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NASA NTRS1989

Making MgO/SiO2 Glasses By The Sol-Gel Process

Silicon dioxide glasses containing 15 mole percent magnesium oxide prepared by sol-gel process. Not made by conventional melting because ingredients immiscible liquids. Synthesis of MgO/SiO2 glass starts with mixing of magnesium nitrate hexahydrate with silicon tetraethoxide, both in alcohol. Water added, and transparent gel forms. Subsequent processing converts gel into glass. Besides producing glasses of new composition at lower processing temperatures, sol-gel method leads to improved homogeneity and higher purity.

Bansal, Narottam P.↗

NASA NTRS1981

Ultrapure glass optical waveguide development in microgravity by the sol-gel process

Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process referred to here is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation. The use of gels offers several advantages such as high purity and lower melting times and temperatures. The sol-gel process is studied for utilization in the preparation of multicomponent ultrapure glass batches for subsequent containerless melting of the batches in space to prepare glass blanks for optical waveguides.

Mukherjee, S. P.↗

NASA NTRS1982

Ultrapure glass optical waveguide development in microgravity by the sol-gel process

Containerless melting of glasses in space for the preparation of ultrapure homogeneous glass for optical waveguides is discussed. The homogenization of the glass using conventional raw materials is normally achieved on Earth either by the gravity induced convection currents or by the mechanical stirring of the melt. Because of the absence of gravity induced convection currents, the homogenization of glass using convectional raw materials is difficult in the space environment. Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation.

Source record↗

NASA NTRS1990

Production of continuous mullite fiber via sol-gel processing

The development of a continuous ceramic fiber which could be used in rocket engine and rocket boosters applications was investigated at the Marshall Space Flight Center. Methods of ceramic fiber production such as melt spinning, chemical vapor deposition, and precursor polymeric fiber decomposition are discussed and compared with sol-gel processing. The production of ceramics via the sol-gel method consists of two steps, hydrolysis and polycondensation, to form the preceramic, followed by consolidation into the glass or ceramic structure. The advantages of the sol-gel method include better homogeneity and purity, lower preparation temperature, and the ability to form unique compositions. The disadvantages are the high cost of raw materials, large shrinkage during drying and firing which can lead to cracks, and long processing times. Preparation procedures for aluminosilicate sol-gel and for continuous mullite fibers are described.

Tucker, Dennis S.↗

NASA NTRS1990

Low temperature synthesis of CaO-SiO2 glasses having stable liquid-liquid immiscibility by sol-gel process

Calcium silicate glass compositions lying within the liquid-liquid immiscibility dome of the phase diagram, which could not have been prepared by the conventional melting method, were synthesized by the sol-gel process. Hydrolysis and polycondensation of tetraethyl orthosilicate (TEOS) solutions containing up to 20 mol percent calcium nitrate resulted in the formation of clear and transparent gels. The gel formation time decreased with increase in water:TEOS mole ratio, calcium content, and the reaction temperature. Smaller values of gel times in the presence of calcium nitrate are probably caused by lowering of the ionic charge on the sol particles by the salt present. The gelation activation energy, E(sub gel), was evaluated from temperature dependence of the gel time. Presence of Ca(2+) ions or the water:TEOS mole ratio did not have an appreciable effect on the value of E(sub gel). Presence of glycerol in the solution helped in the formation of crack-free monolithic gel specimens. Chemical and structural changes occurring in the gels, as a function of the heat treatments, have been monitored using DTA, TGA, IR-spectroscopy, x ray diffraction, surface area and pore size distribution measurements.

Bansal, Narottam P.↗

NASA NTRS1992

Low temperature synthesis of CaO-SiO2 glasses having stable liquid-liquid immiscibility by the sol-gel process

Calcium silicate glass compositions lying within the liquid-liquid immiscibility dome of the phase diagram, which could not have been prepared by the conventional melting method, were synthesized by the sol-gel process. Hydrolysis and polycondensation of tetraethyl orthosilicate (TEOS) solutions containing up to 20 mol percent calcium nitrate resulted in the formation of clear and transparent gels. The gel formation time decreased with increase in water: TEOS mole ratio, calcium content, and the reaction temperature. Smaller values of gel times in the presence of calcium nitrate are probably caused by lowering of the ionic charge on the sol particles by the salt present. The gelation activation energy, E(sub gel), was evaluated from temperature dependence of the gel time. Presence of Ca(2+) ions or the water:TEOS mole ratio did not have an appreciable effect on the value of E(sub gel). Presence of glycerol in the solution helped in the formation of crack-free monolithic gel specimens. Chemical and structural changes occurring in the gels, as a function of the heat treatments, have been monitored using DTA, TGA, IR-spectroscopy, X-ray diffraction, surface area and pore size distribution measurements.

