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All sources NASA NTRS DOE OSTI

DOE OSTI2016

Mn doping effect on optical and ESR studies of Zn{sub 1-x}Mn{sub x}O compound sintered at different temperatures

Polycrystalline bulk samples of Zn{sub 1-x}Mn{sub x}O with x=0.02, 0.04, 0.05 and sintered at different temperatures (500 °C & 800 °C) were studied to investigate the doping effect on the structural, optical properties and spin dynamics in ZnO system. The crystallite size was seen to decrease with no significant change in other structural parameters. FTIR study showed a small effect on the Zn-O stretching bond and other bonds due to presence of Mn. Calculation from UV-Vis spectra showed increase in the optical band gap in the low temperature sintered samples due to Mn doping. In the PL spectra, the UV emission seen to dominate for the 500 °C sintered sample, for 800 °C sample the visible emission dominate indicating increase in non-radiative emission. ESR signals obtained from the microwave absorption shows ferromagnetic signal for the low temperature sintered sample only with a g value of 2.004 for the 2% Mn doped sample. The number of spin participation for resonance is calculated from the ESR signal, which supports the magnetic behaviour of this particular sample.

36 MATERIALS SCIENCE↗

DOE OSTI2019

On the synchronicity of flash sintering and phase transformation

There is growing evidence that oxides of complex chemistries can be formed in one step by reactive flash sintering of their elemental constituents. We explore the temporal relationship between phase transformation and sintering by combining measurements of sintering with in situ measurements of phase transformation. The experiments are carried out under current rate, where flash is induced by injecting current and increasing it at a constant rate. We show that phase transformation of powders of magnesia and α-alumina into single-phase magnesium aluminate spinel was completed in 45 seconds, whereas sintering to full density required 60 seconds.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Laser Sintering of Printed Anodes for Al-Air Batteries

We report on a 3D printed Al anode for Al-air battery combined with laser sintering method. We verified that laser sintering contributed to effective removal of the organic solvent in the slurry and increased the conductivity of the printed anode. By application of infrared laser sintering, we significantly improved electrical contacts of Al nanoparticles and electrochemical performance of Al-air cells. A Pt/C coated hydrophobic carbon paper was used for air cathode to provide a good electrical contact, an oxygen flow ability, and the water sealing. Gel-style KOH was introduced as the electrolyte and waterways also utilized in the chemical reaction. The laser sintered Al-air battery could provide 239 mAh/g discharge capacity and a 0.95 V operation voltage. Also, a 3D structured anode was fabricated by 3D printing the active material on current collectors to achieve a high mass-loading with active material thickness of 360 μm, 560 μm and 680 μm for 1, 2 and 3 layers 3D printed electrodes. The battery cells provide areal discharge capacities of 1.5 mAh/cm 2 , 2.8mAh/cm 2 , and 3.23 mAh/cm 2 , respectively for 1, 2 and 3 layers-electrodes.

25 ENERGY STORAGE↗

DOE OSTI2017

Peridynamic Theory as a New Paradigm for Multiscale Modeling of Sintering

Sintering is a component fabrication process in which powder is compacted by pressing or some other means and then held at elevated temperature for a period of hours. The powder grains bond with each other, leading to the formation of a solid component with much lower porosity, and therefore higher density and higher strength, than the original powder compact. In this project, we investigated a new way of computationally modeling sintering at the length scale of grains. The model uses a high-fidelity, three-dimensional representation with a few hundred nodes per grain. The numerical model solves the peridynamic equations, in which nonlocal forces allow representation of the attraction, adhesion, and mass diffusion between grains. The deformation of the grains is represented through a viscoelastic material model. The project successfully demonstrated the use of this method to reproduce experimentally observed features of material behavior in sintering, including densification, the evolution of microstructure, and the occurrence of random defects in the sintered solid.

36 MATERIALS SCIENCE↗

DOE OSTI2017

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

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 products like wash-basins. To understand the sintering process, a variety of modeling approaches have been pursued at different scales.

