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Degradation of Yttria-Stabilized Zirconia in Molten Regolith Electrolysis Applications

The generation of oxygen from lunar resources is an enabling technology to support a sustained human presence on the lunar surface. Molten regolith electrolysis is a promising process for directly electrolyzing lunar regolith, which is primarily a mixture of oxide minerals. During electrolysis, metallic products (Fe, Si) are formed at the cathode and oxygen is produced at the anode. In order to perform electrolysis, the regolith must be molten to enable ionic transport of metallic cations and oxygen anions, requiring an operating temperature of 1600C. Common refractory oxide materials, such as Al2O3 and MgO, undergo rapid degradation due to the high operating temperature and contact with the corrosive molten regolith. This work investigates yttria-stabilized zirconia (YSZ) for molten regolith electrolysis applications. Corrosion studies are presented to elucidate the degradation mechanism of YSZ powders and crucibles exposed to lunar regolith simulants at 1600C. Two regolith simulants are used to represent regolith from the lunar maria (JSC-1A) and the lunar highlands (LHS-1). Degradation of YSZ in contact with regolith simulants is evaluated using SEM/EDS, XRD, and EBSD. Furthermore, a modified molten regolith electrolysis reactor is presented utilizing YSZ at the anode to enable facile collection of oxygen produced during electrolysis.

Kevin Yu↗

NASA NTRS1978

Fabrication and testing of silver-hydrogen cells

Silver electrodes containing various additives were fabricated and tested in single electrode cells in order to improve the electrochemical utilization of sintered silver cathodes in Ag-H2 aerospace batteries. A standard stack arrangement was used which featured a NASA-developed organic-inorganic separator. All cells were cycled in a regime designed to remove 75% of the cells nominal capacity based on 3.3 gms/AHr Ag utilization. In cases where performance degradation was observed, the main feature mode appeared to be corrosion of either the expanded silver current collector or the connection between the silver electrode and the electrode tab. Promising silver electrodes from single electrode studies were used in the construction of 35 AHr Ag-H2 cells. Two such cells were constructed and installed in heavy walled pressure vessels for testing. Based on the data obtained from all cells tested during the program, four lightweight 35 AHr cells were fabricated. During acceptance testing these cells yielded an average gravimetric energy density of 30 WHr/1b.

Debicarri, D. J.↗

NASA NTRS2005

NASA Tech Briefs, January 2005

Topics covered include: Fiber-Optic Sensor Would Monitor Growth of Polymer Film; Sensors for Pointing Moving Instruments Toward Each Other; Pd/CeO2/SiC Chemical Sensors; Microparticle Flow Sensor; Scattering-Type Surface-Plasmon-Resonance Biosensors; Diode-Laser-Based Spectrometer for Sensing Gases; Improved Cathode Structure for a Direct Methanol Fuel Cell; X-Band, 17-Watt Solid-State Power Amplifier; Improved Anode for a Direct Methanol Fuel Cell; Tools for Designing and Analyzing Structures; Interactive Display of Scenes with Annotations; Solving Common Mathematical Problems; Tools for Basic Statistical Analysis; Program Calculates Forces in Bolted Structural Joints; Integrated Structural Analysis and Test Program; Molybdate Coatings for Protecting Aluminum Against Corrosion; Synthesizing Diamond from Liquid Feedstock; Modifying Silicates for Better Dispersion in Nanocomposites; Powder-Collection System for Ultrasonic/Sonic Drill/Corer; Semiautomated, Reproducible Batch Processing of Soy; Hydrogen Peroxide Enhances Removal of NOx from Flue Gases; Subsurface Ice Probe; Real-Time Simulation of Aeroheating of the Hyper-X Airplane; Using Laser-Induced Incandescence To Measure Soot in Exhaust; Method of Real-Time Principal-Component Analysis; Insect-Inspired Flight Control for Unmanned Aerial Vehicles; Domain Compilation for Embedded Real-Time Planning; Semantic Metrics for Analysis of Software; Simulation of Laser Cooling and Trapping in Engineering Applications; Large Fluvial Fans and Exploration for Hydrocarbons; Doping-Induced Interband Gain in InAs/AlSb Quantum Wells; Development of Software for a Lidar-Altimeter Processor; Upgrading the Space Shuttle Caution and Warning System; and Fractal Reference Signals in Pulse-Width Modulation.