Bansal, N. P.↗

NASA NTRS1991

Improving the temperature performance of low-density ceramic heatshields through sol-gel processing

The performance of rigid insulations for use as thermal protection materials on reentry vehicles can be characterized by their resistance to dimensional and morphological change when exposed to an isothermal environment equivalent to that generated in entry. Improvements in these material characteristics for alumina-enhanced thermal barrier insulation by compositional modification through sol-gel processing are reported.

Bull, Jeffrey↗

NASA NTRS1980

Ultrapure glass optical waveguide development in microgravity by the sol-gel process

The alkali-borosilicate system was selected as the glass system for the preparation of ultrapure low loss glasses suitable for optical communication. The effect of different oxide contents on the absorption loss was critically reviewed. One composition was chosen to develop the gel preparation procedure in the alkali-borosilicate system. In addition, several procedures for the preparation of gels based on two different approaches were developed. The influence of different preparation parameters were investigated qualitatively. Several conclusions are drawn from the results.

Mukherjee, S. P.↗

NASA NTRS1983

Ultrapure glass optical waveguide: Development in microgravity by the sol gel process

The sol-gel process for the preparation of homogeneous gels in three binary oxide systems was investigated. The glass forming ability of certain compositions in the selected oxide systems (SiO-GeO2, GeO2-PbO, and SiO2-TiO2) were studied based on their potential importance in the design of optical waveguide at longer wavelengths.

Mukherjee, S. P.↗

NASA NTRS1993

New materials: Fountainhead for new technologies and new science

The role of materials as the benchmark technologies which give epochs of human history their names continues into the present. The discovery of new materials has nearly always been the source of new materials science, and frequently of new technologies. This paper analyzes the actual processes by which new materials are synthesized, i.e. whether driven by serendipitous observations, new knowledge is pulled by the market, or integrated into a technological thrust. This analysis focuses on modern ceramic materials discoveries, since World War 2 and uses 45 years experience in materials synthesis in the author's own laboratory as case studies. A dozen different families of materials or processes are involved: hydrothermal reactions; sol-gel processing; clays and zeolites; electroceramics; zero expansion ceramics; diamond films; and radioactive waste host phases. Nanocomposite concepts introduced by the author a decade ago offer an entire, large, new class of materials which will dominate synthesis for the next period. The future of materials research for the next 25 years cannot be extrapolated from the past 25 years. We are near the asymptote for materials utilization in most metals. Likewise we are approaching saturation in improvement of many useful properties. Justifying much further 'basic' R/D for incremental improvement in civilian-oriented industries will not be easy. In materials synthesis, the near-term future is sure to emphasize not new phases, but tailored micro- and nanocomposites for chemical, electrical, optical, and magnetic uses. Unexpected new discoveries such as the Lanxide process may offer rarer chances for step function advances. The new structure of knowledge management will rely less on local research than on integration of worldwide inputs. Better scientific and technological opportunities will lie in designing knowledge intensive materials to meet the new environmental and conservation goals, and the human needs of the very large numbers at the bottom of the socio-economic structures of the world.

Rustum, Roy↗

NASA NTRS1990

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.↗

NASA NTRS1987

Zirconia toughened SiC whisker reinforced alumina composites small business innovation research

The objective of this phase 1 project was to develop a ceramic composite with superior fracture toughness and high strength, based on combining two toughness inducing materials: zirconia for transformation toughening and SiC whiskers for reinforcement, in a controlled microstructure alumina matrix. The controlled matrix microstructure is obtained by controlling the nucleation frequency of the alumina gel with seeds (submicron alpha-alumina). The results demonstrate the technical feasibility of producing superior binary composites (Al2O3-ZrO2) and tertiary composites (Al2O3-ZrO2-SiC). Thirty-two composites were prepared, consolidated, and fracture toughness tested. Statistical analysis of the results showed that: (1) the SiC type is the key statistically significant factor for increased toughness; (2) sol-gel processing with a-alumina seed had a statistically significant effect on increasing toughness of the binary and tertiary composites compared to the corresponding mixed powder processing; and (3) ZrO2 content within the range investigated had a minor effect. Binary composites with an average critical fracture toughness of 6.6MPam sup 1/2, were obtained. Tertiary composites with critical fracture toughness in the range of 9.3 to 10.1 MPam sup 1/2 were obtained. Results indicate that these composites are superior to zirconia toughened alumina and SiC whisker reinforced alumina ceramic composites produced by conventional techniques with similar composition from published data.

