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NASA NTRS1996

Hydrogen passivation of N(+)-P and P(+)-N heteroepitaxial InP solar cell structures

Dislocations and related point defect complexes caused by lattice mismatch currently limit the performance of heteroepitaxial InP cells by introducing shunting paths across the active junction and by the formation of deep traps within the base region. We have previously demonstrated that plasma hydrogenation is an effective and stable means to passivate the electrical activity of such defects in specially designed heteroepitaxial InP test structures to probe hydrogen passivation at typical base depths within a cell structure. In this work, we present our results on the hydrogen passivation of actual heteroepitaxial n-p and p-n InP cell structures grown on GaAs substrates by metalorganic chemical vapor deposition (MOCVD). We have found that a 2 hour exposure to a 13.56 MHz hydrogen plasma at 275 C reduces the deep level concentration in the base regions of both n(+)-p and p(+)-n heteroepitaxial InP cell structures from as-grown values of 5-7 x 10(exp 14) cm(exp -3), down to 3-5 x 10(exp 12) cm(exp -3). All dopants were successfully reactivated by a 400 C, 5 minute anneal with no detectable activation of deep levels. One to five analysis indicated a subsequent approximately 100 fold decrease in reverse leakage current at -1 volt reverse bias, and an improved built in voltage for the p(+)-n structures. In addition to being passivated, dislocations are also shown to participate in secondary interactions during hydrogenation. We find that the presence of dislocations enhances hydrogen diffusion into the cell structure, and lowers the apparent dissociation energy of Zn-H complexes from 1.19 eV for homoepitaxial Zn-doped InP to 1.12 eV for heteroepitaxial Zn-doped InP. This is explained by additional hydrogen trapping at dislocations subsequent to the reactivation of Zn dopants after hydrogenation.

Chatterjee, Basab↗

NASA NTRS1995

Hydrogen Passivation of N(+)P and P(+)N Heteroepitaxial InP Solar Cell Structures

Dislocations and related point defect complexes caused by lattice mismatch currently limit the performance of heteroepitaxial InP cells by introducing shunting paths across the active junction and by the formation of deep traps within the base region. We have previously demonstrated that plasma hydrogenation is an effective and stable means to passivate the electrical activity of such defects in specially designed heteroepitaxial InP test structures to probe hydrogen passivation at typical base depths within a cell structure. In this work, we present our results on the hydrogen passivation of actual heteroepitaxial n(+)p and p(+)n InP cell structures grown on GaAs substrates by metalorganic chemical vapor deposition (MOCVD). We have found that a 2 hour exposure to a 13.56 MHz hydrogen plasma at 275 C reduces the deep level concentration in the base regions of both n(+)p and p(+)n heteroepitaxial InP cell structures from as-grown values of 5 - 7 x 10(exp 14)/cc, down to 3 - 5 x 10(exp 12)/cc. All dopants were successfully reactivated by a 400 C, 5 minute anneal With no detectable activation of deep levels. I-V analysis indicated a subsequent approx. 100 fold decrease In reverse leakage current at -1 volt reverse bias, and an improved built in voltage for the p(+)n structures. ln addition to being passivated,dislocations are also shown to participate in secondary interactions during hydrogenation. We find that the presence of dislocations enhances hydrogen diffusion into the cell structure, and lowers the apparent dissociation energy of Zn-H complexes from 1.19 eV for homoepitaxial Zn-doped InP to 1.12 eV for heteroepitaxial Zn-doped InP. This is explained by additional hydrogen trapping at dislocations subsequent to the reactivation of Zn dopants after hydrogenation.

