Search NASA⌕ Search

SEARCH · Search NASA

Results for “sol-gel reaction”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 19 records
All sourcesNASA NTRSDOE OSTI
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 NTRS2016

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↗
NASA NTRS2002

Metal-silica sol-gel materials

The present invention relates to a single phase metal-silica sol-gel glass formed by the co-condensation of a transition metal with silicon atoms where the metal atoms are uniformly distributed within the sol-gel glass as individual metal centers. Any transition metal may be used in the sol-gel glasses. The present invention also relates to sensor materials where the sensor material is formed using the single phase metal-silica sol-gel glasses. The sensor materials may be in the form of a thin film or may be attached to an optical fiber. The present invention also relates to a method of sensing chemicals using the chemical sensors by monitoring the chromatic change of the metal-silica sol-gel glass when the chemical binds to the sensor. The present invention also relates to oxidation catalysts where a metal-silica sol-gel glass catalyzes the reaction. The present invention also relates to a method of performing oxidation reactions using the metal-silica sol-gel glasses. The present invention also relates to organopolymer metal-silica sol-gel composites where the pores of the metal-silica sol-gel glasses are filled with an organic polymer polymerized by the sol-gel glass.

Stiegman, Albert E.↗
NASA NTRS2003

Material for surface-enhanced Raman spectroscopy, and SER sensors and method for preparing same

Metal-doped sol-gel materials, suitable for use as sensors for surface-enhanced Raman spectroscopic analysis for trace chemical detection, are produced by effecting gelation and solvent removal of a doped sol-gel under mild temperature conditions. At least in certain instances reaction and drying will desirably be effected in an oxygen-starved environment. The metal of the sol-gel material functions, when irradiated, to produce a plasmon field for interaction with molecules of an analyte in contact therewith, increasing by orders of magnitude Raman photons that are generate by excitation radiation, and the method allows matching of the metal and metal particle size to a wavelength of light (or incident radiation, e.g., laser radiation) to generate surface plasmons. The porosity of the sol-gel material dramatically increases the surface area, and thereby the amount of metal exposed for analyte interaction. The sensors provided may be in the form of glass vials, fiber optics, multi-well micro-sample plates, etc., having surface coatings of the doped sol-gel material, to provide sampling systems for use in a Raman instrument.

Farquharson, Stuart↗
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 NTRS2004

Synthesis and Characterization of Ru(II) Tris(1,1O-phenanthroline)-Electron Acceptor Dyads Incorporating the 4-benzoyl-N-methylpyridinium Cation or N-Benzyl-N'-methyl-viologen. Improving the Dynamic Range, Sensitivity and Response Time of Sol-Gel Based Optical Oxygen Sensors

The title compounds (1 and 2, above) were synthesized by Sonogashira coupling reactions of appropriate Ru(1I) complexes with the electron a cceptors. Characterization was conducted in solution and in frozen ma trices. Finally, the title compounds were evaluated as dopants of sol-gel materials. It was found that the intramolecular quenching efficie ncy of 4-benzoyl-Nmethylpyridinium cation in solution depends on the solvent: photoluminescence is quenched completely in CH,CN, but not i n methanol or ethanol. On the other hand, intramolecular emission que nching by 4-benzyl-N-methyl viologen is complete in all solvents. The difference between the two quenchers is traced electrochemically to t he solvation of the 4-benzoyl-Nmethylpyridiniums by alcohol. In froze n matrices or adsorbed on the surfaces of silica aerogel, both Ru(I1) complex/electron acceptor dyads of this study are photoluminescent, and the absence of quenching has been traced to the environmental rigi dity. When doped aerogels are cooled at 77 K, the emission intensity increases by approximately 4x, and the spectra shift to the blue, analogous to what is observed with Ru(I1) complexes in solutions undergoi ng fluid-to-rigid transition. However, in contrast to frozen solution s, the luminescent moieties in the bulk of aerogels kept at low tempe ratures are still accessible to gas-phase quenchers diffusing through the mesopores, leading to more sensitive platforms for sensors than o ther room-temperature configurations. Thus the photoluminescence of o ur Ru(I1) complex dyads adsorbed on aerogel is quenchable by O2 both at room temperature and at 77 K. Furthermore, it was also found that O 2 modulates the photoluminescence of aerogels doped with 4-benzoyl -N -methylpyridinium-based dyads over a wider dynamic range compared wi th aerogels doped with either our vislogen-based dyads or with Ru(I1) tris(1,lO-phenanthroline) itself.

