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NASA NTRS2003

Sol-Gel Precursors for Ceramics from Minerals Simulating Soils from the Moon and Mars

Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report some preliminary results on the production of sol-gel precursors for ceramic products using mineral resources available in Martian or Lunar soil. The presence of SiO2, TiO2, and A12O3 in both Martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and Lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from Lunar and Martian simulant soils. Clear sol-gel precursors have been obtained by dissolution of silica from Lunar simulant soil in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Thermogravimetric Analysis and X-ray Photoelectron Spectroscopy were used to characterize the elemental composition and structure of the precursor molecules. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors. In the second set of experiments, we used the same starting materials to synthesize silicate esters in acidified alcohol mixtures. Preliminary results indicate the presence of silicon alkoxides in the product of distillation.

Sibille, Laurent↗

NASA NTRS2003

Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SiO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2,7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil simular in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. The elemental composition and structure of the precursor molecules were characterized. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors.

Sibille, L.↗

NASA NTRS2004

Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil similar JSC-1 in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. Characterization of the precursor molecules and efforts to further concentrate and hydrolyze the products to obtain gel materials will be presented for evaluation as ceramic precursors.

Sibille, L.↗

DOE OSTI2022

Tin sensitization and silver activation on indium tin oxide surfaces

Adhesion of electrical contacts on electronic and optoelectronic devices is important for reliable device operation. Sn-sensitization is a widely used process that improves uniformity and adhesion of plated metals to glass and polymer surfaces. Electrically conductive substrates can significantly benefit from improved uniformity, adhesion, and contact resistance to metallic contact layers. In this study, we investigate the process of Sn-sensitization and Ag-activation on indium tin oxide (ITO) surfaces—a dominant transparent conducting oxide used in optoelectronic devices. Here, our results show that ITO films exposed to Sn-sensitization solutions with HCl concentrations below 10 mM effectively modify the surface termination through the process of Sn-sensitization (Sn-bonding at the surface hydroxide sites) without etching the ITO film. However, the subsequent Ag-activation on an ITO surface does not seem to follow the typical response on a glass substrate, suggesting that Ag-activation of an ITO surface is likely limited by the Ag ion size relative to the area density of surface hydroxide sensitization sites.

42 ENGINEERING↗

DOE OSTI2024

A Hermetic Package Technique for Multi-Functional Fiber Sensors through Pressure Boundary of Energy Systems Based on Glass Sealants

This paper presents a hermitic fiber sensor packaging technique that enables fiber sensors to be embedded in energy systems for performing multi-parameter measurements in high-temperature and strong radiation environments. A high-temperature stable Intrinsic Fabry–Perot interferometer (IFPI) array, inscribed by a femtosecond laser direct writing scheme, is used to measure both temperature and pressure induced strain changes. To address the large disparity in thermo-expansion coefficients (TECs) between silica fibers and metal parts, glass sealants with TEC between silica optical fibers and metals were used to hermetically seal optical fiber sensors inside stainless steel metal tubes. The hermetically sealed package is validated for helium leakages between 1 MPa and 10 MPa using a helium leak detector. An IFPI sensor embedded in glass sealant was used to measure pressure. The paper demonstrates an effective technique to deploy fiber sensors to perform multi-parameter measurements in a wide range of energy systems that utilize high temperatures and strong radiation environments to achieve efficient energy production.

Optics↗

NASA NTRS2005

Processing of Lunar Soil Simulant for Space Exploration Applications

NASA's long-term vision for space exploration includes developing human habitats and conducting scientific investigations on planetary bodies, especially on Moon and Mars. To reduce the level of up-mass processing and utilization of planetary in-situ resources is recognized as an important element of this vision. Within this scope and context, we have undertaken a general effort aimed primarily at extracting and refining metals, developing glass, glass-ceramic, or traditional ceramic type materials using lunar soil simulants. In this paper we will present preliminary results on our effort on carbothermal reduction of oxides for elemental extraction and zone refining for obtaining high purity metals. In additions we will demonstrate the possibility of developing glasses from lunar soil simulant for fixing nuclear waste from potential nuclear power generators on planetary bodies. Compositional analysis, x-ray diffraction patterns and differential thermal analysis of processed samples will be presented.

Sen, Subhayu↗

NASA NTRS2005

Processing of Lunar Soil Simulant for Space Exploration Applications

NASA's long-term vision for space exploration includes developing human habitats and conducting scientific investigations on planetary bodies, especially on Moon and Mars. Processing and utilization of planetary in-situ resources is recognized as an important element of this vision since it can minimize the level of up-mass that will have to be transported from earth to the planetary bodies. Within this scope and context, we have undertaken a general effort aimed primarily at extracting and refining metals, developing glass, glass-ceramic, or traditional ceramic type materials using lunar soil simulants. In this paper we will present preliminary results on our effort on simultaneous carbothermal reduction of oxides for elemental extraction and zone refining for obtaining high purity metals. In additions we will demonstrate the possibility of developing glass fibers as reinforcement agents for planetary habitat construction, glasses for fixing nuclear waste from potential nuclear power generators, and glasses for magnetic applications. The paper will also include initial thermal characterization of the glasses produced from lunar simulant. Compositional analysis of processed samples will be presented.