Chatterjee, B.↗

NASA NTRS2000

Dynamics of Molecular Hydrogen in Hypersaline Microbial Mars

Early Earth microbial communities that centered around the anaerobic decomposition of organic molecular hydrogen as a carrier of electrons, regulator of energy metabolism, and facilitator of syntroph'c microbial interactions. The advent of oxygenic photosynthetic organisms added a highly dynamic and potentially dominant term to the hydrogen economy of these communities. We have examined the daily variations of hydrogen concentrations in cyanobacteria-dominated microbial mats from hypersaline ponds in Baja California Sur, Mexico. These mats bring together phototrophic and anaerobic bacteria (along with virtually all other trophic groups) in a spatially ordered and chemically dynamic matrix that provides a good analog for early Earth microbial ecosystems. Hydrogen concentrations in the photic zone of the mat can be three orders of magnitude or more higher than in the photic zone, which are, in turn, an order of magnitude higher than in the unconsolidated sediments underlying the mat community. Within the photic zone, hydrogen concentrations can fluctuate dramatically during the diel (24 hour day-night) cycle, ranging from less than 0.001% during the day to nearly 10% at night. The resultant nighttime flux of hydrogen from the mat to the environment was up to 17% of the daytime oxygen flux. The daily pattern observed is highly dependent on cyanobacterial species composition within the mat, with Lyngbya-dominated systems having a much greater dynamic range than those dominated by Microcoleus; this may relate largely to differing degrees of nitrogen-fixing and fermentative activity in the two mats. The greatest H2 concentrations and fluxes were observed in the absence of oxygen, suggesting an important potential feedback control in the context of the evolution of atmospheric composition. The impact of adding this highly dynamic photosynthetic term to the hydrogen economy of early microbial ecosystems must have been substantial. From an evolutionary standpoint, the H2 generated in mats could have represented a very important new source of electrons and energy - but one that could not be harnessed without substantial adaptation to the highly variable chemistry of the mat surface. In addition, the emergent chemistry of anaerobic communities is often highly dependent on ambient hydrogen concentrations, so that incorporation of these communities into photosynthetic mats could have significantly affected the composition and flux of reduced "biosignature' gases to the environment.

Hoehler, Tori M.↗

NASA NTRS2002

Reproducibility and Repeatability of Tensile and Low-Cycle Fatigue Properties in Propulsion Grade Hydrogen

Hydrogen has the potential of increased use in the future as an environmentally friendly fuel. It has, however, shown a tendency to embrittle some materials. To be used in a safe manner and to exploit its full potential, it will be necessary to develop a database of material properties in hydrogen environment. The tests needed to produce this data are costly to perform (tensile test cost 25 times more and low cycle fatigue test are 55 times as expensive). Moreover, there is presently a lack of universal test methods to ensure standardized data within the hydrogen community. Each of the industries that work with hydrogen (aerospace, petroleum, fuel cells, etc.) performs tests by their own laboratory-developed methods, thus rendering cross- comparisons of material property data highly questionable. It is extremely important that data generated in a hydrogen environment be done to a standard that reduces variance to a minimum and allows direct comparison of test results from different laboratories. Doing so will assure that all data generated can be used to further our understanding of the hydrogen effects and to make sure components/products designed for hydrogen are the safest and most reliable possible. This paper reviews the results of two 'round-robin' programs conducted by NASA-MSFC. These two programs examined the reproducibility and repeatability of tensile and low-cycle fatigue test results in high-pressure hydrogen environments. The studies indicated that even with the tightest controls available from current commercial standards, the reproducibility (between different laboratories) and repeatability (within a laboratory) results of the tensile tests exhibited five times the variance as in standard ambient air tests. The variance with the LCF tests were on the same order as with air tests, but that was due to the large variation present in the last Interlaboratory air program. The paper concludes with a recommendation for a program that would allow the development of improved test methods, leading to lower variance in the generation of mechanical property data in the future.

