n, γ) nuclear reactions. Irradiation time has been chosen to get 131Te saturation activity (ti=150 m) because much longer irradiation times do not increase significantly total activity. Since parents 131Te and 131mTe have shorter half life than daughter 131I(t1/2=8.05 d) optimal cooling time must permit daughter activity to grow up till a maximum (tc=4d). Then, sintered cylinder shaped radioactive sample is manipulated in a hot cell, transported and put on a quartz tray, keeping Health Physics regulations. The quartz tray is inside a small electric oven enclosed in an airtight box with negative pressure (water 0.5 cm). There, it is gradually heated till melting point (733 °C). From 400 °C on, vapors are pumped out and bubbled in two solutions: one is 0.1 M NaOH, which retains nearly 99.9% of pumped 131I. Other is 0.02 M Na2CO3 (60%) plus 0.0025 M NaHCO3 (40%), which retains the remaining sample residue. Air filtering is accomplished by activated carbon and alumina filters in the inflow, glass wool fiber before bubbling, and activated carbon again in the outflow.

Effect of the application of surface treatments before and after sintering on the flexural strength, phase transformation and surface topography of zirconia.

PubMed

Kurtulmus-Yilmaz, Sevcan; Aktore, Huseyin

2018-05-01

To evaluate the effects of airborne-particle abrasion (APA) and Er,Cr:YSGG laser irradiation on 4-point-flexural strength, phase transformation and morphologic changes of zirconia ceramics treated at pre-sintered or post-sintered stage. Three hundred and forty-two bar shaped zirconia specimens were milled with different sizes according to the flexural strength test (n = 10), X-ray diffraction (XRD) (n = 4) and field emission scanning electron microscope (FE-SEM) (n = 4) analyses. For each test protocol, specimens were divided into 4 main groups whether the surface treatments applied before or after sintering and whether the specimens received heat treatment or not as pre-sintered, post-sintered no-heat and post-sintered heat-treated groups, and a group was served as control. Main groups were further divided into 6 equal subgroups according to surface treatment method applied (2 W-, 3 W-, 4 W-, 5 W-, 6 W-laser irradiations and APA). Surface treatments were applied to pre-sintered groups before sintering and to post-sintered groups after sintering. Post-sintered heat-treated groups were subjected to veneer ceramic firing simulation after surface treatments. Flexural strength and flexural modulus values were statistically analysed and monoclinic phase content was calculated. Weibull analysis was used to evaluate strength reliability and fractographic analysis was conducted. Highest flexural strength values were detected at post-sintered no-heat APA and 4W-laser groups (P < 0.05). Pre-sintered groups showed statistically lower flexural strength values. Heat treatment decreased the strength of the specimens. Monoclinic phase content was only detected at post-sintered no-heat groups and the highest amount was detected at APA group. Rougher surfaces and deeper irregularities were detected at FE-SEM images pre-sintered groups. Application of surface treatments at pre-sintered stage may be detrimental for zirconia ceramics in terms of flexural strength. Treating the surface of zirconia ceramic before sintering process is not recommended due to significant decrease in flexural strength values. 2 W-4 W Er,Cr:YSGG laser irradiations can be regarded as alternative surface treatment methods when zirconia restoration would be subjected to veneer ceramic firing procedures. Copyright © 2018 Elsevier Ltd. All rights reserved.

High density, uniformly distributed W/UO2 for use in Nuclear Thermal Propulsion

NASA Astrophysics Data System (ADS)

Tucker, Dennis S.; Barnes, Marvin W.; Hone, Lance; Cook, Steven

2017-04-01

An inexpensive, quick method has been developed to obtain uniform distributions of UO2 particles in a tungsten matrix utilizing 0.5 wt percent low density polyethylene. Powders were sintered in a Spark Plasma Sintering (SPS) furnace at 1600 °C, 1700 °C, 1750 °C, 1800 °C and 1850 °C using a modified sintering profile. This resulted in a uniform distribution of UO2 particles in a tungsten matrix with high densities, reaching 99.46% of theoretical for the sample sintered at 1850 °C. The powder process is described and the results of this study are given below.

Fabrication of thin layer beta alumina

NASA Technical Reports Server (NTRS)

Tennenhouse, G. J.

1977-01-01

Beta alumina tubes having walls 700 microns, 300 microns, and 140 microns were processed by extrusion and sintering utilizing Ford proprietary binder and fabrication systems. Tubes prepared by this method have properties similar to tubes prepared by isostatic pressing and sintering, i.e. density greater than 98% of theoretical and a helium leak rate less than 3 x 10 to the -9th power cc/sq cm/sec. Ford ultrasonic bonding techniques were used for bonding beta alumina end caps to open ended beta -alumina tubes prior to sintering. After sintering, the bond was hermetic, and the integrity of the bonded area was comparable to the body of the tube.

Liquid phase sintering of silicon carbide

DOEpatents

Cutler, R.A.; Virkar, A.V.; Hurford, A.C.

1989-05-09

Liquid phase sintering is used to densify silicon carbide based ceramics using a compound comprising a rare earth oxide and aluminum oxide to form liquids at temperatures in excess of 1,600 C. The resulting sintered ceramic body has a density greater than 95% of its theoretical density and hardness in excess of 23 GPa. Boron and carbon are not needed to promote densification and silicon carbide powder with an average particle size of greater than one micron can be densified via the liquid phase process. The sintered ceramic bodies made by the present invention are fine grained and have secondary phases resulting from the liquid phase. 4 figs.

Liquid phase sintering of silicon carbide

DOEpatents

Cutler, Raymond A.; Virkar, Anil V.; Hurford, Andrew C.

1989-01-01

Liquid phase sintering is used to densify silicon carbide based ceramics using a compound comprising a rare earth oxide and aluminum oxide to form liquids at temperatures in excess of 1600.degree. C. The resulting sintered ceramic body has a density greater than 95% of its theoretical density and hardness in excess of 23 GPa. Boron and carbon are not needed to promote densification and silicon carbide powder with an average particle size of greater than one micron can be densified via the liquid phase process. The sintered ceramic bodies made by the present invention are fine grained and have secondary phases resulting from the liquid phase.

Numerical investigation of the effects of iron oxidation reactions on the fume formation mechanism in arc welding

NASA Astrophysics Data System (ADS)

Sanibondi, Paolo

2015-09-01

Fume formation during arc welding has been modelled using a stochastic approach taking into account iron oxidation reactions. The model includes the nucleation and condensation of Fe and FeO vapours, the reaction of gaseous O2 and O on the nanoparticle surface, the coagulation of the nanoparticles including a sintering time as a function of temperature and composition, assuming chemical equilibrium for species in the gaseous phase. Results suggest that fumes generated in gas metal arc welding with oxidizing shielding mixtures are composed of aggregates of primary particles that are nucleated from gas-phase FeO and further oxidized to Fe3O4 and Fe2O3 in the liquid and solid phase, respectively. The composition of the fumes at the end of the formation process depends on the relative initial concentration of Fe and O2 species in the gas mixture and on the diameter of the primary particles that compose the aggregates: as the oxidation reactions are driven by deposition of oxygen on nanoparticle surface, the oxidation of larger particles is slower than that of smaller particles because of their lower surface to volume ratio. Solid-state diffusion is limiting the oxidation process at temperatures lower than 1500 K, inducing the formation of not fully oxidized particles composed of Fe3O4.

Effect of electrode material on characteristics of non-volatile resistive memory consisting of Ag{sub 2}S nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jang, Jaewon, E-mail: j1jang@knu.ac.kr

2016-07-15

In this study, Ag{sub 2}S nanoparticles are synthesized and used as the active material for two-terminal resistance switching memory devices. Sintered Ag{sub 2}S films are successfully crystallized on plastic substrates with synthesized Ag{sub 2}S nanoparticles, after a relatively low-temperature sintering process (200 °C). After the sintering process, the crystallite size is increased from 6.8 nm to 80.3 nm. The high ratio of surface atoms to inner atoms of nanoparticles reduces the melting point temperature, deciding the sintering process temperature. In order to investigate the resistance switching characteristics, metal/Ag{sub 2}S/metal structures are fabricated and tested. The effect of the electrode materialmore » on the non-volatile resistive memory characteristics is studied. The bottom electrochemically inert materials, such as Au and Pt, were critical for maintaining stable memory characteristics. By using Au and Pt inert bottom electrodes, we are able to significantly improve the memory endurance and retention to more than 10{sup 3} cycles and 10{sup 4} sec, respectively.« less

Investigation of consolidation kinetics and microstructure evolution of Al alloys in direct metal laser sintering using phase field simulation

NASA Astrophysics Data System (ADS)

Bimal Satpathy, Bubloom; Nandy, Jyotirmoy; Sahoo, Seshadev

2018-03-01

Direct metal laser sintering is one of the very efficient processes which comes under the field of additive manufacturing and is capable of producing products of good mechanical and physical properties. The process parameters affect the physical and mechanical properties of the final products. Rapid solidification plays an important role in the consolidation kinetics as the powdered material sinters and forms a polycrystalline structure. In the recent times, the enormous use of computational modeling has helped in examining the utility of final products in a wide range of applications. In this study, a phase field model has been implemented to foresee the consolidation kinetics during the liquid state sintering. Temperature profiles have been used to study the densification behavior and neck growth which is caused by the surface diffusion of particles at initial stage. Later, importance of grain boundary and the volume diffusion during densification process is analyzed. It is also found that with rise in temperature, neck growth also increases rapidly due to the interaction of adjacent grains through grain boundary diffusion and stabilization of grain growth.

Phase stability, porosity distribution and microstructural evolution of amorphous Al{sub 50}Ti{sub 50} powders consolidated by electrical resistance sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Urban, P., E-mail: purban@us.es; Montes, J. M.; Cintas, J.

2015-03-30

The effect of intensity and duration of the electrical resistance sintering process on the phase stability, porosity distribution and microstructural evolution of Al{sub 50}Ti{sub 50} amorphous powders is studied. The phase transformations during the consolidation process were determined by X-ray diffraction. The porosity distribution was observed by optical and scanning electron microscopy. The amorphous phase is partially transformed to the crystalline phase during the sintering process, and formation of AlTi and AlTi{sub 3} intermetallic compounds occurs for temperatures higher than 300 °C. Finally, it is observed that the compacts core have lower porosity and a higher tendency to the amorphous-crystallinemore » phase transformation than the periphery.« less

Effect of Partial Substitution of Neodymium with Praseodymium on the Magnetic and Process Properties of Sintered Magnets of Type NdFeB

NASA Astrophysics Data System (ADS)

Dormidontov, N. A.; Dormidontov, A. G.; Lileev, A. S.; Kamynin, A. V.; Lukin, A. A.

2017-01-01

The effect of substitution of neodymium with praseodymium in sintered magnets of type NdFeB on their magnetic and process properties in the concentration range of [Pr] = 0 - 13 wt.% is studied. The special features of milling of the alloys, sintering processes and heat treatments in the production of magnets containing praseodymium are discussed. Hysteresis characteristics of B r ≥ 1.2 T, H cJ ≥ 1200 kA/m, H cb ≥ 880 kA/m, H k ≥ 960 kA/m, and BH max ≥ 280 kJ/m3 are obtained for magnets with composition (in wt.%) 33 Nd, 10 Pr, 1.5 (Ti + Al + Cu), 1.3 B, the remainder Fe.

