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At least 235 records · Page 13

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

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.

Yajima, S.↗

Improved performance of silicon nitride-based high temperature ceramics

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.

Ashbrook, R. L.↗

Thermal Conductivity and Stability of HfO2-Y2O3 and La2Zr2O7 Evaluated for 1650 Deg C Thermal/Environmental Barrier Coating Applications

HfO2-Y2O3 and La2Zr2O7 are candidate thermal and environmental barrier coating (T/EBC) materials for gas turbine ceramic matrix composite (CMC) combustor applications because of their relatively low thermal conductivity and high temperature capability. In this paper, thermal conductivity and high temperature stability of hot-pressed and plasma sprayed specimens with representative partially-stabilized and fully-cubic HfO2-Y2O3 compositions and La2Zr2O7 were evaluated at temperatures up to 1700 C using a steady-state laser heat-flux technique. Sintering behavior of the plasmasprayed coatings was determined by monitoring the thermal conductivity increases during a 20-hour test period at various temperatures. Durability and failure mechanisms of the HfO2-Y2O3 and La2Zr2O7 coatings on mullite/SiC hexoloy or SiC/SiC CMC substrates were investigated at 1650 C under thermal gradient cyclic conditions. Coating design and testing issues for the 1650 C thermal/environmental barrier coating applications are also discussed.

Zhu, Dong-Ming↗

Homogeneity Study of ZrC, NbC, and TaC Binary Carbide Fuels for the Application of Nuclear Thermal Propulsion

In alignment with NASA and DARPA goals, efforts towards Nuclear Thermal Propulsion (NTP) have increased in recent years. As progress is made, a main challenge still exists; the fuel in an NTP system must survive the extreme environment experienced during operating conditions. Three fuel forms have been studied including a ceramic-metallic matrix, a ceramic-ceramic matrix, and solid solution carbides. Solid solution carbides were studied previously as a fuel for NTP and was shown to be a promising technology; however, the programs were canceled before demonstration in an NTP engine test. Of the refractory metal carbides of interest, zirconium carbide (ZrC), niobium carbide (NbC) and tantalum carbide (TaC) were studied. ZrC, NbC, and TaC powders were consolidated in monocarbide (ZrC, NbC, TaC) and bi-carbide (ZrC-NbC, ZrC-TaC, NbC-TaC) forms using spark plasma sintering (SPS), with 50-50 mol% compositions of the bi-carbides of interest. The time and temperature conditions to achieve a completely homogeneous solid solution for the mixed carbides is of interest for NTP fuel applications, since this homogeneity is considered to be essential for this fuel form. Homogeneity is typically not achieved during sintering, as surface diffusion (predominant for sintering to near ideal density) tends to occur at lower temperatures than bulk volumetric diffusion (required for solute interdiffusion to achieve a homogeneous solid solution). High temperature isochronal annealing was performed to identify the conditions to achieve a chemically homogeneous sample. The solute interpenetration vs annealing temperature was quantified using energy dispersion spectroscopy (EDS) in a scanning electron microscope (SEM). X-ray diffraction (XRD) was used to accurately measure the phase stability and lattice parameter as a function of annealing conditions. The diffusion data from each sample was then used to determine self-diffusion coefficients for interdiffusion of the Nb, Zr, and Ta solutes and compared to existing literature values. The minimum annealing conditions to achieve complete chemical homogeneity for each carbide was determined.

nuclear thermal propulsion↗

Screenable all-metal solar cell electrodes of nickel and copper

Screenable thick film solar cell electrodes are made using the all-metal electrode system, which eliminates the commonly used glass frit and substitutes an oxide scavenger such as silver fluoride. The low temperature firing copper metal systems give good results on solar cells obtaining cell efficiencies of 13% AM1, and adhering sintered structures are demonstrated with nickel systems. The potential effect of copper upon cell performance at elevated temperatures over long periods of time is determined, and it is found that the formation of a copper-silicon eutectic at 550 C produces needle-like structures with broad bases on the silicon, extending into and occasionally through the metallization layer.

Ross, B.↗

A lime refractory for high temperature use

Lime refractory fabrication and properties for high temperature applications, describing production of calcium oxide grain by sintering process from commercial calcium hydroxide

Benson, J. T.↗

Vacuum-assisted impregnation of materials

Vacuum-assisted liquid-impregnation treatment for silicon-carbide-reinforced carbon-carbon systems improves resistance of silicon-carbide coating to attack by oxygen at elevated temperatures. Porosity reduction treatment might also be applied to sintering silicon-carbide bodies to increase their density and to make them more resistant to hot gases for use in jet engines.