Vesely, E. J.↗

NASA NTRS2005

Hydrogen-powered flight

As the Nation moves towards a hydrogen economy the shape of aviation will change dramatically. To accommodate a switch to hydrogen the aircraft designs, propulsion, and power systems will look much different than the systems of today. Hydrogen will enable a number of new aircraft capabilities from high altitude long endurance remotely operated aircraft (HALE ROA) that will fly weeks to months without refueling to clean, zero emissions transport aircraft. Design and development of new hydrogen powered aircraft have a number of challenges which must be addressed before an operational system can become a reality. While the switch to hydrogen will be most outwardly noticeable in the aircraft designs of the future, other significant changes will be occurring in the environment. A switch to hydrogen for aircraft will completely eliminate harmful greenhouse gases such as carbon monoxide (CO), carbon dioxide (CO2), sulfur oxides (SOx), unburnt hydrocarbons and smoke. While these aircraft emissions are a small percentage of the amount produced on a daily basis, their placement in the upper atmosphere make them particularly harmful. Another troublesome gaseous emission from aircraft is nitrogen oxides (NOx) which contribute to ozone depletion in the upper atmosphere. Nitrogen oxide emissions are produced during the combustion process and are primarily a function of combustion temperature and residence time. The introduction of hydrogen to a gas turbine propulsion system will not eliminate NOx emissions; however the wide flammability range will make low NOx producing, lean burning systems feasible. A revolutionary approach to completely eliminating NOx would be to fly all electric aircraft powered by hydrogen air fuel cells. The fuel cells systems would only produce water, which could be captured on board or released in the lower altitudes. Currently fuel cell systems do not have sufficient energy densities for use in large aircraft, but the long term potential of eliminating greenhouse gas emissions makes it an intriguing and important field of research.

Smith, Timothy D.↗

NASA NTRS2004

Composition and method for hydrogen storage

A method for hydrogen storage includes providing water and hydrogen gas to a containment volume, reducing the temperature of the water and hydrogen gas to form a hydrogen clathrate at a first cryogenic temperature and a first pressure and maintaining the hydrogen clathrate at second cryogenic temperature within a temperature range of up to 250 K to effect hydrogen storage. The low-pressure hydrogen hydrate includes H.sub.2 O molecules, H.sub.2 molecules and a unit cell including polyhedron cages of hydrogen-bonded frameworks of the H.sub.2 O molecules built around the H.sub.2 molecules.

Mao, Wendy L.↗

NASA NTRS2010

Moisture-Induced Alumina Scale Spallation: The Hydrogen Factor

For some time the oxidation community has been concerned with interfacial spallation of protective alumina scales, not just upon immediate cool down, but as a time-delayed phenomenon. Moisture-induced delayed spallation (MIDS) and desktop spallation (DTS) of thermal barrier coatings (TBCs) refer to this process. It is most apparent for relatively adherent alumina scales that have survived initial cool down in a dry environment, have built up considerable thickness and strain energy, and have been somewhat damaged, such as by cyclic oxidation cracking. Indeed, a "sensitive zone" can be described that maximizes the observed effect as a function of all the relevant factors. Moisture has been postulated to serve as a source of interfacial hydrogen embrittlement. Hydrogen is derived from reaction with aluminum in the alloy at an exposed interface. The purpose of this monograph is to trace the close analogy of this phenomenon to other hydrogen-induced effects, such as embrittlement of aluminides and blistering of alloys and anodic alumina films. A formalized, top-down, logic-tree structure is presented as a guide to this discussion. A theoretical basis for interfacial weakening by hydrogen is first cited, as are demonstrations of hydrogen detection as a reaction product or interfacial species. Further support is provided by critical experiments that recreate the moisture effect, but by isolating hydrogen from other potential causative factors. These experiments include tests in H 2-containing atmospheres or cathodic hydrogen charging. Accordingly, they strongly indicate that interfacial hydrogen, derived from moisture, is the key chemical species accounting for delayed alumina scale spallation.

Smialek, James L.↗

NASA NTRS2016

Development of a Microwave Regenerative Sorbent-Based Hydrogen Purifier

This paper describes the design and fabrication of a Microwave Regenerative Sorbent-based Hydrogen Purifier (MRSHP). This unique microwave powered technology was developed for the purification of a hydrogen stream produced by the Plasma Pyrolysis Assembly (PPA). The PPA is a hydrogen recovery (from methane) post processor for NASA's Sabatier-based carbon dioxide reduction process. Embodied in the Carbon dioxide Reduction Assembly (CRA), currently aboard the International Space Station (ISS), the Sabatier reaction employs hydrogen to catalytically recover oxygen, in the form of water, from respiratory carbon dioxide produced by the crew. This same approach is base-lined for future service in the Air Revitalization system on extended missions into deep space where resupply is not practical. Accordingly, manned exploration to Mars may only become feasible with further closure of the air loop as afforded by the greater hydrogen recovery permitted by the PPA with subsequent hydrogen purification. By utilizing the well-known high sorbate loading capacity of molecular sieve 13x, coupled with microwave dielectric heating phenomenon, MRSHP technology is employed as a regenerative filter for a contaminated hydrogen gas stream. By design, freshly regenerated molecular sieve 13x contained in the MRSHP will remove contaminants from the effluent of a 1-CM scale PPA for several hours prior to breakthrough. By reversing flow and pulling a relative vacuum the MRSHP prototype then uses 2.45 GHz microwave power, applied through a novel coaxial antenna array, to rapidly heat the sorbent bed and drive off the contaminants in a short duration vacuum/thermal contaminant desorption step. Finally, following rapid cooling via room temperature cold plates, the MRSHP is again ready to serve as a hydrogen filter.