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

NASA Technical Reports Server (NTRS)

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 chromium site, we could sinter the materials below 1400 C. The doping concentrations were adjusted so that the thermal expansion coefficient matched that of the zirconia electrolyte. Also, the investigation was focused on stoichiometric compositions so that the materials would have better stability. Co-sintering and chemical compatibility with zirconia electrolyte were examined by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy (line scanning and dot map). The results showed that the materials bond well, but do not react, with zirconia electrolyte. The electric conductivity of the materials measured at 900 C in air was about 20 S/cm.

Process for the production of fuel gas from coal

DOEpatents

Patel, Jitendra G.; Sandstrom, William A.; Tarman, Paul B.

1982-01-01

An improved apparatus and process for the conversion of hydrocarbonaceous materials, such as coal, to more valuable gaseous products in a fluidized bed gasification reaction and efficient withdrawal of agglomerated ash from the fluidized bed is disclosed. The improvements are obtained by introducing an oxygen containing gas into the bottom of the fluidized bed through a separate conduit positioned within the center of a nozzle adapted to agglomerate and withdraw the ash from the bottom of the fluidized bed. The conduit extends above the constricted center portion of the nozzle and preferably terminates within and does not extend from the nozzle. In addition to improving ash agglomeration and withdrawal, the present invention prevents sintering and clinkering of the ash in the fluidized bed and permits the efficient recycle of fine material recovered from the product gases by contacting the fines in the fluidized bed with the oxygen as it emanates from the conduit positioned within the withdrawal nozzle. Finally, the present method of oxygen introduction permits the efficient recycle of a portion of the product gases to the reaction zone to increase the reducing properties of the hot product gas.

Microstructure and mechanical properties of nickel coated multi walled carbon nanotube reinforced stainless steel 316L matrix composites by laser sintering process

NASA Astrophysics Data System (ADS)

Mahanthesha, P.; Mohankumar, G. C.

2018-04-01

Electroless Ni coated Multi-walled Carbon nanotubes reinforced with Stainless Steel 316L matrix composite was developed by Direct Metal Laser Sintering process (DMLS). Homogeneous mixture of Stainless Steel 316L powder and carbon nanotubes in different vol. % was obtained by using double cone blender machine. Characterization of electroless Ni coated carbon nanotubes was done by using X-ray diffraction, FESEM and EDS. Test samples were fabricated at different laser scan speeds. Effect of process parameters and CNT vol. % content on solidification microstructure and mechanical properties of test samples was investigated by using Optical microscopy, FESEM, and Hounsfield tensometer. Experimental results reveal DMLS process parameters affect the density and microstructure of sintered parts. Dense parts with minimum porosity when processed at low laser scan speeds and low CNT vol. %. Tensile fractured surface of test specimens evidences the survival of carbon nanotubes under high temperature processing condition.

Strength and fatigue properties of three-step sintered dense nanocrystal hydroxyapatite bioceramics

NASA Astrophysics Data System (ADS)

Guo, Wen-Guang; Qiu, Zhi-Ye; Cui, Han; Wang, Chang-Ming; Zhang, Xiao-Jun; Lee, In-Seop; Dong, Yu-Qi; Cui, Fu-Zhai

2013-06-01

Dense hydroxyapatite (HA) ceramic is a promising material for hard tissue repair due to its unique physical properties and biologic properties. However, the brittleness and low compressive strength of traditional HA ceramics limited their applications, because previous sintering methods produced HA ceramics with crystal sizes greater than nanometer range. In this study, nano-sized HA powder was employed to fabricate dense nanocrystal HA ceramic by high pressure molding, and followed by a three-step sintering process. The phase composition, microstructure, crystal dimension and crystal shape of the sintered ceramic were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Mechanical properties of the HA ceramic were tested, and cytocompatibility was evaluated. The phase of the sintered ceramic was pure HA, and the crystal size was about 200 nm. The compressive strength and elastic modulus of the HA ceramic were comparable to human cortical bone, especially the good fatigue strength overcame brittleness of traditional sintered HA ceramics. Cell attachment experiment also demonstrated that the ceramics had a good cytocompatibility.

Spark plasma sintering synthesis of Ni1-xZnxFe2O4 ferrites: Mössbauer and catalytic study

NASA Astrophysics Data System (ADS)

Velinov, Nikolay; Manova, Elina; Tsoncheva, Tanya; Estournès, Claude; Paneva, Daniela; Tenchev, Krassimir; Petkova, Vilma; Koleva, Kremena; Kunev, Boris; Mitov, Ivan

2012-08-01

Nickel-zinc ferrite nanoparticles, Ni1-xZnxFe2O4 (x = 0, 0.2, 0.5, 0.8, 1.0) were prepared by combination of chemical precipitation and spark plasma sintering (SPS) techniques and conventional thermal treatment of the obtained precursors. The phase composition and structural properties of the obtained materials were investigated by X-ray diffraction and Mössbauer spectroscopy and their catalytic activity in methanol decomposition was tested. A strong effect of reaction medium leading to the transformation of ferrites to a complex mixture of different iron containing phases was detected. A tendency of formation of Fe-carbide was found for the samples synthesized by SPS, while predominantly iron-nickel alloys ware registered in TS obtained samples. The catalytic activity and selectivity in methanol decomposition to CO and methane depended on the current phase composition of the obtained ferrites, which was formed by the influence of the reaction medium.

Low temperature synthesis & characterization of lead-free BCZT ceramics using molten salt method

NASA Astrophysics Data System (ADS)

Jai Shree, K.; Chandrakala, E.; Das, Dibakar

2018-04-01

Piezoelectric properties are greatly influenced by the synthesis route, microstructure, stoichiometry of the chemical composition, purity of the starting materials. In this study, molten salt method was used to prepare lead-free BCZT ceramics. Molten salt method is one of the simplestmethods to prepare chemically-purified, single phase powders in high yield often at lower temperatures and shorten reaction time. Calcination of the molten salt synthesized powders resulted in asingle-phase perovskite structure at 1000 °C which is ˜ 350 °C less than the conventional solid-sate reaction method. With increasing calcination temperature the average template size was increased (˜ 0.5-2 µm). Formation of well dispersive templates improves the sinterability at lower temperatures. Lead-free BCZT ceramics sintered at 1500 °C for 2 h resulted in homogenous and highly dense microstructure with ˜92% of the theoretical density and a grain size of ˜ 35 µm. This highly dense microstructure could enhance the piezoelectric properties of the system.

Development of reaction-sintered SiC mirror for space-borne optics

NASA Astrophysics Data System (ADS)

Yui, Yukari Y.; Kimura, Toshiyoshi; Tange, Yoshio

2017-11-01

We are developing high-strength reaction-sintered silicon carbide (RS-SiC) mirror as one of the new promising candidates for large-diameter space-borne optics. In order to observe earth surface or atmosphere with high spatial resolution from geostationary orbit, larger diameter primary mirrors of 1-2 m are required. One of the difficult problems to be solved to realize such optical system is to obtain as flat mirror surface as possible that ensures imaging performance in infrared - visible - ultraviolet wavelength region. This means that homogeneous nano-order surface flatness/roughness is required for the mirror. The high-strength RS-SiC developed and manufactured by TOSHIBA is one of the most excellent and feasible candidates for such purpose. Small RS-SiC plane sample mirrors have been manufactured and basic physical parameters and optical performances of them have been measured. We show the current state of the art of the RS-SiC mirror and the feasibility of a large-diameter RS-SiC mirror for space-borne optics.

Weakly-agglomerated nanocrystalline (ZrO 2) 0.9(Yb 2O 3) 0.1 powders hydrothermally synthesized at low temperature

NASA Astrophysics Data System (ADS)

Dell'Agli, Gianfranco; Mascolo, Giuseppe; Mascolo, Maria Cristina; Pagliuca, Concetta

2006-09-01

Nanocrystalline ytterbia (10 mol%)-doped cubic zirconia powders were synthesized by hydrothermal treatment of either an amorphous co-precipitate of hydrated ytterbia-zirconia or of zirconia xerogel in mixture with crystalline Yb 2O 3. The treatments were performed at 110 °C in the presence of diluted (0.2 M) or concentrated (2.0 M) solution of (K 2CO 3 + KOH) mineralizer and for different reaction times. The reaction times for the full crystallization of cubic-YbSZ-based products were determined for both the employed precursors and for each mineralizer solution. The various fully crystallized products were characterized in their degree of agglomeration and sintered at 1500 °C for 2 h. The best performance on sintering was achieved with the less agglomerated powder synthesized from the mechanical mixture and in the presence of the diluted solution of the mineralizer. The resulting density was the highest achieved with materials having the same composition.

The Development of a Ti-6Al-4V Alloy via Oxygen Solid Solution Strengthening for Aerospace and Defense Applications

DTIC Science & Technology

2013-03-01

latter strategy. Mixtures of titanium powders and TiO2 particles were employed as starting materials and consolidated by spark - plasma sintering and...were consolidated in a carbon container installed in the spark - plasma sintering (SPS) equipment under vacuum condition (ɞ Pa) at a temperature of...evaluation of tensile properties of the wrought pure titanium materials consolidated by sintering and hot extrusion process, a theoretical approach using

Utilizing Interfaces for Nano- and Micro-scale Control of Thermal Conductivity

DTIC Science & Technology

2015-08-17

performance of these promising materials by 50%. Ballmilling and spark plasma sintering (SPS) processes were investigated to try to lower the thermal...samples fabricated through the spark plasma sintering ”, Mater Renew Sustain Energy, 3, 31-1 31-6 (2014). DOI: 10.1007/s40243-014-0031-8 9. O. Sologub...for doping of foreign elements (therefore no migration problems) is very striking. In further development, addition of Al as a sintering element was

Synthesis of Nano-Scale Fast Ion Conducting Cubic Li7La3Zr2O12

DTIC Science & Technology

2013-09-25

offer the flexibility to make nano-dimensional particles with high sinterability nor the ability to coat/protect electrode powders. By developing a...sintering temperature are needed. One possible approach is to use small particles , such as nano-scale particles , that can be sintered at lower temperatures...matrix to suppress Li dendrite penetration. By developing a sol–gel process, the LLZO particle size can be precisely tuned, from the nanometer to the

Transport, electronic, and structural properties of nanocrystalline CuAlO2 delafossites

NASA Astrophysics Data System (ADS)

Durá, O. J.; Boada, R.; Rivera-Calzada, A.; León, C.; Bauer, E.; de la Torre, M. A. López; Chaboy, J.

2011-01-01

This work reports on the effect of grain size on the electrical, thermal, and structural properties of CuAlO2 samples obtained by solid-state reaction combined with ball milling. Electrical characterization made in microcrystalline and nanocrystalline samples shows that the electrical conductivity decreases several orders of magnitude for the nanocrystalline samples, and, in addition, there is a large discrepancy between the activation energies associated to thermoelectric power ES. The study of the Cu K-edge x-ray absorption spectra of the CuAlO2 samples shows that the local structure around Cu is preserved after the sintering process, indicating that the observed behavior of the electrical conductivity is of intrinsic origin. Complex conductivity measurements as a function of frequency allow us to discard grain-boundaries effects on the electrical transport. Thus, the changes in σ(T) and S(T) are interpreted in terms of charge localization in the framework of small polarons. This is in agreement with the analysis of the near-edge region of the absorption spectra, which indicates that sintering favors the Cu-O hybridization. As a consequence, oxygen atoms progressively lose their capability of trapping holes, and the electrical conductivity is also enhanced.

