Analysis of degraded hydrogen dissociation envelopes by AES
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Ritz, V. H.↗
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An investigation of the effect of surface impurities on the adsorption kinetics of hydrogen chemisorbed onto iron
The goal was to develop an understanding of heterogeneous kinetic processes for those molecular species which produce gaseous hydrogen degradation of the mechanical properties of metallic structural materials. Although hydrogen degradation of metallic materials is believed to result from dissolved protonic hydrogen, the heterogeneous hydrogen interface transport processes often dominate the kinetics of the degradation process. The initial step in the interface transport process is the dissociative chemisorption of the molecular species at the metal surface followed by hydrogen absorption into and transport through the bulk. Modern advanced aerospace applications often require the use of structural materials in high pressure hydrogen environments at temperatures which range from low cryogenic temperatures to very high temperatures (1300 K and greater). Materials proposed for these applications, such as the titanium aluminides, beta-titanium alloys, nickel- and cobalt-based superalloys, molybdenum-rhenium alloys, beryllium, and various beryllides, need to possess a high degree of immunity from hydrogen induced degradation of mechanical properties. In the present program, the interaction of hydrogen with the surfaces of alpha-2 (Ti3Al) titanium aluminide, gamma (TiAl) titanium aluminide, and beryllium were studied. The interaction of low pressure hydrogen with gamma titanium aluminide and beryllium was found to be relatively weak, in the sense that adsorption leads to a low surface concentration of dissociated hydrogen, i.e., the chemisorption process is reversible at room temperature (300 K) for gamma titanium aluminide and the sticking coefficient for chemisorption is extremely small for beryllium. Hydrogen was found to interact readily with alpha-2 titanium aluminide to form a stable surface hydride at 300 K. These results correlate well with other recent studies which show that the mechanical properties for alpha-2 titanium aluminide are readily degraded in hydrogen while gamma titanium aluminide exhibits less degradation and beryllium essentially no degradation. The interaction of oxygen with the surface of these materials has been studied, also, in the present program.
Shanabarger, Mickey R.↗
An investigation of the effect of surface impurities on the adsorption kinetics of hydrogen chemisorbed onto iron
The goal of this program was to develop an understanding of heterogeneous kinetic processes for those molecular species which produce gaseous hydrogen degradation of the mechanical properties of metallic structural materials. Although hydrogen degradation of metallic materials is believed to result from dissolved protonic hydrogen, the heterogeneous hydrogen interface transport processes often dominate the kinetics of degradation. The initial step in the interface transport process is the dissociative chemisorption of the molecular species at the metal surface followed by hydrogen absorption into and transport through the bulk. The interaction of hydrogen with the surfaces of alpha-2(Ti3Al) titanium aluminide, gamma(TiAl) titanium aluminide, and beryllium were studied.
Shanabarger, Mickey R.↗
Hot Hydrogen Exposure Degradation of the Strength of Mullite
This study deals with the corrosion of near stoichiometric mullite (3Al2O3-2SiO2) by pure dry hydrogen gas. Exposure of the mullite samples was at temperatures of 1050 and 1250 C for times up to 500 hours. Preferential attack of the alumino-silicate glass present in the grain boundaries of the mullite occurred after 125 hours at 1250 C. Hydrogen scrubbing of the SiO2 from the glassy grain boundaries and the mullite grains yielded a porous alumina-rich surface. The room temperature strength increased after short exposure times at 1250 C (up to 125 hours), then decreased by 53 percent after exposure for 500 hours. At 1050 C, all exposure times (25 to 500 hours) decreased the strength. After 500 hours in hydrogen at 1050 C, the room temperature strength of mullite decreased 22 percent. We also observed a rapid 25 percent strength loss after short exposure times at 1050 C. This is attributed to the calcium/hydrogen assisted crystallization of the glassy, grain-boundary phase.
Herbell, Thomas P.↗
On the line Q degradation in hydrogen masers
In hydrogen masers, the atomic resonance quality factor is largely determined by the properties of the Teflon coating on the quartz storage bulb. Normally a good Teflon coating will last many years. On the other hand, there may be a relatively fast degradation of the quality factor if the Teflon coating is bad. A series of observations and measurements performed on an hydrogen maser that had successively a bad and a good Teflon coating are discussed.
Bernier, L. G.↗
An investigation of the effect of surface impurities on the adsorption kinetics of hydrogen chemisorbed onto iron
The goal of this program has been to develop an understanding of heterogeneous kinetic processes for those molecular species which produce gaseous hydrogen degradation of the mechanical properties of metallic structural materials. During the present program, the interaction of hydrogen with the surfaces of alpha-2 (Ti3Al) titanium aluminide, gamma (TiAl) titanium aluminide, and beryllium were studied. The interaction of low pressure hydrogen with gamma titanium aluminide and beryllium was found to be relatively weak. Weak in the sense that adsorption leads to a low surface concentration of dissociated hydrogen, i.e., the chemisorption process is reversible at room temperature (300 K) for gamma titanium aluminide and the sticking coefficient for chemisorption is extremely small for beryllium. Hydrogen was found to interact readily with alpha-2 titanium aluminide to form a stable surface hydride at 300 K. These results correlate well with other recent studies which show that the mechanical properties for alpha-2 titanium aluminide are readily degraded in hydrogen while gamma titanium aluminide exhibits less degradation and beryllium essentially no degradation. The interaction of oxygen with the surface of several of these materials was studied. More recently, preliminary hydrogen permeation studies were completed for three high temperature alloys, Incoloy 909, Mo-47.5Re (wt. %), and this past year, Haynes 188.
