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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
NASA NTRS1992

Lunar resources: Oxygen from rocks and soil

The first set of hydrogen reduction experiments to use actual lunar material was recently completed. The sample, 70035, is a coarse-grained vesicular basalt containing 18.46 wt. percent FeO and 12.97 wt. percent TiO2. The mineralogy includes pyroxene, ilmenite, plagioclase, and minor olivine. The sample was crushed to a grain size of less than 500 microns. The crushed basalt was reduced with hydrogen in seven tests at temperatures of 900-1050 C and pressures of 1-10 atm for 30-60 minutes. A capacitance probe, measuring the dew point of the gas stream, was used to follow reaction progress. Experiments were also conducted using a terrestrial basalt similar to some lunar mare samples. Minnesota Lunar Simulant (MLS-1) contains 13.29 wt. percent FeO, 2.96 wt. percent Fe2O3, and 6.56 wt. percent TiO2. The major minerals include plagioclase, pyroxene, olivine, ilmenite, and magnetite. The rock was ground and seived, and experiments were run on the less than 74- and 500-1168-micron fractions. Experiments were also conducted on less than 74-micron powders of olivine, pyroxene, synthetic ilmenite, and TiO2. The terrestrial rock and mineral samples were reduced with flowing hydrogen at 1100 C in a microbalance furnace, with reaction progress monitored by weight loss. Experiments were run at atmospheric pressure for durations of 3-4 hr. Solid samples from both sets of experiments were analyzed by Mossbauer spectroscopy, petrographic microscopy, scanning electron microscopy, tunneling electron microscopy, and x-ray diffraction. Apollo 17 soil 78221 was examined for evidence of natural reduction in the lunar environment. This sample was chosen based on its high maturity level (I sub s/FeO = 93.0). The FeO content is 11.68 wt. percent and the TiO2 content is 3.84 wt. percent. A polished thin section of the 90-150 micron size fraction was analyzed by petrographic microscopy and scanning electron microscopy.

Allen, C. C.↗
NASA NTRS1993

Thermodynamics of lunar ilmenite reduction

With the prospect of returning to the moon, the development of a lunar occupation would fulfill one of the goals of the Space Exploration Initiative (SEI) of the late 1980's. Processing lunar resources into useful products, such as liquid oxygen for fuel and life support, would be one of many aspects of an active lunar base. ilmenite (FeTiO3) is found on the lunar surface and can be used as a feed stock to produce oxygen. Understanding the various ilmenite-reduction reactions elucidates many processing options. Defining the thermodynamic chemical behavior at equilibrium under various conditions of temperature and pressures can be helpful in specifying optimal operating conditions. Differences between a previous theoretical analysis and experimentally determined results has sparked interest in trying to understand the effect of operating pressure on the hydrogen-reduction-of-ilmenite reaction. Various aspects of this reduction reaction are discussed.

Altenberg, B. H.↗
NASA NTRS2008

Carbothermal Processing of Lunar Regolith Using Methane

The processing of lunar regolith for the production of oxygen is a key component of the In-Situ Resource Utilization plans currently being developed by NASA. Among various candidate processes, the modeling of oxygen production by hydrogen reduction, molten salt electrolysis, and carbothermal processing are presently being pursued. In the carbothermal process, a portion of the surface of the regolith in a container is heated by exposure to a heat source such as a laser beam or a concentrated solar heat flux, so that a small zone of molten regolith is established. The molten zone is surrounded by solid regolith particles that are poor conductors of heat. A continuous flow of methane is maintained over the molten regolith zone. Our model is based on a mechanism where methane pyrolyzes when it comes in contact with the surface of the hot molten regolith to form solid carbon and hydrogen gas. Carbon is deposited on the surface of the melt, and hydrogen is released into the gas stream above the melt surface. We assume that the deposited carbon mixes in the molten regolith and reacts with metal oxides in a reduction reaction by which gaseous carbon monoxide is liberated. Carbon monoxide bubbles through the melt and is released into the gas stream. Oxygen is produced subsequently by (catalytically) processing the carbon monoxide downstream. In this paper, we discuss the development of a chemical conversion model of the carbothermal process to predict the rate of production of carbon monoxide.