Loutfy, R. O.↗

NASA NTRS1992

Sol-Gel Synthesis Of Aluminoborosilicate Powders

Application of sol-gel process to synthesis of aluminoborosilicate powders shows potential for control of microstructures of materials. Development of materials having enhanced processing characteristics prove advantageous in extending high-temperature endurance of fibrous refractory composite insulation made from ceramic fibers.

Bull, Jeffrey↗

NASA NTRS1992

Mechanical properties of coated titanium Beta-21S after exposure to air at 700 and 800 C

Mechanical properties of Beta-21S (Ti-15Mo-3Al-2.7Nb-0.2Si, wt percent) with glass, aluminide, and glass-on-aluminide coatings less than 3-micron thick were studied. Coatings were deposited by sol-gel processing or electron-beam evaporation onto 4.5-mil (113-micron) thick Beta-21S sheet from which, after oxidizing in air at 700 or 800 C, tensile test specimens were machined. Plastic elongation was the most severely degraded of the tensile properties; the glass-on-aluminide coatings were the most effective in preventing degradation. It was found that oxygen trapping by forming oxides in the coating, and reactions between the coatings and the Beta-21S alloy played significant roles.

Wiedemann, Karl E.↗

NASA NTRS1992

Sol-gel synthesis and densification of aluminoborosilicate powders. Part 1: Synthesis

Aluminoborosilicate powders high in alumina content were synthesized by the sol-gel process utilizing various methods of preparation. Properties and microstructural effects related to these syntheses were examined. After heating to 600 C for 2 h in flowing air, the powders were amorphous with the metal oxides comprising 87 percent of the weight and uncombusted organics the remainder. DTA of dried powders revealed a T(sub g) at approximately 835 C and an exotherm near 900 C due to crystallization. Powders derived from aluminum secbutoxide consisted of particles with a mean diameter 5 microns less than those from aluminum isopropoxide. Powders synthesized with aluminum isopropoxide produced agglomerates comprised of rod shaped particulates while powders made with the secbutoxide precursor produced irregular glassy shards. Compacts formed from these powders required different loadings for equivalent densities according to the method of synthesis.

Bull, Jeffrey↗

NASA NTRS1992

Sol-gel synthesis and densification of aluminoborosilicate powders. Part 2: Densification

Aluminoborosilicate (ABS) powders, high in alumina content, were synthesized by the sol-gel process utilizing four different methods of synthesis. The effect of these methods on the densification behavior of ABS powder compacts was studied. Five regions of shrinkage in the temperature range 25-1184 C were identified. In these regions, the greatest shrinkage occurred between the gel-to-glass transition temperature (T sub g approximately equal to 835 C) and the crystallization transformation temperature (T sub t approximately equal 900 C). The dominant mechanism of densification in this range was found to be viscous sintering. ABS powders were amorphous to x-rays up to T sub t at which a multiphasic structure crystallized. No 2Al2O3.B2O3 was found in these powders as predicted in the phase diagram. Above T sub t, densification was the result of competing mechanisms including grain growth and boria fluxed viscous sintering. Apparent activation energies for densification in each region varied according to the method of synthesis.

Bull, Jeffrey↗

NASA NTRS1991

Thin film processing of photorefractive BaTiO3

The principle objectives of this ongoing research involve the preparation and characterization of polycrystalline single-domain thin films of BaTiO3 for photorefractive applications. These films must be continuous, free of cracks, and of high optical quality. The two methods proposed are sputtering and sol-gel related processing.

Schuster, Paul R.↗

NASA NTRS1989

Conceptual design study of a 5 kilowatt solar dynamic Brayton power system using a dome Fresnel lens solar concentrator

The primary project objective was to generate a conceptual design for a nominal 5 kW solar dynamic space power system, which uses a unique, patented, transmittance-optimized, dome-shaped, point-focus Fresnel lens as the optical concentrator. Compared to reflective concentrators, the dome lens allows 200 times larger slope errors for the same image displacement. Additionally, the dome lens allows the energy receiver, the power conversion unit (PCU), and the heat rejection radiator to be independently optimized in configuration and orientation, since none of these elements causes any aperture blockage. Based on optical and thermal trade studies, a 6.6 m diameter lens with a focal length of 7.2 m was selected. This lens should provide 87 percent net optical efficienty at 800X geometric concentration ratio. The large lens is comprised of 24 gores, which compactly stow together during launch, and automatically deploy on orbit. The total mass of the microglass lens panels, the graphite/epoxy support structure, and miscellaneous hardware is about 1.2 kg per square meter of aperture. The key problem for the dome lens approach relates to the selection of a space-durable lens material. For the first time, all-glass Fresnel lens samples were successfully made by a sol-gel casting process.

Oneill, Mark J.↗