Source record↗

NASA NTRS2002

Galvanic Liquid Applied Coating System for Protection of Embedded Steel Surfaces from Corrosion

The corrosion of reinforcing steel in concrete is an insidious problem for the Kennedy Space Center, government agencies, and the general public. Existing corrosion protection systems on the market are costly, complex, and time-consuming to install, require continuous maintenance and monitoring, and require specialized skills for installation. NASA's galvanic liquid-applied coating offers companies the ability to conveniently protect embedded steel rebar surfaces from corrosion. Liquid-applied inorganic galvanic coating contains one ore more of the following metallic particles: magnesium, zinc, or indium and may contain moisture attracting compounds that facilitate the protection process. The coating is applied to the outer surface of reinforced concrete so that electrical current is established between metallic particles and surfaces of embedded steel rebar; and electric (ionic) current is responsible for providing the necessary cathodic protection for embedded rebar surfaces.

Curran, Joseph↗

NASA NTRS1981

Technology development for phosphoric acid fuel cell powerplant, phase 2

The development of materials, cell components, and reformers for on site integrated energy systems is described. Progress includes: (1) heat-treatment of 25 sq cm, 350 sq cm and 1200 sq cm cell test hardware was accomplished. Performance of fuel cells is improved by using this material; (2) electrochemical and chemical corrosion rates of heat-treated and as-molded graphite/phenolic resin composites in phosphoric acid were determined; (3) three cell, 5 in. x 15 in. stacks operated for up to 10,000 hours and 12 in. x 17 in. five cell stacks were tested for 5,000 hours; (4) a three cell 5 in. x 15 in. stack with 0.12 mg Pt/sq cm anodes and 0.25 mg Pt/sq cm cathodes was operated for 4,500 hours; and (5) an ERC proprietary high bubble pressure matrix, MAT-1, was tested for up to 10,000 hours.

Christner, L.↗

NASA NTRS2015

Iodine Satellite

The Iodine Satellite (iSat) spacecraft will be the first CubeSat to demonstrate high change in velocity from a primary propulsion system by using Hall thruster technology and iodine as a propellant. The mission will demonstrate CubeSat maneuverability, including plane change, altitude change and change in its closest approach to Earth to ensure atmospheric reentry in less than 90 days. The mission is planned for launch in fall 2017. Hall thruster technology is a type of electric propulsion. Electric propulsion uses electricity, typically from solar panels, to accelerate the propellant. Electric propulsion can accelerate propellant to 10 times higher velocities than traditional chemical propulsion systems, which significantly increases fuel efficiency. To enable the success of the propulsion subsystem, iSat will also demonstrate power management and thermal control capabilities well beyond the current state-of-the-art for spacecraft of its size. This technology is a viable primary propulsion system that can be used on small satellites ranging from about 22 pounds (10 kilograms) to more than 1,000 pounds (450 kilograms). iSat's fuel efficiency is ten times greater and its propulsion per volume is 100 times greater than current cold-gas systems and three times better than the same system operating on xenon. iSat's iodine propulsion system consists of a 200 watt (W) Hall thruster, a cathode, a tank to store solid iodine, a power processing unit (PPU) and the feed system to supply the iodine. This propulsion system is based on a 200 W Hall thruster developed by Busek Co. Inc., which was previously flown using xenon as the propellant. Several improvements have been made to the original system to include a compact PPU, targeting greater than 80 percent reduction in mass and volume of conventional PPU designs. The cathode technology is planned to enable heaterless cathode conditioning, significantly increasing total system efficiency. The feed system has been designed to include iodine compatible control valves with internal heaters and temperature sensors to coincide with the iodine-compatible thruster. A key advantage to using iodine as a propellant is that it may be stored in the tank as an unpressurized solid on the ground and before flight operations. During operations, the tank is heated to vaporize the propellant. Iodine vapor is then routed through custom flow control valves to control mass flow to the thruster and cathode assembly. The thruster then ionizes the vapor and accelerates it via magnetic and electrostatic fields, resulting in high specific impulse, characteristic of a highly efficient propulsion system. The iSat spacecraft is a 12-unit (12U) CubeSat with dimensions of about 8 inches x 8 inches x 12 inches (20 centimeters x 20 centimeters x 30 centimeters). The spacecraft frame will be constructed from aluminum with a finish to prevent iodine-driven corrosion. The iSat spacecraft includes full three-axis control and will leverage heat generated by spacecraft components and radiators for a passive thermal control system. After the CubeSat has successfully detached from its launch vehicle, it will deploy its solar panels, correct for tip-off and maintain attitude control before ground contact. An initial check-out period of two weeks is planned for testing all subsystems. The spacecraft will charge the power system while in sunlight, using momentum wheels and magnetic torque rods to rotate the vehicle to the required attitude.