Shanabarger, Mickey R.↗
Atmospheric degradation mechanisms of hydrogen containing chlorofluorocarbons (HCFC) and fluorocarbons (HFC)
The current knowledge of atmospheric degradation of hydrogen containing chlorofluorocarbons (HCFC 22 (CHClF2), HCFC 123 (CHCl2CF3), HCFC 124 (CHClFCF3), HCFC 141b (CFCl2CH3), HCFC 142b (CF2ClCH3)) and fluorocarbons (HFC 125 (CHF2CF3), HFC 134a (CH2FCF3), HFC 152a (CHF2CH3)) is assessed. Except for the initiation reaction by OH radicals, there are virtually no experimental data available concerning the subsequent oxidative breakdown of these molecules. However, from an analogy to the degradation mechanisms of simple alkanes, some useful guidelines as to the expected intermediates and final products can be derived. A noteable exception from this analogy, however, appears for the oxi-radicals. Here, halogen substitution induces new reaction types (C-Cl and C-C bond ruptures) which are unknown to the unsubstituted analogues and which modify the nature of the expected carbonyl products. Based on an evaluation of these processes using estimated bond strength data, the following simplified rules with regards to the chlorine content of the HCFC's may be deduced: (1) HCFC's containing one chlorine atom such as 22 and 142b seem to release their chlorine content essentially instantaneous with the initial attack on the parent by OH radicals, and for HCFC 124, such release is apparently prevented; (2) HCFC's such as 123 and 141b with two chlorine atoms are expected to release only one of these instantaneously; and the second chlorine atom may be stored in potentially long-lived carbonyl compounds such as CF3CClO or CClFO.
Zellner, Reinhard↗
Hydrogen Embrittlement
Hydrogen embrittlement (HE) is a process resulting in a decrease in the fracture toughness or ductility of a metal due to the presence of atomic hydrogen. In addition to pure hydrogen gas as a direct source for the absorption of atomic hydrogen, the damaging effect can manifest itself from other hydrogen-containing gas species such as hydrogen sulfide (H2S), hydrogen chloride (HCl), and hydrogen bromide (HBr) environments. It has been known that H2S environment may result in a much more severe condition of embrittlement than pure hydrogen gas (H2) for certain types of alloys at similar conditions of stress and gas pressure. The reduction of fracture loads can occur at levels well below the yield strength of the material. Hydrogen embrittlement is usually manifest in terms of singular sharp cracks, in contrast to the extensive branching observed for stress corrosion cracking. The initial crack openings and the local deformation associated with crack propagation may be so small that they are difficult to detect except in special nondestructive examinations. Cracks due to HE can grow rapidly with little macroscopic evidence of mechanical deformation in materials that are normally quite ductile. This Technical Memorandum presents a comprehensive review of experimental data for the effects of gaseous Hydrogen Environment Embrittlement (HEE) for several types of metallic materials. Common material screening methods are used to rate the hydrogen degradation of mechanical properties that occur while the material is under an applied stress and exposed to gaseous hydrogen as compared to air or helium, under slow strain rates (SSR) testing. Due to the simplicity and accelerated nature of these tests, the results expressed in terms of HEE index are not intended to necessarily represent true hydrogen service environment for long-term exposure, but rather to provide a practical approach for material screening, which is a useful concept to qualitatively evaluate the severity of hydrogen embrittlement. The effects of hydrogen gas on mechanical properties such as tensile strength, ductility, fracture, low and high cycle fatigue, crack growth rate, and creep rupture are analyzed with respect to the general trends established from the HEE index values. It is observed that the severity of HE effects is also influenced by environmental factors such as pressure, temperature, and hydrogen gas purity. The severity of HE effects is also influenced by material factors such as surface finish, heat treatment, and product forms, compositions, grain direction, and crystal orientations.