Leventis, Nicholas↗
NASA NTRS1992

Lightweight Protective Coatings For Titanium Alloys

Lightweight coating developed to protect titanium and titanium aluminide alloys and titanium-matrix composite materials from attack by environment when used at high temperatures. Applied by sol-gel methods, and thickness less than 5 micrometers. Reaction-barrier and self-healing diffusion-barrier layers combine to protect titanium alloy against chemical attack by oxygen and nitrogen at high temperatures with very promising results. Can be extended to protection of other environmentally sensitive materials.

Wiedemann, Karl E.↗
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 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 NTRS2004

Preparation of Proton Exchange Membranes and Lithium Batteries from Melamine-containing Ormosils

Our laboratory has recently reported a series of rodcoil polymers for lithium batteries that display dimensionally stable films with good ionic conductivity. The rod segments consist of rigid linear and branched polyimides and the coil segments are polyethylene oxides (PEO). It has been proposed that good mechanical and transport properties are due to phase separation between the rod and coil segments. It was also observed that increased branching and molecular weight lead to increased conductivity. The following study was undertaken to assess the effects of phase separation in polyalkylene oxides connected by melamine linkages. Melamine was chosen as the linking unit because it provides a branching site, cation binding sites to help ionic transport between polymer chains, and the opportunity for self assembly through hydrogen bonding. Polymers were made by the reaction of cyanuric chloride with a series of amine-terminated alkylene oxides. A linear polymer was first made, followed by reaction of the third site on cyanuric chloride with varying ratios of monofunctional Jeffamine and (3-aminopropyl)triethoxysilane. The lithium trifluoromethane sulfonamide-doped polymers are then crosslinked through a sol-gel process to form free-standing films. Initial results have shown mechanically strong films with lithium conductivities on the order of 2 x 10(exp -5) S/cm at ambient temperature. In a separate study, organically modified silanes (Ormosils) that contain sulfonic acid derivatized melamines have been incorporated into proton exchange membranes. The membranes are made by reaction of the primary amine groups of various ratios of melamine derivative and difunctional Jeffamine (MW = 2000) with the epoxide group of (3-Glycidyloxypropyl)trimethoxysilane. The films were then cross-linked through a sol-gel process. Resulting sulfuric acid doped films are strong, flexible, and have proton conductivities on the order of 2 x l0(exp -2) S/cm (120 C, 25% relative humidity). Our best results have been observed when films contain 60% PEO and 40% sulfonated melamine.

Tigelaar, Dean M.↗
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 NTRS1996