Fracture behavior of metal-ceramic fixed dental prostheses with frameworks from cast or a newly developed sintered cobalt-chromium alloy.

PubMed

Krug, Klaus-Peter; Knauber, Andreas W; Nothdurft, Frank P

2015-03-01

The aim of this study was to investigate the fracture behavior of metal-ceramic bridges with frameworks from cobalt-chromium-molybdenum (CoCrMo), which are manufactured using conventional casting or a new computer-aided design/computer-aided manufacturing (CAD/CAM) milling and sintering technique. A total of 32 metal-ceramic fixed dental prostheses (FDPs), which are based on a nonprecious metal framework, was produced using a conventional casting process (n = 16) or a new CAD/CAM milling and sintering process (n = 16). Eight unveneered frameworks were manufactured using each of the techniques. After thermal and mechanical aging of half of the restorations, all samples were subjected to a static loading test in a universal testing machine, in which acoustic emission monitoring was performed. Three different critical forces were revealed: the fracture force (F max), the force at the first reduction in force (F decr1), and the force at the critical acoustic event (F acoust1). With the exception of the veneered restorations with cast or sintered metal frameworks without artificial aging, which presented a statistically significant but slightly different F max, no statistically significant differences between cast and CAD/CAM sintered and milled FDPs were detected. Thermal and mechanical loading did not significantly affect the resulting forces. Cast and CAD/CAM milled and sintered metal-ceramic bridges were determined to be comparable with respect to the fracture behavior. FDPs based on CAD/CAM milled and sintered frameworks may be an applicable and less technique-sensitive alternative to frameworks that are based on conventionally cast frameworks.

Temperature variation in metal ceramic technology analyzed using time domain optical coherence tomography

NASA Astrophysics Data System (ADS)

Sinescu, Cosmin; Topala, Florin I.; Negrutiu, Meda Lavinia; Duma, Virgil-Florin; Podoleanu, Adrian G.

2014-01-01

The quality of dental prostheses is essential in providing good quality medical services. The metal ceramic technology applied in dentistry implies ceramic sintering inside the dental oven. Every ceramic material requires a special sintering chart which is recommended by the producer. For a regular dental technician it is very difficult to evaluate if the temperature inside the oven remains the same as it is programmed on the sintering chart. Also, maintaining the calibration in time is an issue for the practitioners. Metal ceramic crowns develop a very accurate pattern for the ceramic layers depending on the temperature variation inside the oven where they are processed. Different patterns were identified in the present study for the samples processed with a variation in temperature of +30 °C to +50 °C, respectively - 30 0°C to -50 °C. The OCT imagistic evaluations performed for the normal samples present a uniform spread of the ceramic granulation inside the ceramic materials. For the samples sintered at a higher temperature an alternation between white and darker areas between the enamel and opaque layers appear. For the samples sintered at a lower temperature a decrease in the ceramic granulation from the enamel towards the opaque layer is concluded. The TD-OCT methods can therefore be used efficiently for the detection of the temperature variation due to the ceramic sintering inside the ceramic oven.

A sintering study on the β-spodumene-based glass ceramics prepared from gel-derived precursor powders with LiF additive

NASA Astrophysics Data System (ADS)

Wang, Moo-Chin; Wu, Nan-Chung; Yang, Sheng; Wen, Shaw-Bing

2002-01-01

Beta-spodumene (Li2O·Al2O3·4SiO2, LAS) powders were prepared by a sol-gel process using Si(OC2H5)4, Al(OC4H9)3, and LiNO3 as precursors and LiF as a sintering aid agent. Dilatometry, X-ray diffraction (XRD), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and electron diffraction (ED) were utilized to study the sintering, phase transformation, microstructure, and properties of the β-spodumene glass-ceramics prepared from the gel-derived precursor powders with and without LiF additives. For the LAS precursor powders containing no LiF, the only crystalline phase obtained was β-spodumene. For the pellets containing less than 4 wt pct LiF and sintered at 1050 °C for 5 hours the crystalline phases were β-spodumene and β-eucryptite (Li2O·Al2O3·2SiO2). When the LiF content was 5 wt pct and the sintering process was carried out at 1050 °C for 5 hours, the crystalline phases were β-spodumene, β-eucryptite (triclinic), and eucryptite (rhombohedral (hex.)) phases. With the LiF additive increased from 0.5 to 4 wt pct and sintering at 1050 °C for 5 hours, the open porosity of the sintered bodies decrease from 30 to 2.1 pct. The grains size is about to 4 to 5 µm when pellect LAS compact contains LiF 3 wt pct as sintered at 1050 °C for 5 hours. The grains size grew to 8 to 25 µm with a remarkable discontinuous grain growth for pellet LAS compact contain LiF 5 wt pct sintered at 1050 °C for 5 hours. Relative densities greater than 90 pct could be obtained for the LAS precursor powders with LiF > 2 wt pct when sintered at 1050 °C for 5 hours. The coefficient of thermal expansion of the sintered bodies decreased from 8.3 × 10-7 to 5.2 × 10-7/°C (25 °C to 900 °C) as the LiF addition increased from 0 to 5 wt pct.

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

NASA Astrophysics Data System (ADS)

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 of shape loss and viscosity of a semisolid aggregate. A mechanistic model, based on the semisolid rheological characteristics, is developed to predict the magnitude and nature of shape loss. The model shows good correlation with experimental data for bronze. This study offers critical insight into SLPS and provides processing strategies for fabrication of high-density components without shape loss.

High efficiency solution processed sintered CdTe nanocrystal solar cells: the role of interfaces.

PubMed

Panthani, Matthew G; Kurley, J Matthew; Crisp, Ryan W; Dietz, Travis C; Ezzyat, Taha; Luther, Joseph M; Talapin, Dmitri V

2014-02-12

Solution processing of photovoltaic semiconducting layers offers the potential for drastic cost reduction through improved materials utilization and high device throughput. One compelling solution-based processing strategy utilizes semiconductor layers produced by sintering nanocrystals into large-grain semiconductors at relatively low temperatures. Using n-ZnO/p-CdTe as a model system, we fabricate sintered CdTe nanocrystal solar cells processed at 350 °C with power conversion efficiencies (PCE) as high as 12.3%. JSC of over 25 mA cm(-2) are achieved, which are comparable or higher than those achieved using traditional, close-space sublimated CdTe. We find that the VOC can be substantially increased by applying forward bias for short periods of time. Capacitance measurements as well as intensity- and temperature-dependent analysis indicate that the increased VOC is likely due to relaxation of an energetic barrier at the ITO/CdTe interface.

Self Sealing Magmas

NASA Astrophysics Data System (ADS)

von Aulock, Felix W.; Wadsworth, Fabian B.; Kennedy, Ben M.; Lavallee, Yan

2015-04-01

During ascent of magma, pressure decreases and bubbles form. If the volume increases more rapidly than the relaxation timescale, the magma fragments catastrophically. If a permeable network forms, the magma degasses non-violently. This process is generally assumed to be unidirectional, however, recent studies have shown how shear and compaction can drive self sealing. Here, we additionally constrain skin formation during degassing and sintering. We heated natural samples of obsidian in a dry atmosphere and monitored foaming and impermeable skin formation. We suggest a model for skin formation that is controlled by diffusional loss of water and bubble collapse at free surfaces. We heated synthetic glass beads in a hydrous atmosphere to measure the timescale of viscous sintering. The beads sinter at drastically shorter timescales as water vapour rehydrates an otherwise degassed melt, reducing viscosity and glass transition temperatures. Both processes can produce dense inhomogeneities within the timescales of magma ascent and effectively disturb permeabilities and form barriers, particularly at the margins of the conduit, where strain localisation takes place. Localised ash in failure zones (i.e. Tuffisite) then becomes associated with water vapour fluxes and alow rapid rehydration and sintering. When measuring permeabilities in laboratory and field, and when discussing shallow degassing in volcanoes, local barriers for degassing should be taken into account. Highlighting the processes that lead to the formation of such dense skins and sintered infills of cavities can help understanding the bulk permeabilities of volcanic systems.

Effect of Sintering Temperature to Physical, Magnetic Properties and Crystal Structure on Permanent Magnet BaFe12O19 Prepared From Mill Scale

NASA Astrophysics Data System (ADS)

Ramlan; Muljadi; Sardjono, Priyo; Gulo, Fakhili; Setiabudidaya, Dedi

2017-07-01

Permanent magnet of Barium hexa Ferrite with formula BaFe12O19 has been made by metallurgy powder method from raw materials : Barium carbonate (BaCO3 E-merck) and Iron Oxide (Fe2O3 from mill scale). Both of raw materials have been mixed with stoichiometry composition by using a ball mill for 24 hours. The fine powder obtained from milling process was formed by using a hydraulic press at pressure 50 MPa and continued with sintering process. The sintering temperature was varied : 1150°C, 1200°C, 1250°C and 1300°C with holding time for 1 hour. The sintered samples were characterized such as : physical properties (bulk density, porosity and shrinkage), magnetic properties (flux density, remanence, coercivity and magnetic saturation) by using VSM and crystal structure by using XRD. According characterization results show that the crystal structure of BaFe12O19 does not change after sintering process, but the grain size tends to increase. The optimum condition is achieved at temperature 1250°C, and at this condition, the sample has characterization such as : bulk density = 4.35 g/cm3, porosity = 1.03% and firing shrinkage = 11.63%, flux density = 681.1 Gauss, remanence (σr) = 20.78 emu/g, coercivity (Hc) = 2058 Oe and magnetic saturation (σs) 45.16 emu/g.

Dielectric Properties of Sol-Gel Derived Barium Strontium Titanate and Microwave Sintering of Ceramics

NASA Astrophysics Data System (ADS)

Selmi, Fathi A.

This thesis consists of two areas of research: (1) sol-gel processing of Ba_{rm 1-x}Sr_{rm x} TiO_3 ceramics and their dielectric properties measurement; and (2) microwave versus conventional sintering of ceramics such as Al_2 O_3, Ba_{ rm 1-x}Sr_{rm x}TiO_3, Sb-doped SnO _2 and YBa_2Cu _3O_7. Sol-gel powders of BaTiO_3, SrTiO_3, and their solid solutions were synthesized by the hydrolysis of titanium isopropoxide and Ba and Sr methoxyethoxides. The loss tangent and dielectric constant of both sol-gel and conventionally prepared and sintered Ba_{rm 1-x}Sr _{rm x}TiO _3 ceramics were investigated at high frequencies. The sol-gel prepared ceramics showed higher dielectric constant and lower loss compared to those prepared conventionally. Ba _{rm 1-x}Sr _{rm x}TiO_3 ceramics were tunable with applied bias, indicating the potential use of this material for phase shifter applications. Porous Ba_{0.65}Sr _{0.35}TiO_3 was also investigated to lower the dielectric constant. Microwave sintering of alpha -Al_2O_3 and SrTiO_3 was investigated using an ordinary kitchen microwave oven (2.45 GHz; 600 Watts). The use of microwaves with good insulation of alpha -Al_2O_3 and SrTiO_3 samples resulted in their rapid sintering with good final densities of 96 and 98% of the theoretical density, respectively. A comparison of grain size for conventionally and microwave sintered SrTiO_3 samples did not show a noticeable difference. However, the grain size of microwave sintered alpha-Al_2O _3 was found to be larger than that of conventionally sintered sample. These results show that rapid sintering of ceramics can be achieved by using microwave radiation. The sintering behavior of coprecipitated Sb-doped SnO_2 was investigated using microwave power absorption. With microwave power, samples were sintered at 1450^circC for 20 minutes and showed a density as high as 99.9% of theoretical. However, samples fired in a conventional electric furnace at the same temperature for 4 hours showed only 60% of theoretical density. Microwave sintering also led to improvement in terms of uniform structure and electrical properties. Ba_{0.65}Sr _{0.35}TiO_3 was sintered using the microwave power at 1300 ^circC for 10 minutes. A density of 99% was achieved with small and uniform grain size. Superconducting powders have been successfully prepared by the sol-gel process and sintered and annealed using microwave power. Sintering and densification was achieved in a shorter time with microwave heating than with conventional heating and microwave heating appears to result in refined microstructure.

