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NASA NTRS1982

Laser processing

Progress in the Progress ceramic materials is reported. Experiments and models for sintering and microstructure evolution are described. Models and data for understanding the kinetics of grain boundary motion and of pore coarsening and new materials for fuel cells and batteries; are developed. New experimental techniques using lasers for forming fine, monosized powders and for forming stable and metastable structures from liquids, and solar materials research are also developed. Colloidal science and ceramics processing are explored; and research programs on the presintering science necessary for controlled green microstructures are outlined.

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NASA NTRS1986

Structure and grain coarsening during the sintering of alumina

The pore surface area (Sp) and grain-boundary area (Sgb) were measured during the sintering of undoped and doped (100 ppm MgO) alumina compacts. Since the presence of the additive affects only Sgb (raising it at a given value of the density), pinning of the boundaries by solid-solution drag is the only additive function evidenced by the results. The importance of such pinning even at densities as low as 75 percent of theoretical is linked to the existence of microstructural inhomogeneities.

Shaw, N. J.↗

NASA NTRS2000

Electrophoretic Porosimetry of Sol-Gels

It has been hypothesized that gravity has an effect on the formation and resulting microstructure of sol-gels. In order to more clearly resolve the effect of gravity, pores may be non-destructively analyzed in the wet gel, circumventing the shrinkage and coarsening associated with the drying procedure. We discuss the development of an electrophoretic technique, analogous to affinity chromatography, for the determination of pore size distribution and its application to silica gels. Specifically a monodisperse charged dye is monitored by an optical densitometer as it moves through the wet gel under the influence of an electric field. The transmittance data (output) represents the convolution of the dye concentration profile at the beginning of the run (input) with the pore size distribution (transfer function), i.e. linear systems theory applies. Because of the practical difficulty in producing a delta function input dye profile we prefer instead to use a step function. Average pore size is then related to the velocity of this dye front, while the pore size distribution is related to the spreading of the front. Preliminary results of this electrophoretic porosimetry and its application to ground and space-grown samples will be discussed.

Snow, L. A.↗

NASA NTRS2001

High-Pressure Synthesis of Metal-Ceramic Nano-Composites

The major problems in fabrication of nano-crystal line materials form nano-powders are: (1), coarsening of the initial nano-size grains, (2), insufficient densification (high concentration of pores), and, (3), conversion of diamond into graphite (for diamond-based ceramics). We have developed a novel technique of the synthesis of nano-composite materials applying very high (up to about 10 GPa) pressures. In this technique, one component is pre-compacted and placed next to another having a lower melting point temperature. The whole sample is pressed and the temperature raised above the melting point of the second component, what results in the melt getting pressed into the (nano-size) pores of the compact. Upon subsequent crystallization the melt forms the second nanophase. The process is fast, on the order of seconds, and the temperatures are relatively low what prevents, or at least significantly reduces coarsening of the starting nanophase grains. Also, conversion of diamond into graphite can be prevented. The technique allows for control of the final product properties through a proper selection of (1) the initial compact density and grain size, (2) chemical composition of the source, and (3) the temperature and pressure of the process. The application of the technique to the synthesis of SiC and diamond with Si, Ge, and different metals. Results of the in-situ investigation of the synthesis process by synchrotron X-ray diffraction technique will be presented.

Gierlotka, S.↗

NASA NTRS1987

Structure and grain coarsening during the processing of engineering ceramics

Studies have been made of three ceramic systems (Al2O3, Y2O3/MgO, and SiC/C/B), both to explore a surface area/density diagram approach to examining the coarsening processes during sintering and to explore an alternative coarsening parameter, i.e., the grain boundary surface area (raising it at a given value of the density) and not the pore surface area; therefore, pinning of the grain boundaries by solid-solution drag is the only function evidenced by these results. The importance of such pinning even at densities as low as 75% of theoretical is linked to the existence of microstructural inhomogeneities. The early stages of sintering of Y2O3 powder have been examined using two techniques, BET surface area analysis and transmission electron microscopy. Each has given some insight into the process occurring and, used together, have provided some indication of the effect of MgO on coarsening during sintering. Attempts to further elucidate effects of MgO on the coarsening behavior of Y2O3 by the surface area/density diagram approach were unsuccessful due to masking effects of contaminating reactions during sintering and/or thermal etching. The behavior of the undoped SiC which only coarsens can be clearly distinguished by the surface area/density diagram from that of SiC/C/B which also concurrently densifies. Little additional information was obtainable by this method due to unfavorable sample etching characteristics. The advantages, disadvantages, and difficulties of application of these techniques to the study of coarsening during sintering are discussed.

Shaw, Nancy J.↗