Balasubramaniam, R.↗
NASA NTRS2009

Carbothermal Processing of Lunar Regolith Using Methane

The processing of lunar regolith for the production of oxygen is a key component of the In-Situ Resource Utilization plans currently being developed by NASA. Among various candidate processes, the modeling of oxygen production by hydrogen reduction, molten salt electrolysis, and carbothermal processing are presently being pursued. In the carbothermal process, a portion of the surface of the regolith in a container is heated by exposure to a heat source such as a laser beam or a concentrated solar heat flux, so that a small zone of molten regolith is established. The molten zone is surrounded by solid regolith particles that are poor conductors of heat. A continuous flow of methane is maintained over the molten regolith zone. Our model is based on a mechanism where methane pyrolyzes when it comes in contact with the surface of the hot molten regolith to form solid carbon and hydrogen gas. Carbon is deposited on the surface of the melt, and hydrogen is released into the gas stream above the melt surface. We assume that the deposited carbon mixes in the molten regolith and reacts with metal oxides in a reduction reaction by which gaseous carbon monoxide is liberated. Carbon monoxide bubbles through the melt and is released into the gas stream. Oxygen is produced subsequently by (catalytically) processing the carbon monoxide downstream. In this paper, we discuss the development of a chemical conversion model of the carbothermal process to predict the rate of production of carbon monoxide.

Balasubramaniam, R.↗
NASA NTRS1991

Mechanisms of ilmenite reduction and their impact on the design of effective reactor systems

One of the first activities at a lunar base could be oxygen recovery from ilmenite (FeTiO3). Oxygen produced from lunar soils could be used to fuel transportation vehicles operating in near-earth space. The first step in developing a suitable reactor system for lunar operation is to determine the mechanisms and rates of oxygen removal from ilmenite. In-situ gravimetric measurements and microscopic examinations were used to determine the hydrogen reduction mechanisms of synthetic ilmenite discs between 823 to 1353 K. A shrinking core reaction model, modified to account for the growth of an iron film on the surface of discs, was capable of predicting experimentally observed conversion-time relationships. The observed reduction mechanism, kinetic rates, and associated activation energy established a base line from which comparisons could be made to improve oxygen yield and removal rates. One proposed technique to improve the rate and extent of oxygen removal was to preoxidize ilmenite. Preoxidation is commonly used during the reduction of ilmenite ores in the iron industry and has been employed for many years to lower operating temperatures and increase reduction rates. This technology could prove beneficial for oxygen production facilities on the Moon as less massive reactor vessels and/or less energy could be associated with a process including preoxidation. X ray diffraction and energy dispersive spectroscopy were utilized to follow the progression of ilmenite oxidation at 1123 and 1140 K and the reduction of pseudobrookite (Fe2TiO5) at 873 and 973 K. Structures formed during the progress of oxidation were related to the system's phase diagrams. Results indicated that after initially producing ilmenite-hematite solutions and rutile (TiO2), pseudobrookite was the end product of oxidation at all temperatures examined (1049 to 1273 K). Initial results from the reduction of pseudobrookite indicate a series of phases are produced including ferropseudobrookite (FeTi2O5), ulvospinel (Fe2TiO4), and ilmenite. Rates of pseudobrookite reduction were typically 50 to 200 times that of ilmenite.