iSat↗

NASA NTRS2023

Long Life Molten Salt Battery for NASA Venus Application

A development program is being conducted at Advanced Thermal Batteries (ATB) to create a low discharge rate, long life, molten salt battery for a NASA Venus surface probe. Battery goals are 60 days continuous operation at +25V +0/-6 volts and -25V +6/-0 Volts under severe environments of 465°C, 92 atm pressure, and corrosive sulfur dioxide in a super critical carbon dioxide atmosphere. Conveniently, molten salt thermal battery electrochemistry starts to operate efficiently at 330°C. However, a major barrier to direct application of existing thermal battery technology is the high self-discharge rate, resulting in lifetimes in only minutes, not days. The best performance to date, which meets the required voltage regulation, has been a lithium silicon (LiSi) alloy anode discharging through all three voltage plateau versus an iron monosulfide (FeS) cathode. In order to perform reproducibly, additional engineering controls within the battery design are required to limit cell–to–cell parasitic discharge mechanisms. Results of these trials have improved the efficiency and manufacturability of the design.

Thermal Battery↗

NASA NTRS1974

Stress corrosion cracking of a titanium alloy in chloride-containing liquid environments

Ti-8 Al-1 Mo-1 V was tested in solvents containing chloride, bromide or iodide ions. It was found that the region II plateau velocity could be correlated with the inverse of the viscosity for several solvents. It seems most likely that this reflects the influence of the viscosity on the diffusion coefficient of some species involved in a mass transfer process which limits the crack growth. Associated tests were performed in which the potential, pH and concentration of Cl- were varied, in some of the same solutions as used for the viscosity tests. It is concluded from these tests that the absence of cathodic protection against cracking in solutions of low pH arises from an ohmic effect which isolates the crack tip from external potential control.

Smyrl, W. H.↗

NASA NTRS2004

Ionic Liquids and New Proton Exchange Membranes for Fuel Cells

There is currently a great surge of activity in fuel cell research as laboratories across the world seek to take advantage of the high energy capacity provided by &el cells relative to those of other portable electrochemical power systems. Much of this activity is aimed at high temperature fie1 cells, and a vital component of such &el cells must be the availability of a high temperature stable proton-permeable membrane. NASA Glenn Research Center is greatly involved in developing this technology. Other approaches to the high temperature fuel cell involve the use of single- component or almost-single-component electrolytes that provide a path for protons through the cell. A heavily researched case is the phosphoric acid fuel cell, in which the electrolyte is almost pure phosphoric acid and the cathode reaction produces water directly. The phosphoric acid fie1 cell delivers an open circuit voltage of 0.9 V falling to about 0.7 V under operating conditions at 170 C. The proton transport mechanism is mainly vehicular in character according to the viscosity/conductance relation. Here we describe some Proton Transfer Ionic Liquids (PTILs) with low vapor pressure and high temperature stability that have conductivities of unprecedented magnitude for non-aqueous systems. The first requirement of an ionic liquid is that, contrary to experience with most liquids consisting of ions, it must have a melting point that is not much above room temperature. The limit commonly suggested is 100 C. PTILs constitute an interesting class of non-corrosive proton-exchange electrolyte, which can serve well in high temperature (T = 100 - 250 C) fuel cell applications. We will present cell performance data showing that the open circuit voltage output, and the performance of a simple H2(g)Pt/PTIL/Pt/O2(g) fuel cell may be superior to those of the equivalent phosphoric acid electrolyte fuel cell both at ambient temperature and temperatures up to and above 200 C. My work at NASA Glenn Research Center during this summer is to develop and characterize proton exchange membranes doped with ionic liquids. The main techniques used to characterize these materials are: Impedance Spectroscopy, NMR, DSC, TGA, DMA, IR, and SEM ...

Belieres, Jean-Philippe↗

NASA NTRS2005

Anti-Corrosive Powder Particles

The National Aeronautics and Space Administration (NASA) seeks partners for a new approach in protecting embedded steel surfaces from corrosion. Corrosion of reinforced steel in concrete structures is a significant problem for NASA structures at Kennedy Space Center (KSC) because of the close proximity of the structures to salt spray from the nearby Atlantic Ocean. In an effort to minimize the damage to such structures, coatings were developed that could be applied as liquids to the external surfaces of a substrate in which the metal structures were embedded. The Metallic Pigment Powder Particle technology was developed by NASA at KSC. This technology combines the metallic materials into a uniform particle. The resultant powder can be sprayed simultaneously with a liquid binder onto the surface of concrete structures with a uniform distribution of the metallic pigment for optimum cathodic protection of the underlying steel in the concrete. Metallic Pigment Powder Particle technology improves upon the performance of an earlier NASA technology Liquid Galvanic Coating (U.S. Patent No. 6,627,065).