Enhancing Adhesion: Relative Merits of Different Approaches

Adhesive performance is improved mainly by manipulation of the bimaterials interface zone, which is only a few molecules thick. There are three approaches to enhancement of interfacial adhesion at the molecular level. They are 1) changing the nonchemically bonded interactions across the interface from weak ones to strong ones, 2) making the true interfacial area much larger than the simple geometric area, and 3) inducing chemical bonding between the two materials forming the interface. Our goal this summer was to question some of the built-in assumptions contained within these approaches and to determine the most promising approach, both theoretically and practically, for enhancing adhesion in NASA structures. Our computations revealed that all three of these approaches have, in theory, the potential to enhance molecular adhesion approximately ten-fold. Experiments, however, revealed that this excellent level of enhancement is not likely to be reached in practice. Each approach was found to be severely limited by practical problems. In addition, some of the built-in assumptions associated with these approaches were found to be insufficient or inadequate. The first approach, changing the nonchemically bonded interactions from weak to strong, Is an example of one containing inadequate assumptions. The extensive literature on intermolecular interactions, based on solution studies, shows that certain functional group pairs interact much more strongly than others. It has always been assumed that these data can be reliably extended to systems where only one member of the pair is in solution and the other Is contained in a solid surface. Our experiments this summer demonstrated that solution data do not adequately predict the strength of functional group interaction at the solid-liquid interface. Furthermore, the strong solvents needed to dissolve the monomers or polymers to which the functional groups of interest are attached compete successfully with the solid surface for the functional group. As a result, functional groups in solution cannot pair with the complementary groups in the solid surface, and the expected enhancement of nonchemically bonded interactions is not realized. The second approach, increasing the true interfacial area, is an example of one containing inadequate assumptions and suffering from numerous practical problems. First, practitioners have assumed that material removal, such as bead blasting or etching, increases true surface area (and therefore interfacial area) in a meaningful way. Our geometric analysis demonstrated that removal methods increase area by a factor of two at most. To increase interfacial area by an order of magnitude or more. a thin layer of high porosity must be added to the substrate surface prior to application of the adhesive phase. Consistent with this finding, we attempted to create a thin layer of rigid, highly porous glass on the surface of our smooth glass substrate by means of sol-gel technology. We were unable to surmount a wide variety of practical problems and obtained only collapsed, nonporous layers. Thus this approach, appealing in principle, would require long term development and is not promising in the near term. The third approach, inducing chemical bonding at the interface, is an example of one having neither inadequate assumptions nor insurmountable practical problems. When silicate glass is the substrate, there are only a few chemical reactions that can be successfully conducted to create these chemical bonds, and these reactions usually involve silicon-containing reagents. We compared the silazane reagents to the silane reagents and found through experiment that the silazanes react with the glass surface much more readily, and under milder conditions, than the silanes. The functional groups attached to the glass surface by silazane reactions were not able to be removed by solvent extraction, elevated temperature exposure, or mechanical action. This clearly indicates that the formation of chemical bonds at the interface is the most effective approach for enhancing molecular adhesion.

Penn, L. S.↗
NASA NTRS2005

X-Aerogels for Structural Components and High Temperature Applications

Future NASA missions and space explorations rely on the use of materials that are strong ultra lightweight and able to withstand extreme temperatures. Aerogels are low density (0.01-0.5 g/cu cm) high porosity materials that contain a glass like structure formed through standard sol-gel chemistry. As a result of these structural properties, aerogels are excellent thermal insulators and are able to withstand temperatures in excess of l,000 C. The open structure of aerogels, however, renders these materials extremely fragile (fracturing at stress forces less than 0.5 N/sq cm). The goal of NASA Glenn Research Center is to increase the strength of these materials by templating polymers and metals onto the surface of an aerogel network facilitating the use of this material for practical applications such as structural components of space vehicles used in exploration. The work this past year focused on two areas; (1) the research and development of new templated aerogels materials and (2) process development for future manufacturing of structural components. Research and development occurred on the production and characterization of new templating materials onto the standard silica aerogel. Materials examined included polymers such as polyimides, fluorinated isocyanates and epoxies, and, metals such as silver, gold and platinum. The final properties indicated that the density of the material formed using an isocyanate is around 0.50 g/cc with a strength greater than that of steel and has low thermal conductivity. The process used to construct these materials is extremely time consuming and labor intensive. One aspect of the project involved investigating the feasibility of shortening the process time by preparing the aerogels in the templating solvent. Traditionally the polymerization used THF as the solvent and after several washes to remove any residual monomers and water, the solvent around the aerogels was changed to acetonitrile for the templating step. This process took a couple of days. It was experimentally determined that the polymerization reaction could be done in acetonitrile instead of THF with no detrimental effects to the properties of the resulting aerogel. Other changes in the time needed to crosslink the gels in the isocyanate solution as well as changes to the subsequent washing procedure could also shorten the processing time with no effect on the properties. Processing methods were also developed that allowed a variety of shapes as well as sizes of these materials to be formed.

Source record↗
NASA NTRS1987

Sol-Gel synthesis of MgO-SiO2 glass compositions having stable liquid-liquid immiscibility