36 MATERIALS SCIENCE↗

NASA NTRS1974

Effect of gravity on liquid phase sintering

The unique conditions offered by the earth orbital environment in material processing involving both solid and liquid phases, such as liquid phase sintering, were studied. An experimental development program involving both test and theoretical work was initiated. Experimental work using material combinations selected such that maximum information about the effect of gravity can be derived has been conducted. Wetting of the solid phase by the liquid during sintering is an important phenomenon in liquid phase sintering, and gravity has influence on both capillary phenomenon and density segregation; hence, material combinations were selected such that these two effects can be suitably studies. The experimental work is meant to form the basis for similar comparative work done under low-g conditions. The part of the model dealing with the capillary phenomenon, as related to liquid phase sintering and the effect of gravity on it, suggest that gravity will have negligible effect on the Bond number and that the cohesive force is dependent on both the amount of liquid phase and the angle of contact.

Mookherji, T.↗

NASA NTRS1975

Sinter of uniform, predictable, blemish-free nickel plaque for large aerospace nickel cadmium cells

A series of nickel slurry compositions were tested. Important slurry parameters were found to be the nature of the binder, a pore former and the method of mixing. A slow roll mixing which is non-turbulent successfully eliminated entrapped air so that bubbles and pockets were avoided in the sinter. A slurry applicator was developed which enabled an equal quantity of slurry to be applied to both sides of the grid. Sintering in a furnace having a graded atmosphere characteristic, ranging from oxidizing to strongly reducing, improved adhesion of porous sinter to grid and resulted in a uniform welding of nickel particles to each other throughout the plaque. Sintering was carried out in a horizontal furnace having three heating zones and 16 heating control circuits. Tests used for plaque evaluation include (1) appearance, (2) grid location and adhesion, (3) mechanical strength, (4) thickness, (5) weight per unit area, (6) void volume per unit area, (7) surface area and (8) electrical resistance. Plaque material was impregnated using Heliotek proprietary processes and 100 AH cells were fabricated.

Seiger, H. N.↗

NASA NTRS1975

The formation of lunar breccias - Sintering and crystallization kinetics

The process of clastic breccia formation by viscous sintering in a stress-free environment is analyzed by treating crystallization and sintering as concurrent, competing processes. The kinetic analysis of crystallization is based on the construction of continuous cooling curves corresponding to the degree of crystallinity observed in the matrix of the breccia. These curves are obtained from corresponding time-temperature-transformation curves, which in turn are constructed from measured values of the crystal growth rate together with calculated values of the nucleation frequency. The kinetic analysis of sintering is based on a modification of the Frenkel (1945) treatment of viscous sintering appropriate for conditions of continuous cooling. The analysis is applied to Lunar Composition 70019 to illustrate the approach. It is shown that it is possible from the kinetic analysis to estimate both the rate at which a given breccia cooled and the minimum temperature at which the matrix particles came in contact. The results obtained for Lunar Composition 70019 seem physically reasonable and suggest that this sample cooled on the surface of the moon in its present form rather than buried in an ejecta blanket from which it was later excavated.

Uhlmann, D. R.↗

NASA NTRS1981

The structures of the sintered plaque in the nickel hydroxide electrode

The various failure mechanisms were identified for the nickel electrode. The nickel sinter is involved in all these failure modes. The first one, chemical attack by carbonate, nitrate or other electrolyte components, involves corrosion of the nickel sinters. The second is the physical mode, which involves swelling of the electrode and physical shifting of the sinter in the electrodes. The third is the mechanical failure mode, and is due to fatigue or to the oxygen pressure that causes deformation or fracture of the sinter.

Vyas, B.↗

NASA NTRS1980

Effect of milling and leaching on the structure of sintered silicon

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.

Yeh, H. C.↗

NASA NTRS1980

Sintered reaction bonded Si3N4 for the AGT 101 turbine rotor

The sintered reaction reaction bonded Si3N4 (SRBSN) process, with Y2O3 as a sintering aid, was selected for the fabrication of the AGT 101 turbine rotor. Experiments to determine the optimum Y2O3 composition of this system are discussed. The room temperature strength of the optimum material (RM-1) exceeds 700 MPa while the 1200 C strength exceeds 550 MPa. The slip casting fabrication technique employed for the AGT 101 simulated rotor is described. Rotors have been cast, nitrided and sintered. Densities exceeding 97% of theoretical (3.26 g/cc) have been obtained. Problems relating to sintering reproducibility, and the overall quality of the simulated rotors have been identified.