Wheeler, Richard R., Jr.↗

NASA NTRS2016

Hydrogen Purification and Recycling for an Integrated Oxygen Recovery System Architecture

The United States Atmosphere Revitalization life support system on the International Space Station (ISS) performs several services for the crew including oxygen generation, trace contaminant control, carbon dioxide (CO2) removal, and oxygen recovery. Oxygen recovery is performed using a Sabatier reactor developed by Hamilton Sundstrand, wherein CO2 is reduced with hydrogen in a catalytic reactor to produce methane and water. The water product is purified in the Water Purification Assembly and recycled to the Oxygen Generation Assembly (OGA) to provide O2 to the crew. This architecture results in a theoretical maximum oxygen recovery from CO2 of approx.54% due to the loss of reactant hydrogen in Sabatier-produced methane that is currently vented outside of ISS. Plasma Pyrolysis Assembly (PPA) technology, developed by Umpqua Research Company, provides the capability to further close the Atmosphere Revitalization oxygen loop by recovering hydrogen from Sabatier-produced methane. A key aspect of this technology approach is the need to purify the hydrogen from the PPA product stream which includes acetylene, unreacted methane and byproduct water and carbon monoxide. In 2015, four sub-scale hydrogen separation systems were delivered to NASA for evaluation. These included two electrolysis single-cell hydrogen purification cell stacks developed by Sustainable Innovations, LLC, a sorbent-based hydrogen purification unit using microwave power for sorbent regeneration developed by Umpqua Research Company, and a LaNi4.6Sn0.4 metal hydride produced by Hydrogen Consultants, Inc. Here we report the results of these evaluations to-date, discuss potential architecture options, and propose future work.

Abney, Morgan B.↗

NASA NTRS2016

Hydrogen Purification and Recycling for an Integrated Oxygen Recovery System Architecture

The United States Atmosphere Revitalization life support system on the International Space Station (ISS) performs several services for the crew including oxygen generation, trace contaminant control, carbon dioxide (CO2) removal, and oxygen recovery. Oxygen recovery is performed using a Sabatier reactor developed by Hamilton Sundstrand, wherein CO2 is reduced with hydrogen in a catalytic reactor to produce methane and water. The water product is purified in the Water Purification Assembly and recycled to the Oxygen Generation Assembly (OGA) to provide O2 to the crew. This architecture results in a theoretical maximum oxygen recovery from CO2 of approximately 54% due to the loss of reactant hydrogen in Sabatier-produced methane that is currently vented outside of ISS. Plasma Methane Pyrolysis technology (PPA), developed by Umpqua Research Company, provides the capability to further close the Atmosphere Revitalization oxygen loop by recovering hydrogen from Sabatier-produced methane. A key aspect of this technology approach is to purify the hydrogen from the PPA product stream which includes acetylene, unreacted methane and byproduct water and carbon monoxide. In 2015, four sub-scale hydrogen separation systems were delivered to NASA for evaluation. These included two electrolysis single-cell hydrogen purification cell stacks developed by Sustainable Innovations, LLC, a sorbent-based hydrogen purification unit using microwave power for sorbent regeneration developed by Umpqua Research Company, and a LaNi4.6Sn0.4 metal hydride produced by Hydrogen Consultants, Inc. Here we report the results of these evaluations, discuss potential architecture options, and propose future work.