Effect of Starch on Sintering Behavior for Fabricating Porous Cordierite Ceramic

NASA Astrophysics Data System (ADS)

Li, Ye; Cao, Wei; Gong, Lunlun; Zhang, Ruifang; Cheng, Xudong

2016-10-01

Porous cordierite ceramics were prepared with starch as pore-forming agent by solid-state method. The green bodies were sintered at 1,100-1,400 °C for 2 h. The characterization was focused on thermal analysis, phase evolution, sintering behavior, porosity and micro-structural changes. The results show that cordierite becomes the main crystallization phase at 1,200 °C. The shrinkage behavior shows the most obvious dependence on the sintering temperature and starch content, and it can be divided into three stages. Moreover, the open porosity increases with the increase of starch content, but the pore-forming effectivity decreases. Nevertheless, compared with the open porosity curves, the bulk density curves are more in line with the linear rule. The microphotographs show the densification process with the sintering temperature and the variation of pore connectivity with the starch content.

PRODUCCION DE PLACAS DELGADAS DE UO$sub 2$ INFORME NO. 71. (Production of Thin Plates of UO$sub 2$. Report No. 71)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koll, H.; Carrea, A.J.

1962-01-01

The effect of some parameters on the fabrication of thin plates of UO/ sub 2/ by the sintering process is studied. Compacting pressures of 0.25 to 2 ton/cm/sub 2/, temperatures from 1100 to 1400 deg C, and sintering times from 1 to 3 hrs were used to determine the optimum values of these parameters. An analysis of the effect of the lubricant during the compression showed that the results were improved by the substitution of polyethylene glycol types for steric types, as the former were more easily removed from the compact and did not attack the UO/sub 2/ during sintering.more » Fracture during compression and extraction was studied. The compression law for the powder was determined, and the valid ity of the Bal'shin law was proved. The furnace atmospher is of importance to the sintered product. Two types of atmosphere were analyzed ---neutral atmosphere during sintering with final reduction in hydrogen and slightly reducing atmosphere during the entire process. An analysis of the effects on the final density and porosity showed that adding 3% H/sub 2/ to Ar produced good density and a stoichiometric oxide in the final product. It was shown that density is not a sufficient measurement to evaluate the degree of sintering. Only the combined use of density and porosity give a good evaluation. The compression pressure has a great effect on the pore size and distribution in the sintered product. Best results are obtained with high pressures, which gives small uniformly distributed pores. A metallographic study was made to determine the relation between pore size and distribution and the process parameters. Compact zones'' were observed with mean diameter from 1 to 2 mm with very reduced porosity. These zones had better hardness and resistance to corrosion and chemical attack than the rest of the material. (tr-auth)« less

Reproducibility of Aluminum Foam by Combining Sintering and Dissolution Process with Precursor Foaming Process

NASA Astrophysics Data System (ADS)

Hangai, Yoshihiko; Matsushita, Hayato; Koyama, Shinji; Suzuki, Ryosuke; Matsubara, Masaaki

2017-07-01

A preliminary study of the reproducibility of aluminum foam was performed. Aluminum foam was fabricated by a sintering and dissolution process. It was found that aluminum foam containing a blowing agent can be fabricated without the decomposition of the blowing agent, namely, the densified aluminum foam can be used as a foamable precursor for refoaming. By heat treatment of the densified aluminum foam containing the blowing agent, pores were reproduced in the aluminum.

Influence of processing parameters on the structure and properties of barium strontium titanate ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yun Sining; Department of Materials Physics, School of Science, Xi'an Jiaotong University, Xi'an 710049; Wang Xiaoli

2008-08-04

Barium strontium titanate (BST) with the molar formula (Ba{sub 0.8}Sr{sub 0.2}TiO{sub 3}) has been prepared by two different processing methods: mixed-oxide (BST-MO) and reaction-sintering (BST-RS). X-ray powder diffraction study shows differences in grain size and crystal symmetry for both these ceramics. The former shows a tetragonal symmetry while the latter presents a cubic symmetry. The occurrence of polar micro-regions associated with the higher chemical non-homogeneous distribution of ion defects from the influence of the processing parameters is the main reason for the higher peak dielectric constant (K{sub m}), the higher remanent polarization (P{sub r}), the higher coercive field (E{sub c}),more » the higher peak current density (J{sub m}), and the lower temperature of peak dielectric constant (T{sub m}) in BST-MO ceramics.« less

WSi2 in Si(1-x)Ge(x) Composites: Processing and Thermoelectric Properties

NASA Technical Reports Server (NTRS)

Mackey, Jonathan A.; Sehirlioglu, Alp; Dynys, Fred

2015-01-01

Traditional SiGe thermoelectrics have potential for enhanced figure of merit (ZT) via nano-structuring with a silicide phase, such as WSi2. A second phase of nano-sized silicides can theoretically reduce the lattice component of thermal conductivity without significantly reducing the electrical conductivity. However, experimentally achieving such improvements in line with the theory is complicated by factors such as control of silicide size during sintering, dopant segregation, matrix homogeneity, and sintering kinetics. Samples were prepared using powder metallurgy techniques; including mechano-chemical alloying, via ball milling, and spark plasma sintering for densification. Processing, micro-structural development, and thermoelectric properties will be discussed. Additionally, couple and device level characterization will be introduced.

Processing of non-oxide ceramics from sol-gel methods

DOEpatents

Landingham, Richard; Reibold, Robert A.; Satcher, Joe

2014-12-12

A general procedure applied to a variety of sol-gel precursors and solvent systems for preparing and controlling homogeneous dispersions of very small particles within each other. Fine homogenous dispersions processed at elevated temperatures and controlled atmospheres make a ceramic powder to be consolidated into a component by standard commercial means: sinter, hot press, hot isostatic pressing (HIP), hot/cold extrusion, spark plasma sinter (SPS), etc.

Examination of the Mass Transfer of Additive Elements in Barium Titanate Ceramics during Sintering Process by Laser Ablation ICP-MS.

PubMed

Sakate, Daisuke; Iwazaki, Yoshiki; Kon, Yoshiaki; Yokoyama, Takaomi; Ohata, Masaki

2018-01-01

The mass transfer of additive elements during the sintering of barium titanate (BaTiO 3 ) ceramic was examined by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) in the present study. An analytical sample consisting of two pellets of BaTiO 3 with different concentrations of additive elements of manganese (Mn) and holmium (Ho) as well as silicon (Si) as a sintering reagent was prepared and measured by LA-ICP-MS with small laser irradiated diameter of 10 μm to evaluate the distributions and concentrations of additive elements in order to examine their mass transfers. As results, enrichments of Mn and Si as an additive element and a sintering reagent, respectively, were observed on the adhesive surface between two BaTiO 3 pellets, even though Ho did not show a similar phenomenon. The mass transfers of additive elements of Mn and Ho were also examined, and Mn seemed to show a larger mass transfer than that of Ho during the sintering process for BaTiO 3 ceramics. The results obtained in this study shows the effectives of LA-ICP-MS for the future improvement of MLCCs.

Study of sintering on Mg-Zn-Ca alloy system

NASA Astrophysics Data System (ADS)

Annur, Dhyah; Lestari, Franciska P.; Erryani, Aprilia; Kartika, Ika

2018-05-01

Magnesium and its alloy have gained a lot of interest to be used in biomedical application due to its biodegradable and biocompatible properties. In this study, sintering process in powder metallurgy was chosen to fabricatenonporous Mg-6Zn-1Ca (in wt%) alloy and porous Mg-6Zn-1Ca-10 Carbamide alloy. For creating porous alloy, carbamide (CO(NH2)2 was added to alloy system as the space holder to create porous structure material. Effect of the space holder addition and sintering temperature on porosity, phase formation, mechanical properties, and corrosion properties was observed. Sintering process was done in a tube furnace under Argon atmosphere in for 5 hours. The heat treatment was done in two steps; heated up at 250 °C for 4 hours to decompose spacer particle, followed by heated up at 580 °C or 630 °C for 5 hours. The porous structure of the resulted alloys was examined using Scanning Electron Microscope (SEM), while the phase formation was characterized by X-ray diffraction (XRD) analysis. Mechanical properties were examined using compression testing. From this study, increasing sintering temperature up to 630 °C reduced the mechanical properties of Mg-Zn-Ca alloy.

Thermoelectric properties of Ca0.8Dy0.2MnO3 synthesized by solution combustion process

NASA Astrophysics Data System (ADS)

Park, Kyeongsoon; Lee, Ga Won

2011-10-01

High-quality Ca0.8Dy0.2MnO3 nano-powders were synthesized by the solution combustion process. The size of the synthesized Ca0.8Dy0.2MnO3 powders was approximately 23 nm. The green pellets were sintered at 1150-1300°C at a step size of 50°C. Sintered Ca0.8Dy0.2MnO3 bodies crystallized in the perovskite structure with an orthorhombic symmetry. The sintering temperature did not affect the Seebeck coefficient, but significantly affected the electrical conductivity. The electrical conductivity of Ca0.8Dy0.2MnO3 increased with increasing temperature, indicating a semiconducting behavior. The absolute value of the Seebeck coefficient gradually increased with an increase in temperature. The highest power factor (3.7 × 10-5 Wm-1 K-2 at 800°C) was obtained for Ca0.8Dy0.2MnO3 sintered at 1,250°C. In this study, we investigated the microstructure and thermoelectric properties of Ca0.8Dy0.2MnO3, depending on sintering temperature.

Thermoelectric properties of Ca0.8Dy0.2MnO3 synthesized by solution combustion process

PubMed Central

2011-01-01

High-quality Ca0.8Dy0.2MnO3 nano-powders were synthesized by the solution combustion process. The size of the synthesized Ca0.8Dy0.2MnO3 powders was approximately 23 nm. The green pellets were sintered at 1150-1300°C at a step size of 50°C. Sintered Ca0.8Dy0.2MnO3 bodies crystallized in the perovskite structure with an orthorhombic symmetry. The sintering temperature did not affect the Seebeck coefficient, but significantly affected the electrical conductivity. The electrical conductivity of Ca0.8Dy0.2MnO3 increased with increasing temperature, indicating a semiconducting behavior. The absolute value of the Seebeck coefficient gradually increased with an increase in temperature. The highest power factor (3.7 × 10-5 Wm-1 K-2 at 800°C) was obtained for Ca0.8Dy0.2MnO3 sintered at 1,250°C. In this study, we investigated the microstructure and thermoelectric properties of Ca0.8Dy0.2MnO3, depending on sintering temperature. PMID:21974984

Thermoelectric properties of Ca0.8Dy0.2MnO3 synthesized by solution combustion process.