Mangels, J. A.↗

NASA NTRS1982

Microstructure and property characterization of sintered Si3N4, SiC, and SiAlON

Commercially-produced, pressureless sintered Si3N4, SiC, and SiAlON were characterized with respect to density, phases present, bend strength, and oxidation resistance. The room-temperature bend strengths of sintered Si3N4, SiC, and SiAlON are comparable. However, the room-temperature strengths are much lower (approximately 40 to 50%) than the room-temperature strength of hot-pressed Si3N4 (NC-132). The strength loss in Si3N4 and SiAlON materials at high temperature was attributed to a viscous grain-boundary phase, retained during cooling from the sintering temperature. The oxidation resistance of sintered alpha-SiC was the best of any materials tested.

Dutta, S.↗

NASA NTRS1983

Sintering, properties and fabrication of Si3N4 + Y2O3 based ceramics

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.

Quackenbush, C. L.↗

NASA NTRS1985

Sintered Lining for Heat-Pipe Evaporator

Hotspots eliminated by lining inner wall. Distribution of heat transfer liquid in heat-pipe evaporator improved by lining inner wall with layer of sintered metal. Sintered layer takes place of layer of screen wick formerly sintered or bonded to wall. Since sintered layer always full of liquid, no hotspot of type that previously arose where former screen wick did not fit properly against wall.

Ernst, D. M.↗

NASA NTRS1984

Fabrication of highly dense SiN4 ceramics without additives by high pressure sintering

Silicon nitride (Si3N4) is one of candidate materials for the engineering ceramics which is used at high temperatures. The mechanical strengths of hot pressed or sintered Si2N4 ceramics containing some amount of additives, however, are deteriorated at elevated temperatures. To improve the high temperature strength of Si3N4 ceramics, an attempt to consolidate Si3N4 without additives was made by high pressure sintering technique. Scanning electron micrographs of fracture surfaces of the sintered bodies showed the bodies had finely grained and fully self-bonded sintered bodies were 310N sq m at room temperature and 174N/sq m at 1200 C.

Takatori, K.↗

NASA NTRS1985

Manufacture of dense sintered bodies containing silicon nitride

Sintered bodies containing 1-32.5 Si oxide and 1.5 wt.% SiC (Si oxide/SiC wt. ratio 3/2) are prepared and kept in a 10-3000 kg/2 sq. cm. N (g) atmosphere at 1500-2300 degrees, while simultaneously maintaining the CO (g) partial pressure around the body lower than the nitrogenation equil. pressure to give a dense sintered body. The prepared dense sintered body has high strength at high temperatures. Thus, SiC 40, oxide 30 and Si3N4 30 wt% were fired to a body which was kept in 1500 kg/sq. cm. N (g) for 20 h at 2000 degrees to give a dense sintered body having high bending strength at high temperatures.

Hirota, K.↗

NASA NTRS1986

On the sintering of silicon carbide

This document deals with the sintering of silicon carbide using pressureless sintering. This technique makes it possible to sinter a primarily covalent material to usable densities up to over 98% thD without having to use a high amount of sinter additives as is the case with other non-oxide ceramic materials. The process takes place rapidly, and it is also possible to produce relatively thick-walled structural parts without major problems. This sheds more light on the true characteristics of silicon carbide in one structural part, since there is no second or nearly no second phase. Heat pressing has improved stability.

Gugel, E.↗

NASA NTRS1989

Strength of hot isostatically pressed and sintered reaction bonded silicon nitrides containing Y2O3

The hot isostatic pressing of reaction bonded Si3N4 containing Y2O3 produced specimens with greater room temperature strengths than those by high pressure nitrogen sintering of the same material. Average room temperature bend strengths for hot isostatically pressed reaction bonded silicon nitride and high pressure nitrogen sintered reaction bonded silicon nitride were 767 and 670 MPa, respectively. Values of 472 and 495 MPa were observed at 1370 C. For specimens of similar but lower Y2O3 content produced from Si3N4 powder using the same high pressure nitrogen sintering conditions, the room temperature strength was 664 MPa and the 1370 C strength was 402 MPa. The greater strengths of the reaction bonded silicon nitride materials in comparison to the sintered silicon nitride powder material are attributed to the combined effect of processing method and higher Y2O3 content.

William A Sanders↗