Sen, Subhayu↗

NASA NTRS1984

Surface tension of ZrF4-BaF2-LaF3 glass

A solidified pendant drop technique is presently used in the measurement of surface tension of a 62 mol pct ZrF4, 33 mol pct BaF2, 5 mol pct LaF3 heavy metal-fluoride glass, in keeping with a requirement from a comparison experiment planned for microgravity conditions aboard the Space Shuttle. The surface tension at 550 C is 0.174 + or - 0.005 J/sq m.

Bansal, N. P.↗

NASA NTRS1991

Thermal shock testing for assuring reliability of glass-sealed microelectronic packages

Tests were performed to determine if thermal shocking is destructive to glass-to-metal seal microelectronic packages and if thermal shock step stressing can compare package reliabilities. Thermal shocking was shown to be not destructive to highly reliable glass seals. Pin-pull tests used to compare the interfacial pin glass strengths showed no differences between thermal shocked and not-thermal shocked headers. A 'critical stress resistance temperature' was not exhibited by the 14 pin Dual In-line Package (DIP) headers evaluated. Headers manufactured in cryogenic nitrogen based and exothermically generated atmospheres showed differences in as-received leak rates, residual oxide depths and pin glass interfacial strengths; these were caused by the different manufacturing methods, in particular, by the chemically etched pins used by one manufacturer. Both header types passed thermal shock tests to temperature differentials of 646 C. The sensitivity of helium leak rate measurements was improved up to 70 percent by baking headers for two hours at 200 C after thermal shocking.

Thomas, Walter B., III↗

NASA NTRS1987

Practical significance and calculation of surface tension of glass, enamels and glazes

Surface tension is important in the formation of streaks in the whole procedure of enameling and glazing., in the action of TiO2 as opacifier, in the addition of borax to enamels, or metals to glasses, and in the corrosion of refractories by molten charges. By the use of known methods for measuring surface tension additive constants are found which give correct results within 1% with no discrepancy due to B2O3.

Dietzel, A.↗

NASA NTRS1973

Structural considerations in design of lightweight glass-fiber composite pressure vessels

The design concepts used for metal-lined glass-fiber composite pressure vessels are described, comparing the structural characteristics of the composite designs with each other and with homogeneous metal pressure vessels. Specific design techniques and available design data are identified. The discussion centers around two distinctly different design concepts, which provide the basis for defining metal lined composite vessels as either (1) thin-metal lined, or (2) glass fiber reinforced (GFR). Both concepts are described and associated development problems are identified and discussed. Relevant fabrication and testing experience from a series of NASA-Lewis Research Center development efforts is presented.

Faddoul, J. R.↗

NASA NTRS2015

Grazing Incidence Optics Technology

This project is to demonstrate the capability to directly fabricate lightweight, high-resolution, grazing-incidence x-ray optics using a commercially available robotic polishing machine. Typical x-ray optics production at NASA Marshall Space Flight Center (MSFC) uses a replication process in which metal mirrors are electroformed on to figured and polished mandrels from which they are later removed. The attraction of this process is that multiple copies can be made from a single master. The drawback is that the replication process limits the angular resolution that can be attained. By directly fabricating each shell, errors inherent in the replication process are removed. The principal challenge now becomes how to support the mirror shell during all aspects of fabrication, including the necessary metrology to converge on the required mirror performance specifications. This program makes use of a Zeeko seven-axis computer-controlled polishing machine (see fig. 1) and supporting fabrication, metrology, and test equipment at MSFC. The overall development plan calls for proof-of-concept demonstration with relatively thick mirror shells (5-6 mm, fig. 2) which are straightforward to support and then a transition to much thinner shells (2-3 mm), which are an order of magnitude thinner than those used for Chandra. Both glass and metal substrates are being investigated. Currently, a thick glass shell is being figured. This has enabled experience to be gained with programming and operating the polishing machine without worrying about shell distortions or breakage. It has also allowed time for more complex support mechanisms for figuring/ polishing and metrology to be designed for the more challenging thinner shells. These are now in fabrication. Figure 1: Zeeko polishing machine.

Ramsey, Brian↗

NASA NTRS1992

Magnetic Susceptibility Measurements for in Situ Characterization of Lunar Soil

Magnetic separation is a viable method for concentration of components of lunar soils and rocks for use as feedstocks for manufacture of metals, oxygen, and for recovery of volatiles such as He-3. Work with lunar materials indicates that immature soils are the best candidates for magnetic beneficiation. The magnetic susceptibility at which selected soil components such as anorthite, ilmenite, or metallic iron are separated is not affected by soil maturity, but the recovery of the concentrated components is. Increasing soil maturity lowers recovery. Mature soils contain significant amounts of glass-encased metallic iron. Magnetic susceptibility, which is sensitive to metallic iron content, can be used to measure soil maturity. The relationship between the ratio of magnetic susceptibility and iron oxide and the conventional maturity parameter, I(sub s)/FeO, ferromagnetic resonant intensity divided by iron oxide content is given. The magnetic susceptibilities were determined using apparatus designed for magnetic separation of the lunar soils.