PubMed

Park, Kyeongsoon; Lee, Ga Won

2011-10-05

High-quality Ca0.8Dy0.2MnO3 nano-powders were synthesized by the solution combustion process. The size of the synthesized Ca0.8Dy0.2MnO3 powders was approximately 23 nm. The green pellets were sintered at 1150-1300°C at a step size of 50°C. Sintered Ca0.8Dy0.2MnO3 bodies crystallized in the perovskite structure with an orthorhombic symmetry. The sintering temperature did not affect the Seebeck coefficient, but significantly affected the electrical conductivity. The electrical conductivity of Ca0.8Dy0.2MnO3 increased with increasing temperature, indicating a semiconducting behavior. The absolute value of the Seebeck coefficient gradually increased with an increase in temperature. The highest power factor (3.7 × 10-5 Wm-1 K-2 at 800°C) was obtained for Ca0.8Dy0.2MnO3 sintered at 1,250°C. In this study, we investigated the microstructure and thermoelectric properties of Ca0.8Dy0.2MnO3, depending on sintering temperature.

Calcium aluminate in alumina

NASA Astrophysics Data System (ADS)

Altay, Arzu

The properties of ceramic materials are determined not only by the composition and structure of the phases present, but also by the distribution of impurities, intergranular films and second phases. The phase distribution and microstructure both depend on the fabrication techniques, the raw materials used, the phase-equilibrium relations, grain growth and sintering processes. In this dissertation research, various approaches have been employed to understand fundamental phenomena such as grain growth, impurity segregation, second-phase formation and crystallization. The materials system chosen was alumina intentionally doped with calcium. Atomic-scale structural analyses of grain boundaries in alumina were carried on the processed samples. It was found that above certain calcium concentrations, CA6 precipitated as a second phase at all sintering temperatures. The results also showed that abnormal grain growth can occur after precipitation and it is not only related to the calcium level, but it is also temperature dependent. In order to understand the formation mechanism of CA6 precipitates in calcium doped alumina samples, several studies have been carried out using either bulk materials or thin films The crystallization of CA2 and CA6 powders has been studied. Chemical processing techniques were used to synthesize the powders. It was observed that CA2 powders crystallized directly, however CA6 powders crystallized through gamma-Al 2O3 solid solution. The results of energy-loss near-edge spectrometry confirmed that gamma-Al2O3 can dissolve calcium. Calcium aluminate/alumina reaction couples have also been investigated. All reaction couples were heat treated following deposition. It was found that gamma-Al2O3 was formed at the interface as a result of the interfacial reaction between the film and the substrate. gamma-Al 2O3 at the interface was stable at much higher temperatures compared to the bulk gamma-Al2O3 formed prior to the CA6 crystallization. In order to complement the studies carried out on the calcium aluminate phases, energy-loss near-edge structure (ELNES) fingerprints of CA2 and CA6 were obtained. It was shown that it is possible to distinguish these phases from each other by comparing the ELNES fingerprints. Theoretical calculations of ELNES were used to assign spectral features to certain symmetry environments that can later be used to understand the structures of unknown materials.

Improved Tubulars for Better Economics in Deep Gas Well Drilling using Microwave Technology

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dinesh Agrawal; Paul Gigl; Mahlon Dennis

2006-02-01

The objective of the research program has been to improve the rate-of-penetration in deep hostile environments by improving the life cycle and performance of coiled-tubing, an important component of a deep well drilling system for oil and gas exploration. The current process of the manufacture long tubular steel products consists of shaping the tube from flat strip, welding the seam and sections into lengths that can be miles long, and coiling onto reels. However, the welds, that are a weak point, now limit the performance of the coil tubing. This is not only from a toughness standpoint but also frommore » a corrosion standpoint. By utilizing the latest developments in the sintering of materials with microwave energy and powder metal extrusion technology for the manufacture of seamless coiled tubing and other tubular products, these problems can be eliminated. The project is therefore to develop a continuous microwave process to sinter continuously steel tubulars and butt-join them using microwave/induction process. The program started about three years ago and now we are in the middle of Phase II. In Phase I (which ended in February 2005) a feasibility study of the extrusion process of steel powder and continuously sinter the extruded tubing was conducted. The research program has been based on the development of microwave technology to process tubular specimens of powder metals, especially steels. The existing microwave systems at the Materials Research Laboratory (MRL) and Dennis Tool Company (DTC) were suitably modified to process tubular small specimens. The precursor powder metals were either extruded or cold isostatically pressed (CIP) to form tubular specimens. After conducting an extensive and systematic investigation of extrusion process for producing long tubes, it was determined that there were several difficulties in adopting extrusion process and it cannot be economically used for producing thousands of feet long green tubing. Therefore, in the Phase II the approach was modified to the microwave sintering combined with Cold Isostatic Press (CIP) and joining (by induction or microwave). This process can be developed into a semi-continuous sintering process if the CIP can produce parts fast enough to match the microwave sintering rates. This report summarizes the progress made to-date in this new approach. The final steel composition matching with the Quality tubing's QT-16Cr80 was short listed and used for all experiments. Bonding experiments using 4 different braze powders were conducted and the process optimized to obtain high degree of bonding strength. For fabrication of green tubulars a large CIP unit was acquired and tested. This equipment is located at the Dennis Tool facility in Houston. Microwave sintering experiments for continuous processing of the CIPed tubes are under progress in order to identify the optimum conditions. There have been some reproducibility problems and we are at present working to resolve these problems.« less

Correlation of gold in siliceous sinters with 3He 4He in hot spring waters of Yellowstone National Park

USGS Publications Warehouse

Fournier, R.O.; Kennedy, B.M.; Aoki, M.; Thompson, J.M.

1994-01-01

Opaline sinter samples collected at Yellowstone National Park (YNP) were analyzed for gold by neutron activation and for other trace elements by the inductively coupled plasma optical emission spectroscopy (ICP-OES) method. No correlation was found between Au and As, Sb, or total Fe in the sinters, although the sample containing the highest Au also contains the highest Sb. There also was no correlation of Au in the sinter with the H2S concentration in the discharged hot spring water or with the estimated temperature of last equilibration of the water with the surrounding rock. The Au in rhyolitic tuffs and lavas at YNP found within the Yellowstone caldera show the same range in Au as do those outside the caldera, while thermal waters from within this caldera all have been found to contain relatively low dissolved Au and to deposit sinters that contain relatively little Au. Therefore, it is not likely that variations in Au concentrations among these sinters simply reflect differences in leachable Au in the rocks through which the hydrothermal fluids have passed. Rather, variations in [H2S], the concentration of total dissolved sulfide, that result from different physical and chemical processes that occur in different parts of the hydrothermal system appear to exert the main control on the abundance of Au in these sinters. Hydrothermal fluids at YNP convect upward through a series of successively shallower and cooler reservoirs where water-rock chemical and isotopic reactions occur in response to changing temperature and pressure. In some parts of the system the fluids undergo decompressional boiling, and in other parts they cool conductively without boiling. Mixing of ascending water from deep in the system with shallow groundwaters is common. All three processes generally result in a decrease in [H2S] and destabilize dissolved gold bisulfide complexes in reservoir waters in the YNP system. Thus, different reservoirs in rocks of similar composition and at similar temperatures may contain waters with different [H2S] and [Au]. The [H2S] in a subsurface reservoir water is difficult to assess on the basis of analyses of hot spring waters because of uncertainties about steam loss during fluid ascent. However, the same processes that result in low [H2S] in reservoir waters also tend to result in decreases in the ratio of 3He 4He(R) dissolved in that water. Values of R relative to this ratio in air (Ra) attain values > 15 in YNP thermal waters. To date, all of the thermal waters at YNP that have R Ra values <9 have been found to deposit sinters with relatively low gold concentrations. These include all of the thermal waters that discharge from 180-215??C reservoirs at Upper, Midway, and Lower Geyser Basins within the western part of the Yellowstone caldera, and thermal waters at Norris Geyser Basin, outside the Yellowstone caldera, where some of the waters flow directly to the surface from a reservoir where the temperature is about 300??C. A high 3He 4He ratio in thermal water discharged at the surface does not guarantee high gold concentrations in the sinter deposited by this water. Boiling with loss of steam (the gas phase takes a separate route to the surface) during rapid upflow from the shallowest reservoir to the surface decreases the [H2S] and total He dissolved in the residual liquid without appreciably changing the 3He 4He ratio. This is because the isotopic composition of the He of the initial bulk fluid is unchanged and there is too little time for much radiogenic 4He to build back into the liquid during this rapid ascent from the near-surface reservoir. However, if boiling with phase separation and loss of steam occurs deep in the system, the 3He 4He ratio in the residual liquid, now depleted in H2S and total He, will be susceptible to dilution with radiogenic 4He that is acquired during the longer residence time underground. Some or all of the Au that comes out of solution when an initial gold bisulfide complex breaks

Porous calcium polyphosphate bone substitutes: additive manufacturing versus conventional gravity sinter processing-effect on structure and mechanical properties.

PubMed

Hu, Youxin; Shanjani, Yaser; Toyserkani, Ehsan; Grynpas, Marc; Wang, Rizhi; Pilliar, Robert

2014-02-01

Porous calcium polyphosphate (CPP) structures proposed as bone-substitute implants and made by sintering CPP powders to form bending test samples of approximately 35 vol % porosity were machined from preformed blocks made either by additive manufacturing (AM) or conventional gravity sintering (CS) methods and the structure and mechanical characteristics of samples so made were compared. AM-made samples displayed higher bending strengths (≈1.2-1.4 times greater than CS-made samples), whereas elastic constant (i.e., effective elastic modulus of the porous structures) that is determined by material elastic modulus and structural geometry of the samples was ≈1.9-2.3 times greater for AM-made samples. X-ray diffraction analysis showed that samples made by either method displayed the same crystal structure forming β-CPP after sinter annealing. The material elastic modulus, E, determined using nanoindentation tests also showed the same value for both sample types (i.e., E ≈ 64 GPa). Examination of the porous structures indicated that significantly larger sinter necks resulted in the AM-made samples which presumably resulted in the higher mechanical properties. The development of mechanical properties was attributed to the different sinter anneal procedures required to make 35 vol % porous samples by the two methods. A primary objective of the present study, in addition to reporting on bending strength and sample stiffness (elastic constant) characteristics, was to determine why the two processes resulted in the observed mechanical property differences for samples of equivalent volume percentage of porosity. An understanding of the fundamental reason(s) for the observed effect is considered important for developing improved processes for preparation of porous CPP implants as bone substitutes for use in high load-bearing skeletal sites. Copyright © 2013 Wiley Periodicals, Inc.