Abney, Morgan B.↗

NASA NTRSDate not supplied

Hydrogen Sensor via Plasma Techniques Development

Currently, NASA Kennedy Space Center’s Exploration Ground Systems (EGS) uses liquid hydrogen (LH 2 ) as fuel for launches and ensures hydrogen is no longer in the fill lines by sampling gas into a controlled environment. Then they use a catalytic sensor that detects when hydrogen interacts with oxygen. However, this procedure requires repeatedly backfilling and flushing with helium, which can be wasteful during a global helium shortage and expensive for each sampling port. Therefore, the team at KSC set out to establish proof-of-concept of a plasma-based hydrogen sensor that is anaerobic – and can in fact detect in most environments and below atmospheric pressures – and with a small footprint and more sensitive than other hydrogen sensors currently on the market. The technology development was done by testing known concentrations of hydrogen in argon gas fed through a vacuum cube containing an electrode feedthrough at varying pressures. The resultant emission spectra were recorded with a fiber optic spectrometer and analyzed to determine the instrument's accuracy. Throughout testing, efforts were made to prove the off-the-shelf capabilities of the setup. The traditional high voltage AC-power source was switched to an affordable, handheld plasma lighter. Additionally, the spectrometer was supplemented with a double photodiode circuit to take targeted measurements of the Balmer-α and - β lines in the hydrogen spectrum. From this, we established a proof of concept sensor. SLS required it to detect as low as 100 ppm whereas we detected hydrogen in concentrations as low as 50 ppm and in an anaerobic environment. * Work supported by NASA Kennedy Space Center’s Science Mission Directorate Innovative Research and Development Fund.

Plasma↗

NASA NTRS2023

Effects of Strain Rate and Surface Finish on Tensile Properties in High Pressure Hydrogen — A Case Study for LP-DED NASA HR-1

NASA has advanced NASA HR-1 as a solution for liquid rocket engine components that operate in hydrogen rich environments using various AM techniques. The NASA HR-1 for AM applications was specifically formulated for high ductility in high pressure gaseous hydrogen environment in addition to high strength and low cycle fatigue (LCF) resistance. NASA HR-1 meets materials requirements for liquid rocket engine components, including good hydrogen resistance, high conductivity, good LCF performance, and high elongation and strength for components in medium heat flux environments. NASA has completed fabrication of several subscale and full-scale channel wall nozzles in LP-DED NASA HR-1 and completed hot-fire testing. This includes refinement of the process to produce thin-walls and various channel geometries to meet the requirements for channel wall nozzle applications. The main objective of this investigation is to better understand the effects of tensile test strain rate and specimen surface finish on the amount of tensile ductility degradation in high pressure gaseous hydrogen environments. Performing smooth tensile tests in high pressure hydrogen and nitrogen environments can serve as a rapid and economical screening method to determine the relative susceptibility of materials to HEE. This paper presents the tensile test results for LP-DED NASA HR-1 in hydrogen and details the material evaluation on the effects of strain rate and surface finish condition on surface cracking behavior and fracture characteristics. The resistance to HEE for LP-DED NASA HR-1 and the wrought alloy is compared under the same testing conditions. Loss of tensile ductility is quantified in terms of changes in elongation at failure in hydrogen to compare HEE susceptibility. The most suitable strain rate and specimen surface finish condition for future HEE screening testing at MSFC are recommended.

Additive manufacturing↗

NASA NTRS1971

The role of hydrogen in hot-salt stress corrosion cracking of titanium-aluminum alloys

Additional support is presented for the previously proposed role of hydrogen as an embrittling agent in hot-salt stress corrosion cracking of titanium-aluminum alloys. The main source of hydrogen formed during the reactions of titanium alloys with hot salt was identified as water associated with the salt. Hydrogen is produced by the reaction of an intermediate (hydrogen halide) with the alloy rather than from metal-water reactions. The fracture mode of precracked tensile specimens was ductile when the specimens were tested in air, and brittle when tests were made in high-pressure hydrogen. Stressed titanium-aluminum alloys also were cracked by bombardment with hydrogen ions produced in a proton accelerator. The approximate concentrations of the hydrogen ions in the alloys were calculated.