MgO-SiO2 glasses containing up to 15 mol % MgO, which could not have been prepared by the conventional glass melting method due to the presence of stable liquid-liquid immiscibility, were synthesized by the sol-gel technique. Clear and transparent gels were obtained from the hydrolysis and polycondensation of silicon tetraethoxide (TEOS) and magnesium nitrate hexahydrate when the water/TEOS mole ratio was four or more. The gelling time decreased with increase in magnesium content, water/TEOS ratio, and reaction temperature. Magnesium nitrate hexahydrate crystallized out of the gels containing 15 and 20 mol % MgO on slow drying. This problem was partially alleviated by drying the gels quickly at higher temperatures. Monolithic gel samples were prepared using glycerol as the drying control additive. The gels were subjected to various thermal treatments and characterized by several methods. No organic groups could be detected in the glasses after heat treatments to approx. 800 C, but trace amounts of hydroxyl groups were still present. No crystalline phase was found from X-ray diffraction in the gel samples to approx. 890 C. At higher temperatures, alpha quartz precipitated out as the crystalline phase in gels containing up to 10 mol % MgO. The overall activation energy for gel formation in 10MgO-90SiO2 (mol %) system for water/TEOS mole ratio of 7.5 was calculated to be 58.7 kJ/mol.

Bansal, Narottam P.↗
NASA NTRS1988

Sol-gel synthesis of magnesium oxide-silicon dioxide glass compositions

MgO-SiO2 glasses containing up to 15 mol pct MgO, which could not have been prepared by the conventional glass melting method due to the presence of stable liquid-liquid immiscibility, were synthesized by the sol-gel technique. Clear and transparent gels were obtained from the hydrolysis and polycondensation of silicon tetraethoxide (TEOS) and magnesium nitrate hexahydrate when the water/TEOS mole ratio was four or more. The gelling time decreased with increase in magnesium content, water/TEOS ratio, and reaction temperature. Magnesium nitrate hexahydrate crystallized out of the gels containing 15 and 20 mol pct MgO on slow drying. This problem was partially alleviated by drying the gels quickly at higher temperatures. Monolithic gel samples were prepared using glycerol as the drying control additive. The gels were subjected to various thermal treatments and characterized by several methods. No organic groups could be detected in the glasses after heat treatments to approx. 800 C, but trace amounts of hydroxyl groups were still present. No crystalline phase was found from X-ray diffraction in the gel samples to approx. 890 C. At higher temperatures, alpha quartz precipitated out as the crystalline phase in gels containing up to 10 mol pct MgO. The overall activation energy for gel formation in 10MgO-90SiO2 (mol pct) system for water/TEOS mole ratio of 7.5 was calculated to be 58.7 kJ/mol.

Bansal, Narottam P.↗
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 NTRS1999

Effects of Microgravity on the Formation of Aerogels

This paper describes research to investigate fundamental aspects of the effects of microgravity on the formation of the microstructure of metal oxide alcogels and aerogels. We are studying the role of gravity on pore structure and gel uniformity in collaboration with Marshall Space Flight Center (MSFC) on gelling systems under microgravity conditions. While this project was just initiated in May 1998, related research performed earlier is described along with the plans and rationale for the current microgravity investigation to provide background and describe newly developing techniques that should be useful for the current gellation studies. The role of gravity in materials processing must be investigated through the study of well-mastered systems. Sol-gel processed materials are near-perfect candidates to determine the effect of gravity on the formation and growth of random clusters from hierarchies of aggregated units. The processes of hydrolysis, condensation, aggregation and gellation in the formation of alcogels are affected by gravity and therefore provide a rich system to study under microgravity conditions. Supercritical drying of the otherwise unstable wet alcogel preserves the alcogel structure produced during sol-gel processing as aerogel. Supercritically dried aerogel provides for the study of material microstructures without interference from the effects of surface tension, evaporation, and solvent flow. Aerogels are microstructured, low density open-pore solids. They have many unusual properties including: transparency, excellent thermal resistance, high surface area, very low refractive index, a dielectric constant approaching that of air, and extremely low sound velocity. Aerogels are synthesized using sol-gel processing followed by supercritical solvent extraction that leaves the original gel structure virtually intact. These studies will elucidate the effects of microgravity on the homogeneity of the microstructure and porosity of aerogel. The presence of poorly controlled microporosity in aerogel leads to material non-uniformity that gives rise to increased light scattering. Investigation of the effect of gravity driven solute flows within microclusters and their effect on condensation and agglomeration reactions will enable us to improve the preparation and properties of aerogel. Increased clarity of images viewed through aerogel and decreased scattering from the pores of aerogel will significantly improve the prospects for large-scale adoption of aerogel in such applications as transparent insulating windows, high performance thermal insulation, and Cherenkov detectors.

Hunt, A. J.↗