Development of high Tc (greater than 110K) Bi, Tl and Y-based materials as superconducting circuit elements

NASA Technical Reports Server (NTRS)

Haertling, Gene H.; Lee, Burtrand; Grabert, Gregory; Gilmour, Phillip

1991-01-01

This report is presented in two parts. Part 1 deals primarily with Bi-based materials and a small amount of work on a Y-based composition while Part 2 covers work on Tl-based materials. In Part 1, a reliable and reproducible process for producing bulk bismuth-based superconductors has been developed. It is noted however, that a percentage of the tapecast material experiences curling and fracturing after a 30 hour sintering period and is thus in need of further examination. The Bi-Sr-Ca-Cu-O (BSCCO) material has been characterized by critical temperature data, X-ray diffraction data, and surface morphology. In the case of T sub c, it is not critical to anneal the material. It appears that the BSCCO material has the possibility of producing a better grounding strap than that of the 123 material. Attempts to reproduce near room temperature superconductors in the Y-Ba-Cu-O system were unsuccessful. In Part 2, several methods of processing the high temperature superconductor Tl2Ba2Ca2Cu3O10 were investigated; i.e., different precursor compositions were sintered at various sintering times and temperatures. The highest superconductig temperature was found to be 117.8K when fired at 900 C for three hours. Higher sintering temperatures produced a melted sample which was nonsuperconducting at liquid nitrogen temperature. Also, a preliminary study found Li2O substitutions for copper appeared to increase the transition temperature and create fluxing action upon sintering. It was suggested that lower sintering temperatures might be obtained with lithium additions to produce reliable Tl2Ba2Ca2Cu3O10 processing methods.

Sinterable Powders from Laser Driven Reactions

DTIC Science & Technology

1979-07-01

18) line was based on information from the liter- ature (Tindal, et. al., 1942) rather than direct correlation with spectro- graphic data. Amonia ...number of lines to be measured; (2) laser intensity was sufficiently low to preclude virtually any heating of the silane or amonia . Two methods were used

High resolution laser micro sintering / melting using q-switched and high brilliant laser radiation

NASA Astrophysics Data System (ADS)

Exner, H.; Streek, A.

2015-03-01

Since the discovery of selective laser sintering/melting, numerous modifications have been made to upgrade or customize this technology for industrial purposes. Laser micro sintering (LMS) is one of those modifications: Powders with particles in the range of a few micrometers are used to obtain products with highly resolved structures. Pulses of a q-switched laser had been considered necessary in order to generate sinter layers from the micrometer scaled metal powders. LMS has been applied with powders from metals as well as from ceramic and cermet feedstock's to generate micro parts. Recent technological progress and the application of high brilliant continuous laser radiation have now allowed an efficient laser sintering/melting of micrometer scaled metal powders. Thereby it is remarkable that thin sinter layers are generated using high continuous laser power. The principles of the process, the state of the art in LMS concerning its advantages and limitations and furthermore the latest results of the recent development of this technology will be presented. Laser Micro Sintering / Laser Micro Melting (LMM) offer a vision for a new dimension of additive fabrication of miniature and precise parts also with application potential in all engineering fields.

Characterizing Sintered Nano-Hydroxyapatite Sol-Gel Coating Deposited on a Biomedical Ti-Zr-Nb Alloy

NASA Astrophysics Data System (ADS)

Jafari, Hassan; Hessam, Hamid; Shahri, Seyed Morteza Ghaffari; Assadian, Mahtab; Shairazifard, Shahin Hamtaie Pour; Idris, Mohd Hasbullah

2016-03-01

In this study, sol-gel dip-coating method was used to coat nano-hydroxyapatite on specimens of Ti-14Zr-13Nb alloy for orthopedic applications. The coated specimens were sintered at three different temperatures and time spans to evaluate the impact of sintering process on microstructure, mechanical, bio-corrosion, and bioactivity properties of the coating. Field-emission scanning electron microscopy and x-ray diffraction were used to analyze the coating microstructure. Coating adhesion and mechanical performance were also investigated by scratch testing. Besides, electrochemical corrosion and immersion tests were performed in simulated body fluid to examine the sintering effect on corrosion performance and bioactivity of the coatings, respectively. The evaluations of coated specimens displayed that sintering at elevated temperatures leads to higher surface integrity and improves crystallinity of the nano-hydroxyapatite to approximately 89% which brings about distinctively enhanced mechanical properties. Similarly, it improved the corrosion rate for about 17 times through sintering at 700 °C. Immersion test proved that the coating increased the bioactivity resulted from the dissolution of calcium phosphates into the corresponding environment. It is noticeable that sintering the dip-coated specimens in the nano-hydroxyapatite improves corrosion performance and maintains bioactive behaviors as well.

Generalized green synthesis and formation mechanism of sponge-like ferrite micro-polyhedra with tunable structure and composition

NASA Astrophysics Data System (ADS)

Tong, Guoxiu; Du, Fangfang; Xiang, Lingjing; Liu, Fangting; Mao, Lulu; Guan, Jianguo

2013-12-01

This paper describes a green versatile glucose-engineered precipitation-sintering process that allows for the selective and mass preparation of spongy porous ferrite (M = Fe, Zn, Co, Ni, Mn, etc.) micro-polyhedra with tunable morphology, texture, and composition. Some kinetic factors, such as the molar ratio of glucose to metal nitrates, reaction temperature, sintering temperature and time, and type of metal nitrates, can be expediently employed to modulate their aspect ratio, shape, size, composition, and textural properties. In this protocol, glucose functions as a reductant, protecting agent, structure-directing agent, and a sacrificial template to guide the assembly of sheet-like nuclei into polyhedral precursors and the formation of spongy porous structures. Owing to larger EM parameters, multiresonant behavior, and dissipative current, spongy porous Fe3O4 polyhedra exhibited enhanced microwave-absorbing properties. This endows them with important potential applications in magnetic devices, catalysis, sorption, photoluminescence, electromagnetic wave absorbing materials, anode materials, and so on. Meanwhile, this general approach can be extended to synthesize other porous sponges with regular geometric configuration because it is simple, inexpensive, environmentally benign, and suitable for extensive production.This paper describes a green versatile glucose-engineered precipitation-sintering process that allows for the selective and mass preparation of spongy porous ferrite (M = Fe, Zn, Co, Ni, Mn, etc.) micro-polyhedra with tunable morphology, texture, and composition. Some kinetic factors, such as the molar ratio of glucose to metal nitrates, reaction temperature, sintering temperature and time, and type of metal nitrates, can be expediently employed to modulate their aspect ratio, shape, size, composition, and textural properties. In this protocol, glucose functions as a reductant, protecting agent, structure-directing agent, and a sacrificial template to guide the assembly of sheet-like nuclei into polyhedral precursors and the formation of spongy porous structures. Owing to larger EM parameters, multiresonant behavior, and dissipative current, spongy porous Fe3O4 polyhedra exhibited enhanced microwave-absorbing properties. This endows them with important potential applications in magnetic devices, catalysis, sorption, photoluminescence, electromagnetic wave absorbing materials, anode materials, and so on. Meanwhile, this general approach can be extended to synthesize other porous sponges with regular geometric configuration because it is simple, inexpensive, environmentally benign, and suitable for extensive production. Electronic supplementary information (ESI) available: Nitrogen adsorption-desorption isotherms, the corresponding pore size distribution curves, TG-DSC curves, XRD pattern, and IR spectra for the precursors; XRD patterns of the samples obtained at various temperatures under N2; XRD pattern, reduction rate, and reactive oxygen species production of ZnO-ZnFe2O4 XRD patterns, SEM images, EDX patterns, nitrogen adsorption-desorption isotherms, and the corresponding pore size distribution curves of CoFe2O4-NiFe2O4-Co1.29Ni1.71O4 polyhedra and NiO-ZnFe2O4. See DOI: 10.1039/c3nr03745b

Utilization of lignite power generation residues for the production of lightweight aggregates.

PubMed

Anagnostopoulos, Iason M; Stivanakis, Victor E

2009-04-15

A novel process is proposed for the utilization of lignite combustion solid residues in the production of inflammable lightweight aggregates (LWA). The process consists of two stages, pelletization and sintering, and carbon contained in BA was used as the process fuel. The main residues bottom ash (BA) and fly ash (FA) from Megalopolis power plant were characterized, mixed in different proportions and treated through pelletization and sintering process. Sintering benefits from combustion of BA carbon content and the product is a hardened porous cake. The energy required for achievement of high temperatures, in the range of 1250 degrees C, was offered by carbon combustion and CO(2) evolution is responsible for porous structure formation. Selected physical properties of sintered material relevant to use as lightweight aggregates were determined, including bulk density, porosity and water absorption. Bulk density varies from 0.83 to 0.91 g/cm(3), porosity varies from 60% to 64% and water absorption varies from 66% to 80%. LWA formed is used for the production of lightweight aggregate concrete (LWAC). Thermal conductivity coefficient varies from 0.25 to 0.37 W/mK (lower than maximum limit 0.43 W/mK) and compressive strength varies from 19 to 23 MPa (higher than minimum limit 17 MPa). The results indicate that sintering of lignite combustion residues is an efficient method of utilization of carbon containing BA and production of LWA for structural and insulating purposes. Carbon content of BA is a key factor in LWA production. Finally, this research work comprises the first proposed application for utilization of BA in Greece.

Additive Manufacturing Consolidation of Low-Cost Water Atomized Steel Powder Using Micro-Induction Sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carter, William G.; Rios, Orlando; U

ORNL worked with Grid Logic Inc to demonstrate micro induction sintering (MIS) and binder decomposition of steel powders. It was shown that MIS effectively emits spatially confined electromagnetic energy that is directly coupled to metallic powders resulting in resistive heating of individual particles. The non-uniformity of particle morphology and distribution of the water atomized steel powders resulted in inefficient transfer of energy. It was shown that adhering the particles together using polymer binders resulted in more efficient coupling. Using the MIS processes, debinding and sintering could be done in a single step. When combined with another system, such as binder-jet,more » this could reduce the amount of required post-processing. An invention disclosure was filed on hybrid systems that use MIS to reduce the amount of required post-processing.« less

Phenomenological study of the behavior of some silica formers in a high velocity jet fuel burner

NASA Technical Reports Server (NTRS)

Cawley, J. D.; Handschuh, R. F.

1985-01-01

Samples of four silica formers: single crystal SiC, sintered alpha-SiC, reaction sintered Si3N4 and polycrystalline MoSi2, were subjected to a Mach 1 jet fuel burner for 1 hr, at a sample temperature of 1375 deg C (2500 deg F). Two phenomena were identified which may be deleterious to a gas turbine application of these materials. The glass layer formed on the MoSi2 deformed appreciably under the aerodynamic load. A scale developed on the samples of the other materials which consisted of particular matter from the gas stream entrapped in a SiO2 matrix.

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

NASA Astrophysics Data System (ADS)

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.

Microstructure and Mechanical Properties of Ti-6Al-4V Fabricated by Selective Laser Melting of Powder Produced by Granulation-Sintering-Deoxygenation Method

NASA Astrophysics Data System (ADS)

Sun, Pei; Fang, Z. Zak; Zhang, Ying; Xia, Yang

2017-12-01

Commercial spherical Ti powders for additive manufacturing applications are produced today by melt-atomization methods at relatively high costs. A meltless production method, called granulation-sintering-deoxygenation (GSD), was developed recently to produce spherical Ti alloy powder at a significantly reduced cost. In this new process, fine hydrogenated Ti particles are agglomerated to form spherical granules, which are then sintered to dense spherical particles. After sintering, the solid fully dense spherical Ti alloy particles are deoxygenated using novel low-temperature deoxygenation processes with either Mg or Ca. This technical communication presents results of 3D printing using GSD powder and the selective laser melting (SLM) technique. The results showed that tensile properties of parts fabricated from spherical GSD Ti-6Al-4V powder by SLM are comparable with typical mill-annealed Ti-6Al-4V. The characteristics of 3D printed Ti-6Al-4V from GSD powder are also compared with that of commercial materials.