Briggs, R. A.↗
NASA NTRS2009

Oxygen Production from Lunar Regolith using Ionic Liquids

The objective of this work and future follow-on work is to develop a safe, efficient, and recyclable method for oxygen and/or metals extraction from lunar regolith, in support of establishing a manned lunar outpost. The approach is to solubilize the oxides that comprise lunar regolith in media consisting of ionic liquids (ILs) and/or their mixtures at temperatures at or below 300 C. Once in solution, electrolysis can either be performed in-situ to generate oxygen at the anode and hydrogen and/or metals (silicon, iron, aluminum, titanium, etc.) at the cathode. Alternatively, the water that is generated during the solubilization process can be distilled out and condensed into a separate IL and then electrolysized to produce hydrogen and oxygen. In the case of lunar regolith, this method could theoretically produce 44g oxygen per 100g of regolith. The oxygen can be used for human life support and/or as an oxidizer for rocket fuels, and the metals can be used as raw materials for construction and/or device fabrication. Moreover, the hydrogen produced can be used to re-generate the acidic medium, which can then be used to process additional regolith, thereby making the materials recyclable and limiting upmass requirements. An important advantage of IL acid systems is that they are much "greener" and safer than conventional materials used for regolith processing such as sulfuric or hydrochloric acids. They have very low vapor pressures, which means that they contain virtually no toxic and/or flammable volatile content, they are relatively non-corrosive, and they can exhibit good stability in harsh environments (extreme temperatures, hard vacuum, etc.). Furthermore, regolith processing can be achieved at lower temperatures than other processes such as molten oxide electrolysis or hydrogen reduction, thereby reducing initial power requirements. Six ILs have been synthesized and tested for their capability to dissolve lunar simulant, and for electrochemical and thermal stability. The results showed that ILs can be very efficient electrolytes; in particular IL/phosphoric-acid mixtures appear extremely promising for solubilizing lunar simulant. Results from preliminary experiments for distillation of water produced from the oxygen within the metal oxides of the simulant and the hydrogen from the acid indicates that over 75% of the oxygen from the simulant can be harvested as water at a temperature of 150 C. A method for collection of oxygen from electrolysis of the water derived from solubilizing simulant was developed by using a liquid nitrogen trap to liquefy and collect the oxygen. Although precise quantification of the liquid oxygen trapped is difficult to obtain, the amount of hydrogen and oxygen collected from electrolysis of water in this system was greater than 98%. This set-up also included a portable mass spectrometer for the identification of gases released from electrolysis cells. Regeneration of ILs through re-protonation was also demonstrated. Four sequential re-generations of an IL following solubilization of simulant showed no significant differences in amounts of simulant dissolved. Follow-on work for this project should include more studies of IL/phosphoric acid systems. Also, much more work is necessary for defining methods for electrolysis and purification of metals from regolith solubilized in ILs, and for developing a system to use the produced hydrogen to regenerate the spent IL. Finally, design and development of flight breadboard and prototype hardware is required.

Paley, Mark Steven↗
DOE OSTI2025

Superconductivity in the Parent Infinite-Layer Nickelate NdNiO 2

We report evidence for superconductivity with onset temperatures up to 11 K in thin films of the infinite-layer nickelate parent compound NdNiO 2 . A combination of oxide molecular beam epitaxy and atomic hydrogen reduction yields samples with high crystallinity and low residual resistivities, a substantial fraction of which exhibit superconducting transitions. We survey a large series of samples with a variety of techniques, including electrical transport, scanning transmission electron microscopy, x-ray absorption spectroscopy, and resonant inelastic x-ray scattering, to investigate the possible origins of superconductivity. We propose that superconductivity could be intrinsic to the undoped infinite-layer nickelates but suppressed by disorder due to a possibly sign-changing order parameter, a finding which would necessitate a reconsideration of the nickelate phase diagram. Another possible hypothesis is that the parent materials can be hole doped from randomly dispersed apical oxygen atoms, which would suggest an alternative pathway for achieving superconductivity. Published by the American Physical Society 2025

36 MATERIALS SCIENCE↗
DOE OSTI2024

Institute for Catalysis in Energy Processes (ICEP) (Final Report)

The Institute for Catalysis in Energy Processes (ICEP) was a multi-PI program located at the Northwestern University Center for Catalysis and Surface Science from 2006-2024. Over several renewal cycles and several organizing themes, ICEP addressed fundamental questions in catalysis science. In turn, the scientific questions addressed were directly relevant to the efficient use of the nation’s resources to produce fuels and commodity chemicals, harness alternate energy sources for chemical reactions such as light or electricity, reduce emissions and waste, and minimize the impact of our use of plastics. Selective oxidation, (oxidative) dehydrogenation, deNOx, CO 2 reduction, hydrogen release, polymer decomposition / depolymerization, and many other reactions of intense interest to the US Department of Energy were studied in the center. Major ICEP strengths were in catalyst synthesis, in measurements that elucidated catalyst properties, in reaction mechanisms and kinetics, and in predictive theory and modeling. ICEP researchers were often the inventors or developers of materials and methods that were brought to bear on the Institute’s catalytic systems. Key characterization tools advanced through this project included resonance Raman and related techniques, sum frequency generation, and X-ray standing wave spectroscopy. Center members relied extensively on computational tools such as density functional theory and microkinetic modeling to fully investigate catalyst structures and catalytic mechanisms. ICEP researchers were early developers of atomic layer deposition (ALD) for catalyst synthesis and were early pioneers of metal organic frameworks for catalysis. ICEP innovations are found in areas of intense research such as single-atom catalysts, catalytic deconstruction of plastics, and catalytic MOFs, to name a few. Research areas initiated by ICEP indirectly led to DOE EFRCs, startup companies, and other achievements. Over its 18 years of existence, ICEP involved two different PIs (Stair and Notestein) and 24 senior investigators across several academic disciplines at Northwestern University. There were tight collaborations with Argonne National Laboratory, including specialized equipment and experiments permanently located there. The center supported ~400 person-years of effort by graduate students and postdocs, either directly through DOE support or indirectly by leveraging independent support provided to the trainees, e.g. through the NSF GRFP or internal fellowships. The project resulted in 328 manuscripts and numerous conference presentations.