Rogers, D. C.↗

The non-Newtonian heat and mass transport of He 2 in porous media used for vapor-liquid phase separation

This investigation of vapor-liquid phase separation (VLPS) of He 2 is related to long-term storage of cryogenic liquid. The VLPS system utilizes porous plugs in order to generate thermomechanical (thermo-osmotic) force which in turn prevents liquid from flowing out of the cryo-vessel (e.g., Infrared Astronomical Satellite). An apparatus was built and VLPS data were collected for a 2 and a 10 micrometer sintered stainless steel plug and a 5 to 15 micrometer sintered bronze plug. The VLPS data obtained at high temperature were in the nonlinear turbulent regime. At low temperature, the Stokes regime was approached. A turbulent flow model was developed, which provides a phenomenological description of the VLPS data. According to the model, most of the phase separation data are in the turbulent regime. The model is based on concepts of the Gorter-Mellink transport involving the mutual friction known from the zero net mass flow (ZNMF) studies. The latter had to be modified to obtain agreement with the present experimental VLPS evidence. In contrast to the well-known ZNMF mode, the VLPS results require a geometry dependent constant (Gorter-Mellink constant). A theoretical interpretation of the phenomenological equation for the VLPS data obtained, is based on modelling of the dynamics of quantized vortices proposed by Vinen. In extending Vinen's model to the VLPS transport of He 2 in porous media, a correlation between the K*(GM) and K(p) was obtained which permits an interpretation of the present findings. As K(p) is crucial, various methods were introduced to measure the permeability of the porous media at low temperatures. Good agreement was found between the room temperature and the low temperature K(p)-value of the plugs.

Yuan, S. W. K.↗

Sintering, microstructural, radiographic, and strength characterization of a high-purity Si3N4-based composition

A commercially available high purity alpha-Si3N4 powder (UBE SN-E10) was characterized, milled with additives, and sintered in a high-pressure nitrogen atmosphere at temperatures ranging from 1750 to 2140 C. The composition selected for this study has been previously examined using a different alpha-Si3N4 powder. Densification behavior, microstructure characteristics, X-radiographic appearance, room- and high-temperatures flexural strength, and fracture-initiating flaw sites were determined. The high-temperature flexural strengths significantly exceeded those observed in the earlier studies using an identical composition (different alpha-Si3N4 powder) and similar processing techniques.

Kiser, J. D.↗

Advanced Oxide Material Systems for 1650 C Thermal/Environmental Barrier Coating Applications

Advanced thermal and environmental barrier coatings (TEBCs) are being developed for low-emission SiC/SiC ceramic matrix composite (CMC) combustor and vane applications to extend the CMC liner and vane temperature capability to 1650 C (3000 F) in oxidizing and water-vapor-containing combustion environments. The advanced 1650 C TEBC system is required to have a better high-temperature stability, lower thermal conductivity, and more resistance to sintering and thermal stress than current coating systems under engine high-heat-flux and severe thermal cycling conditions. In this report, the thermal conductivity and water vapor stability of selected candidate hafnia-, pyrochlore- and magnetoplumbite-based TEBC materials are evaluated. The effects of dopants on the materials properties are also discussed. The test results have been used to downselect the TEBC materials and help demonstrate the feasibility of advanced 1650 C coatings with long-term thermal cycling durability.

Zhu, Dong-Ming↗

Method of densifying an article formed of reaction bonded silicon nitride

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.

Mangels, John A.↗

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

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.

Moore, C.↗

Fabrication and characterization of Si3N4 ceramics without additives by high pressure hot pressing

High pressure hot-pressing of Si3N4 without additives was performed using various kinds of Si3N4 powder as starting materials, and the relation between densification and alpha-beta phase transformation was studied. The temperature dependences of Vickers microhardness and fracture toughness were also examined. Densification of Si3N4 was divided into three stages, and it was found that densification and phase transformation of Si3N4 under pressure were closely associated. The results of the temperature dependence of Vickers microhardness indicated that the high-temperature hardness was strongly influenced not only by the density and microstructure of sintered body but also by the purity of starting powder. The fracture toughness values of Si3N4 bodies without additives were 3.29-4.39 MN/m to the 3/2 power and independent of temperature up to 1400 C.

Shimada, M.↗

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

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.

Dynys, F.↗

Thermal Conductivity and Water Vapor Stability of Ceramic HfO2-Based Coating Materials

HfO2-Y2O3 and La2Zr2O7 are candidate thermal/environmental barrier coating materials for gas turbine ceramic matrix composite (CMC) combustor liner applications because of their relatively low thermal conductivity and high temperature capability. In this paper, thermal conductivity and high temperature phase stability of plasma-sprayed coatings and/or hot-pressed HfO2-5mol%Y2O3, HfO2-15mol%Y2O3 and La2Zr2O7 were evaluated at temperatures up to 1700 C using a steady-state laser heat-flux technique. Sintering behavior of the plasma-sprayed coatings was determined by monitoring the thermal conductivity increases during a 20-hour test period at various temperatures. Durability and failure mechanisms of the HfO2-Y2O3 and La2Zr2O7 coatings on mullite/SiC Hexoloy or CMC substrates were investigated at 1650 C under thermal gradient cyclic conditions. Coating design and testing issues for the 1650 C thermal/environmental barrier coating applications will also be discussed.