Intrinsic and extrinsic relaxation of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramics: Effect of sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, J. Y.; Zhao, X. T.; Li, S. T.

2010-11-15

The effect of sintering process on the electrical properties of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) ceramic dielectrics were investigated in this paper. It was found that grain size is affected by sintering and the nonlinear current-voltage (I-V) property will decrease with the increased sintering time. Also, the frequency and temperature dependences of dielectric permittivity and loss in the ranges of 10{sup -1}-10{sup 7} Hz and 130-270 K were studied. Two relaxation processes with activation energy of 0.51 eV and 0.10 eV, respectively, were found in the frequency dependence of tan {delta} and Cole-Cole planes, which can be interpreted in termsmore » of insulating grain boundaries and semiconducting grains. It was suggested that grain boundary Maxwell-Wagner relaxation and ionization of oxygen vacancy V{sub O}{sup ++}, proposed as extrinsic and intrinsic relaxations, are responsible for the dielectric behaviors of CCTO ceramics.« less

Copper-polydopamine composite derived from bioinspired polymer coating

DOE PAGES

Zhao, Yao; Wang, Hsin; Qian, Bosen; ...

2018-04-01

Metal matrix composites with nanocarbon phases, such carbon nanotube (CNT) and graphene, have shown potentials to achieve improved mechanical, thermal, and electrical properties. However, incorporation of these nanocarbons into the metal matrix usually involves complicated processes. Here, this study explored a new processing method to fabricate copper (Cu) matrix composite by coating Cu powder particles with nanometer-thick polydopamine (PDA) thin films and sintering of the powder compacts. For sintering temperatures between 300°C and 750°C, the Cu-PDA composite samples showed higher electrical conductivity and thermal conductivity than the uncoated Cu samples, which is likely related to the higher mass densities ofmore » the composite samples. After being sintered at 950°C, the thermal conductivity of the Cu-PDA sample was approximately 12% higher than the Cu sample, while the electrical conductivity did not show significant difference. On the other hand, Knoop micro-hardness values were comparable between the Cu-PDA and Cu samples sintered at the same temperatures.« less

Improved silicon nitride for advanced heat engines

NASA Technical Reports Server (NTRS)

Yeh, H. C.; Wimmer, J. M.; Huang, H. H.; Rorabaugh, M. E.; Schienle, J.; Styhr, K. H.

1985-01-01

The AiResearch Casting Company baseline silicon nitride (92 percent GTE SN-502 Si sub 3 N sub 4 plus 6 percent Y sub 2 O sub 3 plus 2 percent Al sub 2 O sub 3) was characterized with methods that included chemical analysis, oxygen content determination, electrophoresis, particle size distribution analysis, surface area determination, and analysis of the degree of agglomeration and maximum particle size of elutriated powder. Test bars were injection molded and processed through sintering at 0.68 MPa (100 psi) of nitrogen. The as-sintered test bars were evaluated by X-ray phase analysis, room and elevated temperature modulus of rupture strength, Weibull modulus, stress rupture, strength after oxidation, fracture origins, microstructure, and density from quantities of samples sufficiently large to generate statistically valid results. A series of small test matrices were conducted to study the effects and interactions of processing parameters which included raw materials, binder systems, binder removal cycles, injection molding temperatures, particle size distribution, sintering additives, and sintering cycle parameters.

Low-Cost Manufacturing of Bioresorbable Conductors by Evaporation-Condensation-Mediated Laser Printing and Sintering of Zn Nanoparticles.

PubMed

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.

Adjustment of Part Properties for an Elastomeric Laser Sintering Material

NASA Astrophysics Data System (ADS)

Wegner, A.; Ünlü, T.

2018-03-01

Laser sintering of polymers is gaining more and more importance within the field of small series productions. Polyamide 12 is predominantly used, although a variety of other materials are also available for the laser sintering process. For example, elastomeric, rubberlike materials offer very different part property profiles. Those make the production of flexible parts like, e.g., sealings, flexible tubes or shoe soles possible because they offer high part ductility and low hardness. At the chair for manufacturing technology, a new elastomeric laser sintering material has been developed and then commercialized by a spin-off from university. The aim of the presented study was the analysis of the new material's properties. Proof was found that Shore hardness can be modified by varying the parameter settings. Therefore, the correlation between process parameters, energy input, Shore hardness and other part properties like mechanical properties were analyzed. Based on these results, suitable parameter settings were established which lead to the possibility of producing parts with different Shore hardnesses.

Copper-polydopamine composite derived from bioinspired polymer coating

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Yao; Wang, Hsin; Qian, Bosen

Metal matrix composites with nanocarbon phases, such carbon nanotube (CNT) and graphene, have shown potentials to achieve improved mechanical, thermal, and electrical properties. However, incorporation of these nanocarbons into the metal matrix usually involves complicated processes. Here, this study explored a new processing method to fabricate copper (Cu) matrix composite by coating Cu powder particles with nanometer-thick polydopamine (PDA) thin films and sintering of the powder compacts. For sintering temperatures between 300°C and 750°C, the Cu-PDA composite samples showed higher electrical conductivity and thermal conductivity than the uncoated Cu samples, which is likely related to the higher mass densities ofmore » the composite samples. After being sintered at 950°C, the thermal conductivity of the Cu-PDA sample was approximately 12% higher than the Cu sample, while the electrical conductivity did not show significant difference. On the other hand, Knoop micro-hardness values were comparable between the Cu-PDA and Cu samples sintered at the same temperatures.« less

A new integrated evaluation method of heavy metals pollution control during melting and sintering of MSWI fly ash.

PubMed

Li, Rundong; Li, Yanlong; Yang, Tianhua; Wang, Lei; Wang, Weiyun

2015-05-30

Evaluations of technologies for heavy metal control mainly examine the residual and leaching rates of a single heavy metal, such that developed evaluation method have no coordination or uniqueness and are therefore unsuitable for hazard control effect evaluation. An overall pollution toxicity index (OPTI) was established in this paper, based on the developed index, an integrated evaluation method of heavy metal pollution control was established. Application of this method in the melting and sintering of fly ash revealed the following results: The integrated control efficiency of the melting process was higher in all instances than that of the sintering process. The lowest integrated control efficiency of melting was 56.2%, and the highest integrated control efficiency of sintering was 46.6%. Using the same technology, higher integrated control efficiency conditions were all achieved with lower temperatures and shorter times. This study demonstrated the unification and consistency of this method. Copyright © 2015 Elsevier B.V. All rights reserved.

Magnetic properties of ball-milled SrFe12O19 particles consolidated by Spark-Plasma Sintering

PubMed Central

Stingaciu, Marian; Topole, Martin; McGuiness, Paul; Christensen, Mogens

2015-01-01

The room-temperature magnetic properties of ball-milled strontium hexaferrite particles consolidated by spark-plasma sintering are strongly influenced by the milling time. Scanning electron microscopy revealed the ball-milled SrFe12O19 particles to have sizes varying over several hundred nanometers. X-Ray powder-diffraction studies performed on the ball-milled particles before sintering clearly demonstrate the occurrence of a pronounced amorphization process. During sintering at 950 oC, re-crystallization takes place, even for short sintering times of only 2 minutes and transformation of the amorphous phase into a secondary phase is unavoidable. The concentration of this secondary phase increases with increasing ball-milling time. The remanence and maximum magnetization values at 1T are weakly influenced, while the coercivity drops dramatically from 2340 Oe to 1100 Oe for the consolidated sample containing the largest amount of secondary phase. PMID:26369360

Fabrication and thermoelectric properties of n-type (Sr0.9Gd0.1)TiO3 oxides

NASA Astrophysics Data System (ADS)

Li, Liangliang; Qin, Xiaoying; Liu, Yongfei; Xin, Hongxing; Zhang, Jian; Li, Di; Song, Chunjun; Guo, Guanglei; Dou, Yunchen; Zou, Tianhua

2014-02-01

The n-type oxides (Sr0.9Gd0.1)TiO3 (SGTO) have been successfully prepared via a sol-gel process followed by solid-state sintering. The effects of sintering temperature on the thermoelectric (TE) properties of the SGTO samples have been investigated. The Seebeck coefficient showed no obvious difference, while the electrical conductivity increased with increasing sintering temperature, benefiting from an enhancement of densification. The maximum power factor (PF) value, 20.5μW/K2cm at 370 K in the metallic region, was observed for the sample sintered at 1748 K. As a result, the peak figure of merit (ZT) values for the samples sintered at higher than 1673 K were in the range of 0.28-0.30. All the results indicate that such synthetic method provides a simple and effective way to prepare TE oxides.

Multilayer ceramic oxide solid electrolyte for fuel cells and electrolysis cells and method for fabrication thereof

NASA Technical Reports Server (NTRS)

Schroeder, James E. (Inventor); Anderson, Harlan U. (Inventor)

1990-01-01

An unitary layered ceramic structure is disclosed which comprises co-sintered layers. The co-sintered structure comprises a sintered central layer of yttria stabilized zirconia (YSZ) which is about 8 mole percent yttria and having a density of at least about 95% of theoretical, and sintered outer layers of strontium lanthanum manganite (LSM) having the approximate molecular composition La.sub.0.8 Sr.sub.0.2 MnO.sub.3, having a density from about 50 to about 60% of theoretical, and having interconnected porosity from about 40 to 50% with an interconnected pore diameter from about one micron to about five microns. The sintered central layer is sandwiched by and bonded and sintered to the outer layers and is essentially free of significant amounts of manganese. A process for making the unitary composition-of-matter is also disclosed which involves tape casting a LSM tape and then on top thereof casting a YSZ tape. The process comprises presintering LSM powder at 1250.degree. F., crushing the presintered commercially available LSM powder, forming a slurry with the crushed LSM, a binder and solvent, tape casting the slurry and allowing the slurry to air dry. A mixture of commercially available submicron size particle YSZ powder is milled with a dispersant and solvent to disperse the YSZ particles thereby forming a dispersed YSZ slurry. The YSZ slurry is then tape cast on the dried LSM tape. If desired, a third layer of LSM can be cast on top of the dried YSZ layer. After drying the composite LSM/YSZ and LSM/YSZ/LSM tapes are fired at 1300.degree. C. No migration of manganese into the YSZ layer was observed with scanning electron microscope/edax in the sintered multilayer tape.