36 MATERIALS SCIENCE↗
NASA NTRS1976

Development and study of chemical vapor deposited tantalum base alloys

A technique for the chemical vapor deposition of alloys was developed. The process, termed pulsing, involves the periodic injection of reactant gases into a previously-evacuated reaction chamber where they blanket the substrate almost instantaneously. Formation of alternating layers of the alloy components and subsequent homogenization allows the formation of an alloy of uniform composition with the composition being determined by the duration and relative numbers of the various cycles. The technique has been utilized to produce dense alloys of uniform thickness and composition (Ta- 10 wt % W) by depositing alternating layers of Ta and W by the hydrogen reduction of TaCl5 and WCl6. A similar attempt to deposit a Ta - 8 wt % W - 2 wt% Hf alloy was unsuccessful because of the difficulty in reducing HfCl4 at temperatures below those at which gas phase nucleation of Ta and W occurred.

Meier, G. H.↗
NASA NTRS1980

Low-cost solar array project task 1: Silicon material. Gaseous melt replenishment system

The operation of a silicon production technique was demonstrated. The essentials of the method comprise chemical vapor deposition of silicon, by hydrogen reduction of chlorosilanes, on the inside of a quartz reaction vessel having large internal surface area. The system was designed to allow successive deposition-melting cycles, with silicon removal being accomplished by discharging the molten silicon. The liquid product would be suitable for transfer to a crystal growth process, casting into solid form, or production of shots. A scaled-down prototype reactor demonstrated single pass conversion efficiency of 20 percent and deposition rates and energy consumption better than conventional Siemens reactors, via deposition rates of 365 microns/hr. and electrical consumption of 35 Kwhr/kg of silicon produced.

Jewett, D. N.↗
NASA NTRS1983

Efficient Silicon Reactor

High-purity silicon efficiently produced and transferred by continuous two-cycle reactor. New reactor operates in relatively-narrow temperature rate and uses large surfaces area to minimize heat expenditure and processing time in producing silicon by hydrogen reduction of trichlorosilane. Two cycles of reactor consists of silicon production and removal.

Bates, H. E.↗
NASA NTRS1986

Processes and process development in Japan

The commercialization of solar power generation necessitates the development of low cost manufacturing method of silicon suitable for solar cells. The manufacturing methods of semiconductor grade silicon (SEG-Si) and the development of solar grade silicon (SOG-Si) in foreign countries was investigated. It was concluded that the most efficient method of developing such materials was the hydrogen reduction process of trichlorosilane (TCS), using a fluidized bed reactor. The low cost reduction of polysilicon requires cost reductions of raw materials, energy, labor, and capital. These conditions were carefully reviewed. The overall conclusion was that a development program should be based on the TCS-FBR process and that the experimental program should be conducted in test facilities capable of producing 10 tons of silicon granules per year.

Noda, T.↗
NASA NTRS1985

Toward a spartan scenario for use of lunar materials

The present discussion has the objective to identify those raw materials for use in manufacture which can most readily be obtained from lunar materials as they are currently known. The state of lunar exploration is incomplete, and concentrated ores may exist for elements now regarded as rare or dispersed. This paper provides a description of minimum possibilities, based on the notion of making do with the least feasible amounts of separation and processing. The discussion is limited to the most abundant materials observed at lunar sites visited by the Apollo missions. The ground rules for use of lunar products are considered along with the tools required to carry out any significant production of raw materials for manufacture, and lunar surface conditions. Readily available materials include unprocessed regolith and minimally processed regolith. A few examples of processing methods are provided, giving attention to thermal release of gases, hydrogen reduction of ilmenite, carbonyl processing, electrolysis of molten silicate, and destructive distillation.

Haskin, L. A.↗