Parker, Donald↗

NASA NTRS1989

Advanced rechargeable sodium batteries with novel cathodes

Various high energy density rechargeable batteries are being considered for future space applications. Of these, the sodium-sulfur battery is one of the leading candidates. The primary advantage is the high energy density (760 Wh/kg theoretical). Energy densities in excess of 180 Wh/kg were realized in practical batteries. Other technological advantages include its chemical simplicity, absence of self-discharge, and long cycle life possibility. More recently, other high temperature sodium batteries have come into the spotlight. These systems can be described as follow: Na/Beta Double Prime-Al2O3/NaAlCl4/Metal Dichloride Sodium/metal dichloride systems are colloquially known as the zebra system and are currently being developed for traction and load leveling applications. The sodium-metal dichloride systems appear to offer many of the same advantages of the Na/S system, especially in terms of energy density and chemical simplicity. The metal dichloride systems offer increased safety and good resistance to overcharge and operate over a wide range of temperatures from 150 to 400 C with less corrosion problems.

Distefano, S.↗

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↗

NASA NTRS1991

Magma Electrolysis: An update

Electrolytic extraction of O2 from molten lunar soil is conceptually simple and thus a candidate process for producing O2 on the Moon. Possible container and electrode materials are being tested for durability in corrosive high-temperature silicate melts and looking for complications that might increase energy requirements. Gaseous oxygen is being produced by electrolysis of 1-2 gram quantities of silicate melts in spinel (MgAl2O4) crucibles; in these melts, spinel is a stable phase. The concentration of FeO was kept low because FeO decrease O2 production efficiency. Platinum electrodes were placed about 0.5 cm apart in the melt. The spinel crucible was still intact after 40 minutes of electrolysis, when the experiment was halted for examination. The Pt anode was also intact; its Pt was maintained in a dynamci state in which the anode was continuously oxidized but quickly reduced again by the silicate melt, inhibiting migration of Pt away from the anode. In melts with low concentrations of Al2O3 + SiO2 (2 wt percent), the energy of resistance heating was only approximately equal to 10 to 20 percent of the theoretical amount required to produce O2. In melts substantially more concentrated in Al2O3 + SiO2, higher melt viscosity resulted in frothing that, in the worst case, caused high enough melt resistivities to raise the energy requirements to nearly 10 times theoretical. Both Fe and Si are produced at the cathode; in iron-rich melts, a- and c-iron and molten ferrosilicon were observed. Production was also observed at the cathode of a previously unrecognized gas; which is not yet identified. The solubility of metallic species was measured in silicate melts. They are too low to reduce significantly the efficiency of O2 production.

Colson, Russell O.↗

NASA NTRS1991

The effect of zinc additions on the environmental stability of Alloy 8090 (Al-Li-Cu-Mg-Zr)

Stress corrosion cracking (SCC) remains a problem in both Al-Li and conventional Al heat treatable alloys. It has recently been found that relatively small additions (less than or approximately 1 wt-percent) of Zn can dramatically improve the SCC performance of alloy 8090 (Al-Li-Cu-Mg-Zr). Constant load time to failure experiments using cylindrical tensile samples loaded between 30 and 85 percent of TYS indicate improvements of orders of magnitude over the baseline 8090 for the Zn-containing alloys under certain aging conditions. However, the toughnesses of the alloys were noticeably degraded due to the formation of second phase particles which primarily reside on grain and subgrain boundaries. EDS revealed that these intermetallic particles were Cu and Zn rich. The particles were present in the T3 condition and were not found to be the result of quench rate, though their size and distribution were. At 5 hours at 160 C, the alloys displayed the greatest susceptibility to SCC but by 20 hours at 160 C the alloys demonstrated markedly improved TTF lifetimes. Aging past this time did not provide separable TTF results, however, the alloy toughnesses continued to worsen. Initial examination of the alloys microstructures at 5 and 20 hours indicated some changes most notably the S' and delta' distributions. A possible model by which this may occur will be explored. Polarization experiments indicated a change in the trend of E(sub BR) and passive current density at peak aging as compared to the baseline 8090. Initial pitting experiments indicated that the primary pitting mechanism in chloride environments is one occurring at constituent (Al-Fe-Cu) particles and that the Cu and Zn rich boundary precipitates posses a breakaway potential similar to that of the matrix acting neither anodic or cathodic in the first set of aerated 3.5 w/o NaCl experiments. Future work will focus on the identification of the second phase particles, evaluation of K(sub 1SCC) and plateau da/dt via both DCB and slow strain rate techniques. A lower Zn content variant will be examined in the near future in hopes of optimizing toughness, density and SCC performance.

Kilmer, Raymond J.↗