Multilayer ceramic oxide solid electrolyte for fuel cells and electrolysis cells

NASA Technical Reports Server (NTRS)

Schroeder, James E. (Inventor); Anderson, Harlan U. (Inventor)

1991-01-01

A unitary layered ceramic structure is disclosed which comprises co-sintered layers. The co-sintered structure comprises a sintered central layer of yttria stabilized zirconia (YSZ) which is about 8 mole percent yttria and having a density of at least about 95% of theoretical, and sintered outer layers of strontium lanthanum manganite (LSM) having the approximate molecular composition La.sub.0.8 Sr.sub.0.2 MnO.sub.3, having a density from about 50 to about 60% of theoretical, and having interconnected porosity from about 40 to 50% with an interconnected pore diameter from about one micron to about five microns. The sintered central layer is sandwiched by and bonded and sintered to the outer layers and is essentially free of significant amounts of manganese. A process for making the unitary composition-of-matter is also disclosed which involves tape casting a LSM tape and then on top thereof casting a YSZ tape. The process comprises presintering LSM powder at 1250.degree. F., crushing the presintered commercially available LSM powder, forming a slurry with the crushed LSM, a binder and solvent, tape casting the slurry and allowing the slurry to air dry. A mixture of commercially available submicron size particle YSZ powder is milled with a dispersant and solvent to disperse the YSZ particles thereby forming a dispersed YSZ slurry. The YSZ slurry is then tape cast on the dried LSM tape. If desired, a third layer of LSM can be cast on top of the dried YSZ layer. After drying the composite LSM/YSZ and LSM/YSZ/LSM tapes are fired at 1300.degree. C. No migration of manganese into the YSZ layer was observed with scanning electron microscope/edax in the sintered multilayer tape.

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

NASA Astrophysics Data System (ADS)

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.

Process Simulation of Cold Pressing and Sintering of Armstrong CP-Ti Powders

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gorti, Sarma B; Sabau, Adrian S; Peter, William H

A computational methodology is presented for the process simulation of cold pressing and sintering of Armstrong CP-Ti powders. Since the powder consolidation is governed by specific pressure-dependent constitutive equations, solution algorithms were developed for the ABAQUS user material subroutine, UMAT, for computing the plastic strain increments based on an implicit integration of the nonlinear yield function, flow rule, and hardening equations. Sintering was simulated using a model based on diffusional creep using the user subroutine CREEP. The initial mesh, stress, and density for the simulation of sintering were obtained from the results of the cold pressing simulation, minimizing the errorsmore » from decoupling the cold pressing and sintering simulations. Numerical simulation results are presented for the cold compaction followed by a sintering step of the Ti powders. The numerical simulation results for the relative density were compared to those measured from experiments before and after sintering, showing that the relative density can be accurately predicted. Notice: This manuscript has been authored by UT-Battelle, LLC, under Contract No. DE-AC05-00OR22725 with the U.S. Department of Energy. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce the published form of this manuscript, or allow others to do so, for United States Government purposes. ACKNOWLEDGEMENTS This research was sponsored by the U.S. DOE, and carried out at ORNL, under Contract DE-AC05-00OR22725 with UT-Battelle, LLC. This research was sponsored by the U.S. DOE, EERE Industrial Technology Program Office under CPS Agreement # 17881.« less

A new in vivo screening model for posterior spinal bone formation: comparison of ten calcium phosphate ceramic material treatments.

PubMed

Wilson, Clayton E; Kruyt, Moyo C; de Bruijn, Joost D; van Blitterswijk, Clemens A; Oner, F Cumhur; Verbout, Abraham J; Dhert, Wouter J A

2006-01-01

This study presents a new screening model for evaluating the influence of multiple conditions on the initial process of bone formation in the posterior lumbar spine of a large animal. This model uses cages designed for placement on the decorticated transverse process of the goat lumbar spine. Five conduction channels per cage, each be defined by a different material treatment, are open to both the underlying bone and overlying soft tissue. The model was validated in ten adult Dutch milk goats, with each animal implanted with two cages containing a total of ten calcium phosphate material treatments according to a randomized complete block design. The ten calcium phosphate ceramic materials were created through a combination of material chemistry (BCP, TCP, HA), sintering temperature (low, medium, high), calcination and surface roughness treatments. To monitor the bone formation over time, fluorochrome markers were administered at 3, 5 and 7 weeks and the animals were sacrificed at 9 weeks after implantation. Bone formation in the conduction channels was investigated by histology and histomorphometry of non-decalcified sections using traditional light and epifluorescent microscopy. According to both observed and measured bone formation parameters, materials were ranked in order of increasing magnitude as follows: low sintering temperature BCP (rough and smooth) approximately medium sintering temperature BCP approximately = TCP > calcined low sintering temperature HA > non-calcined low sintering temperature HA > high sintering temperature BCP (rough and smooth) > high sintering temperature HA (calcined and non-calcined). These results agree closely with those obtained in previous studies of osteoconduction and bioactivity of ceramics thereby validating the screening model presented in this study.

Fabrication of β-tricalcium phosphate composite ceramic sphere-based scaffolds with hierarchical pore structure for bone regeneration.

PubMed

He, Fupo; Qian, Guowen; Ren, Weiwei; Li, Jiyan; Fan, Peirong; Shi, Haishan; Shi, Xuetao; Deng, Xin; Wu, Shanghua; Ye, Jiandong

2017-04-24

Polymer sphere-based scaffolds, which are prepared by bonding the adjacent spheres via sintering the randomly packed spheres, feature uniform pore structure, full three-dimensional (3D) interconnection, and considerable mechanical strength. However, bioceramic sphere-based scaffolds fabricated by this method have never been reported. Due to high melting temperature of bioceramic, only limited diffusion rate can be achieved when sintering the bioceramic spheres, which is far from enough to form robust bonding between spheres. In the present study, for the first time we fabricated 3D interconnected β-tricalcium phosphate ceramic sphere-based (PG/TCP) scaffolds by introducing phosphate-based glass (PG) as sintering additive and placing uniaxial pressure during the sintering process. The sintering mechanism of PG/TCP scaffolds was unveiled. The PG/TCP scaffolds had hierarchical pore structure, which was composed by interconnected macropores (>200 μm) among spheres, pores (20–120 μm) in the interior of spheres, and micropores (1–3 μm) among the grains. During the sintering process, partial PG reacted with β-TCP, forming β-Ca2P2O7; metal ions from PG substituted to Ca2+ sites of β-TCP. The mechanical properties (compressive strength 2.8–10.6 MPa; compressive modulus 190–620 MPa) and porosity (30%–50%) of scaffolds could be tailored by manipulating the sintering temperatures. The introduction of PG accelerated in vitro degradation of scaffolds, and the PG/TCP scaffolds showed good cytocompatibility. This work may offer a new strategy to prepare bioceramic scaffolds with satisfactory physicochemical properties for application in bone regeneration.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oro, Raquel, E-mail: raqueld@chalmers.se; Hryha, Eduard, E-mail: hryha@chalmers.se; Campos, Mónica, E-mail: campos@ing.uc3m.es

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-raymore » 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 boundaries by oxide inclusions • Reducing agents efficient at low temperatures critical for avoiding oxide inclusions.« less

Heat treatment of Na2O-CaO-P2O5-SiO2 bioactive glasses: densification processes and postsintering bioactivity.

PubMed

Sola, A; Bellucci, D; Raucci, M G; Zeppetelli, S; Ambrosio, L; Cannillo, V

2012-02-01

Because of their excellent bioactivity, bioactive glasses are increasingly diffused to produce biomedical devices for bone prostheses, to face the dysfunctions that may be caused by traumatic events, diseases, or even natural aging. However, several processing routes, such as the production of scaffolds or the deposition of coatings, include a thermal treatment to apply or sinter the glass. The exposure to high temperature may induce a devetrification phenomenon, altering the properties and, in particular, the bioactivity of the glass. The present contribution offers an overview of the thermal behavior and properties of two glasses belonging to the Na2O-CaO-P2O5-SiO2 system, to be compared to the standard 45S5 Bioglass(®). The basic goal is to understand the effect of both the original composition and the thermal treatment on the performance of the sintered glasses. The new glasses, the one (BG_Na) with a high content of Na2O, the other (BG_Ca) with a high content of CaO, were fully characterized and sintering tests were performed to define the most interesting firing cycles. The sintered samples, treated at 880°C and 800°C respectively, were investigated from a microstructural point of view and their mechanical properties were compared to those of the bulk (not sintered) glass counterparts. The effect of sintering was especially striking on the BG_Ca material, whose Vickers hardness increased from 598.9 ± 46.7 HV to 1053.4 ± 35.0 HV. The in vitro tests confirmed the ability of the glasses, both in bulk and sintered form, of generating a hydroxyapatite surface layer when immersed in a simulated body fluid. More accurate biological tests performed on the sintered glasses proved the high bioactivity of the CaO-rich composition even after a heat treatment. Copyright © 2011 Wiley Periodicals, Inc.

Method for recovery of actinides from refractory oxides thereof using O.sub. F.sub.2

DOEpatents

Asprey, Larned B.; Eller, Phillip G.

1988-01-01

Method for recovery of actinides from nuclear waste material containing sintered and other oxides thereof using O.sub.2 F.sub.2 to generate the hexafluorides of the actinides present therein. The fluorinating agent, O.sub.2 F.sub.2, has been observed to perform the above-described tasks at sufficiently low temperatures that there is virtually no damage to the containment vessels. Moreover, the resulting actinide hexafluorides are not destroyed by high temperature reactions with the walls of the reaction vessel. Dioxygen difluoride is readily prepared, stored and transferred to the place of reaction.

Method of densifying an article formed of reaction bonded silicon nitride

NASA Technical Reports Server (NTRS)

Mangels, John A. (Inventor)

1982-01-01

A method of densifying an article formed of reaction bonded silicon nitride is disclosed. The reaction bonded silicon nitride article is packed in a packing mixture consisting of silicon nitride powder and a densification aid. The reaction bonded silicon nitride article and packing powder are sujected to a positive, low pressure nitrogen gas treatment while being heated to a treatment temperature and for a treatment time to cause any open porosity originally found in the reaction bonded silicon nitride article to be substantially closed. Thereafter, the reaction bonded silicon nitride article and packing powder are subjected to a positive high pressure nitrogen gas treatment while being heated to a treatment temperature and for a treatment time to cause a sintering of the reaction bonded silicon nitride article whereby the strength of the reaction bonded silicon nitride article is increased.

Characterization of Reaction Sintered Silicon Nitride Radomes

DTIC Science & Technology

1977-10-01

A. Ossin , "A Three Dtraenslonal Stress Analysis on the Effects of a Laser Induced Local Hot Spot on a Silicon Nitride Shell, " Martin Marietta...not stated by Ossin , et al, these boundary conditions are extremes and bracket the realistic case. ** In cases where only a few large flaws limit

40 CFR 63.1542 - Definitions.

Code of Federal Regulations, 2014 CFR

2014-07-01

... materials are introduced into a sinter machine, blast furnace, or dross furnace. Dross furnace means any... which material is prepared for charging to a sinter machine or smelting furnace or other lead processing operation. Operating time means the period of time in hours that an affected source is in operation...

40 CFR 63.1542 - Definitions.

Code of Federal Regulations, 2013 CFR

2013-07-01

... materials are introduced into a sinter machine, blast furnace, or dross furnace. Dross furnace means any... which material is prepared for charging to a sinter machine or smelting furnace or other lead processing operation. Operating time means the period of time in hours that an affected source is in operation...

40 CFR 63.1542 - Definitions.

Code of Federal Regulations, 2012 CFR

2012-07-01

... materials are introduced into a sinter machine, blast furnace, or dross furnace. Dross furnace means any... which material is prepared for charging to a sinter machine or smelting furnace or other lead processing operation. Operating time means the period of time in hours that an affected source is in operation...