Oder, R. R.↗

NASA NTRS1966

Mechanism facilitates coating of inner surfaces of metal cylinders

Cylinder is rotated about shielded hot filament to vapor deposit thin coatings of aluminum or other metallic substances on the inner surface of a cylinder while avoiding heat-producing high-density current flow which causes outgassing of the coating surface. This method is acceptable for glass or metal.

Billingsley, J. M.↗

NASA NTRS1981

Attenuation of ultrasonic interface waves on metal-polymer-metal boundaries

The measured sensitivity of interface wave attenuation to defects near the bondline and to variations in the viscosity of the adhesive layer was compared with theoretical changes predicted by the Rokhin model. Differential interferometric optical measurements of interface wave attenuation due to defects near glass polymer metal boundaries are discussed. Pitch catch and pulse echo methods which use variable angle wedge transducers to generate and receive modified interface waves and to measure large bondline defects and adhesive viscosity are described.

Claus, R. O.↗

NASA NTRS1986

Containerless glass fiber processing

An acoustic levitation furnace system is described that was developed for testing the feasibility of containerless fiber pulling experiments. It is possible to levitate very dense materials such as platinum at room temperature. Levitation at elevated temperatures is much more difficult. Samples of dense heavy metal fluoride glass were levitated at 300 C. It is therefore possible that containerless fiber pulling experiments could be performed. Fiber pulling from the melt at 650 C is not possible at unit gravity but could be possible at reduced gravities. The Acoustic Levitation Furnace is described, including engineering parameters and processing information. It is illustrated that a shaped reflector greatly increases the levitation force aiding the levitation of more dense materials.

Ethridge, E. C.↗

NASA NTRS2006

Microspheres in Plasma Display Panels

Filling small bubbles of molten glass with gases is just as difficult as it sounds, but the technical staff at NASA is not known to shy away from a difficult task. When Microsphere Systems, Inc. (MSI), of Ypsilanti, Michigan, and Imaging Systems Technology, Inc. (IST), of Toledo, Ohio, were trying to push the limits of plasma displays but were having difficulty with the designs, NASA s Glenn Garrett Morgan Commercialization Initiative (GMCI) assembled key personnel at Glenn Research Center and Ohio State University for a brainstorming session to come up with a solution for the companies. They needed a system that could produce hollow, glass micro-sized spheres (microspheres) that could be filled with a variety of gasses. But the extremely high temperature required to force the micro-sized glass bubbles to form at the tip of a metal nozzle resulted in severe discoloration of the microspheres. After countless experiments on various glass-metal combinations, they had turned to the GMCI for help. NASA experts in advanced metals, ceramics, and glass concluded that a new design approach was necessary. The team determined that what was needed was a phosphate glass composition that would remain transparent, and they went to work on a solution. Six weeks later, using the design tips from the NASA team, Tim Henderson, president of MSI, had designed a new system in which all surfaces in contact with the molten glass would be ceramic instead of metal. Meanwhile, IST was able to complete a Phase I Small Business Innovation Research (SBIR) grant supported by the National Science Foundation (NSF) and supply a potential customer with samples of the microspheres for evaluation as filler materials for high-performance insulations.

Source record↗

DOE OSTI2020

Near-Field Corrosion Interactions between Glass and Corrosion Resistant Alloys

This study explores the corrosion interactions between model nuclear waste glass materials and corrosion resistant alloys, under conditions that simulate the near field of a nuclear waste repository. The interactions between the corrosion of stainless steel (SS) 316, alloy G30, or alloy 625, and international simple glass or soda-lime silica glass are systematically studied. The dissimilar materials were exposed in close proximity to each other in different electrolytes at 90 oC. After exposure, the glass surface exposed near metals showed different regimes of corrosion, with distinct surface morphologies and chemistries that were likely affected by the local environment created by the localized corrosion of metals. Surface and solution analyses showed that the corrosion rate of glass was enhanced by the presence of metals. Infrared spectroscopy data suggested the local build-up of stresses in the contact area of glass, which may lead to the mechanical instability of the glass alteration layer. On the other hand, the effect of glass on metal corrosion is strongly dependent on the leaching solution. In electrolytes containing abundant aggressive anions such as Cl-, glass seems to suppress the localized corrosion of SS by the precipitation of a Si-rich surface film that protects the SS substrate from solutions. However, in less aggressive electrolytes, the corrosion rate of SS was increased by the presence of glass corrosion products. Overall, our study showed that the hidden and localized damage on glass in contact with metals may enhance the release of incorporated radionuclides compared to typical uniform glass corrosion. Therefore, more attention should be paid to the corrosion interactions between metals and glass under repository conditions.

Guo, Xiaolei↗