Ondrejcin, R. S.↗

NASA NTRS1973

Quantitative observations of hydrogen-induced, slow crack growth in a low alloy steel

Hydrogen-induced slow crack growth, da/dt, was studied in AISI-SAE 4130 low alloy steel in gaseous hydrogen and distilled water environments as a function of applied stress intensity, K, at various temperatures, hydrogen pressures, and alloy strength levels. At low values of K, da/dt was found to exhibit a strong exponential K dependence (Stage 1 growth) in both hydrogen and water. At intermediate values of K, da/dt exhibited a small but finite K dependence (Stage 2), with the Stage 2 slope being greater in hydrogen than in water. In hydrogen, at a constant K, (da/dt) sub 2 varied inversely with alloy strength level and varied essentially in the same complex manner with temperature and hydrogen pressure as noted previously. The results of this study provide support for most of the qualitative predictions of the lattice decohesion theory as recently modified by Oriani. The lack of quantitative agreement between data and theory and the inability of theory to explain the observed pressure dependence of slow crack growth are mentioned and possible rationalizations to account for these differences are presented.

Nelson, H. G.↗

NASA NTRS1974

Trapping of hydrogen atoms in X-irradiated salts at room temperature and the decay kinetics

The salts (hypophosphites, formates, a phosphite, a phosphate, and an oxalate) were X-irradiated, whereby hydrogen formed chemically by a radiolytic process becomes trapped in the solid. By room temperature vacuum extraction, the kinetics for the evolution of this trapped hydrogen was studied mass spectrometrically. All salts except two exhibited second-order kinetics. The two exceptions (NaH2PO2(H2O) and K2HPO4) showed first-order kinetics. Based on experimental results, the escape of hydrogen involves three steps: the diffusion of hydrogen atoms from the bulk to the surface, association of these atoms on the surface (rate controlling step for second-order hydrogen evolution), and the desorption of molecular hydrogen from the surface. The hydrogen does not escape if the irradiated salt is stored in air, apparently because adsorbed air molecules occupy surface sites required in the escape mechanism.

May, C. E.↗

NASA NTRS1974

Compact hydrogenator

The development and characteristics of a hydrogenating apparatus are described. The device consists of a reaction chamber which is selectively permeable to atomic hydrogen and catalytically active to a hydrogenating reaction. In one device, hydrogen is pumped out of the reaction chamber while the reactant remains inside to remove molecular hydrogen so that more atomic hydrogen can pass through the walls. In another device, the reactant is pumped through the reaction chamber, and the hydrogen is removed from the material leaving the chamber. The reactant is then cycled through the chamber.

Simmonds, P. G.↗

NASA NTRS1975

Effect of hydrogen on the mechanical properties of titanium and its alloys

Occluded hydrogen resulting from cathodic charging of commercially pure titanium and titanium alloys, Ti-8Al-1Mo-1V and Ti-6Al-4V, was shown to cause embrittlement of the alloys. Embrittlement was a function of the interstitial hydrogen content rather than the amount of precipitated titanium hydride. The effects of hydrogen concentration on the critical strain for plastic instability along pure shear directions was determined for alloys Ti-8Al-1Mo-1V and Ti-5Al-2.5Sn. Hydrogen, in concentrations below that necessary for spontaneous hydride precipitation, increased the strain necessary for instability formation or instability failure. The strain rate sensitivity also increased with increasing hydrogen concentration. The effect of hydrogen on slip and twinning was determined for titanium single crystals. The critical resolved shear stress for prism slip was increased and the critical resolved shear stress for twinning was decreased with increasing hydrogen concentration.

Beck, F. H.↗

NASA NTRS1975

Hydrogen-environment embrittlement of metals and its control

Types of hydrogen embrittlement are discussed together with characteristics of hydrogen-environment embrittlement, the degree of hydrogen-environment embrittlement of a wide variety of alloys, the effect of hydrogen environments on various properties, (tension, fatigue, creep and fracture mechanics), and the influence of hydrogen exposure parameters on the degree of embrittlement. Design methods for high-pressure hydrogen service and for prevention of hydrogen-environment embrittlement are also covered.

Chandler, W. T.↗