Zhu, Dong-Ming↗

Low Temperature Regolith Bricks for In-Situ Structural Material

Current technology for producing in-situ structural materials on future missions to Mars or the moon relies heavily on energy-intensive sintering processes to produce solid bricks from regolith. This process requires heating the material up to temperatures in excess of 1000 C and results in solid regolith pieces with compressive strengths in the range of 14000 to 28000 psi, but are heavily dependent on the porosity of the final material and are brittle. This method is currently preferred over a low temperature cementation process to prevent consumption of precious water and other non-renewable materials. A high strength structural material with low energy requirements is still needed for future colonization of other planets. To fulfill these requirements, a nano-functionalization process has been developed to produce structural bricks from regolith simulant and shows promising mechanical strength results. Functionalization of granular silicate particles into alkoxides using a simple low temperature chemical process produces a high surface area zeolite particles that are held together via inter-particle oxygen bonding. Addition of water in the resulting zeolite particles produces a sol-gel reaction called "inorganic polymerization" which gives a strong solid material after a curing process at 60 C. The aqueous solution by-product of the reaction is currently being investigated for its reusability; an essential component of any ISRU technology. For this study, two batches of regolith bricks are synthesized from JSC-1A; the first batch from fresh solvents and chemicals, the second batch made from the water solution by-product of the first batch. This is done to determine the feasibility of recycling necessary components of the synthesis process, mainly water. Characterization including BET surface area, SEM, and EDS has been done on the regolith bricks as well as the constituent particles,. The specific surface area of 17.53 sq m/g (average) of the granular regolith material was obtained from nitrogen adsorption isotherm measurement. The size, shape and textures of regolith from SEM shows that the particles are 25-50 micrometers in size and mostly irregular in shape (Figure 1a). The elemental composition of regolith was identified from EDS analysis showed the presence of Si, Al, Fe, Na, Mg, Ca, Ti, O and C (see figure 1b). Each set of cylindrical brick samples were prepared by low energy process, and cured for 21 and 28 days, respectively to compare their compressive strength. Figure 1c, and d shows the JSC-1A brick and the compressive strength measurements. The results from the 21 day cured bricks (2 bricks) have been done and yielded an aver-age strength of 3050 psi, considerably higher than Portland cement mortars (Type IV and V). This promising technology provides the benefits of construction material similar to concrete, with a low complexity, low energy synthesis process and the likelihood of complete reusability of precious resources. Compressive strength using this method can be improved by increasing the surface area of the particles, using bi-modal particle size distribution, and adding certain additives to increase inter-particle forces.

ISRU↗

A very low resistance, non-sintered contact system for use on indium phosphide concentrator/shallow junction solar cells

An investigation is made into the possibility of providing low resistance contacts to shallow junction InP solar cells which do not require sintering and which do not cause device degradation even when subjected to extended annealing at elevated temperatures. We show that the addition of In to Au contacts in amounts that exceed the solid solubility limit lowers the as-fabricated (unsintered) contact resistivity (R sub c) to the 10(exp -5) ohm cm(exp 2) range. We next consider the contact system Au/Au2P3, which has been shown to exhibit as-fabricated R sub c values in the 10(exp -6) ohm cm(exp 2) range, but which fails quickly when heated. We show that the substitution of a refractory metal (W, Ta) for Au preserves the low R sub c values while preventing the destructive reactions that would normally take place in this system at high temperatures. We show, finally, that R sub c values in the 10(exp -7) ohm cm(exp 2) range can be achieved without sintering by combining the effects of In or Ga additions to Au contacts with the effects of introducing a thin Au2P3 layer at the metal-InP interface.

Weizer, Victor G.↗

A very low resistance, non-sintered contact system for use on indium phosphide concentrator/shallow junction solar cells

An investigation is made into the possibility of providing low resistance contacts to shallow junction InP solar cells which do not require sintering and which do not cause device degradation even when subjected to extended annealing at elevated temperatures. We show that the addition of In to Au contacts in amounts that exceed the solid solubility limit lowers the as-fabricated (unsintered) contact resistivity (R sub c) to the 10(exp -5) ohm cm(exp 2) range. We next consider the contact system Au/Au2P3 which has been shown to exhibit as-fabricated R sub c values in the 10(exp -6) ohm cm(exp 2) range, but which fails quickly when heated. We show that the substitution of a refractory metal (W, Ta) for Au preserves the low R sub c values while preventing the destructive reactions that would normally take place in this system at high temperatures. We show, finally, that R sub c values in the 10(exp -7) ohm cm(exp 2) range can be achieved without sintering by combining the effects of In or Ga additions to Au contacts with the effects of introducing a thin Au2P3 layer at the metal-InP interface.

Weizer, Victor G.↗