Jonathan A. Lee↗
Hot Hydrogen Testing of Refractory Metals and Ceramics
The objective of this investigation is to develop a technique with which refractory metal carbide samples can be exposed to hydrogen containing gases at high temperatures, and to use various microstructural and analytical techniques to determine the chemical and rate processes involved in hydrogen degradation in these materials. Five types of carbides were examined including WC, NbC, HfC, ZrC, and TaC. The ceramics were purchased and were all monolithic in nature. The temperature range investigated was from 850 to 1600 C with a hydrogen pressure of one atmosphere. Control experiments, in vacuum, were also conducted for comparison so that the net effects due to hydrogen could be isolated. The samples were analyzed prior to and after exposure. Gas samples were collected in selected experiments and analyzed using gas chromography. Characterization of the resulting microstructure after exposure to hydrogen was conducted using optical microscopy, x-ray diffraction, scanning electron microscopy, and weight change. The ceramics were purchased and were all monolithic in nature. It was found that all samples lost weight after exposure, both in hydrogen and vacuum. Results from the microstructure analyses show that the degradation processes are different among the five types of ceramics involved. In addition, the apparent activation energy for the degradation process is a function of temperature even within the same material. This indicates that there are more than one mechanism involved in each material, and that the mechanisms are temperature dependent.
Zee, Ralph↗
Status of SAFT silver hydrogen cell development
Nickel-hydrogen cells appear to be an improvement over the nickel-cadmium in applications requiring longer lifetime and reduced weight. An even more efficient couple, the silver-hydrogen couple, is also considered. After a theoretical study first performed by the Battelle Institute of Geneva under ESA (European Space Agency) contract, SAFT has undertaken more detailed analyses of the silver-hydrogen degradation mechanisms. ESA and the French Department of Defense contracted with SAFT for a full-development program of the silver-hydrogen technology.
Goualard, B. J.↗
An Investigation of the Effect of Surface Impurities on the Adsorption Kinetics of Hydrogen Chemisorbed onto Iron
The original goal of this program was to investigate the effect surface impurities have on the heterogeneous kinetic processes of those molecular species which produce gaseous hydrogen degradation of the mechanical properties of metallic structural materials. However, shortly after the initiation of the original program, the program's NASA Technical Monitor, Dr. Howard Nelson, requested that the effort supported by this Co-operative Agreement be redirected to study more pressing materials issues associated to the development of the National Aero-Space Plane (NASP). The results of these efforts are outlined in this report. Detailed discussions of specific work, including experimental techniques and procedures, will be found in the publications listed with the subsection discussing that specific work as well and in Section 5. No inventions were generated or disclosed within this Agreement.
Shanabarger, M. R.↗
An Investigation of the Effect of Surface Impurities on the Adsorption Kinetics of Hydrogen Chemisorbed onto Iron
The original goal of this program was to investigate the effect surface impurities have on the heterogeneous kinetic processes of those molecular species which produce gaseous hydrogen degradation of the mechanical properties of metallic structural materials. However, shortly after the initiation of the original program, the program's NASA Technical Monitor, Dr. Howard Nelson, requested that the effort supported by this Co-operative Agreement be redirected to study more pressing materials issues associated to the development of the National Aero-Space Plane (NASP). The results of these efforts are outlined in this report. Detailed discussions of specific work, including experimental techniques and procedures, will be found in the publications listed with the subsection discussing that specific work as well and in Section 5. No inventions were generated or disclosed within this Agreement.
Shanabarger, R. M.↗
Low noise buffer amplifiers and buffered phase comparators for precise time and frequency measurement and distribution
Extremely low noise, high performance, wideband buffer amplifiers and buffered phase comparators were developed. These buffer amplifiers are designed to distribute reference frequencies from 30 KHz to 45 MHz from a hydrogen maser without degrading the hydrogen maser's performance. The buffered phase comparators are designed to intercompare the phase of state of the art hydrogen masers without adding any significant measurement system noise. These devices have a 27 femtosecond phase stability floor and are stable to better than one picosecond for long periods of time. Their temperature coefficient is less than one picosecond per degree C, and they have shown virtually no voltage coefficients.
Eichinger, R. A.↗
Development of Laser Powder Bed Fusion NASA HR-2 for Hydrogen Sensitive Liquid Rocket Engine Applications
The National Aeronautics and Space Administration (NASA) has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. AM has provided new design and manufacturing opportunities to reduce cost and schedule, consolidate parts, and optimize performance. Laser Powder Bed Fusion (L-PBF) is one of the most commonly used AM processes to fabricate components that have complex shape and need fine feature resolution. Due to exposure to high pressure gaseous hydrogen, mechanical property degradation caused by hydrogen environment embrittlement (HEE) is a critical concern for many materials in liquid hydrogen propulsion systems. NASA has identified the need to develop and advance new materials in unique engine applications using liquid hydrogen as a propellant. One such material being developed at NASA Marshall Space Flight Center is L-PBF NASA HR-2 (Hydrogen Resistant-2), a high-strength Fe-Ni-based superalloy resistant to HEE. The chemistry of NASA HR-2 was formulated to meet requirements for key liquid rocket engine (LRE) components that operate in high-pressure hydrogen environments. Initial development and material characterization found NASA HR-2 has excellent L-PBF printability and its microstructure evolves well after heat treatment. This new alloy has undergone fundamental metallurgical evaluations, heat treatment studies, detailed microstructure characterization, and mechanical testing across a range of temperatures. Tensile testing was performed in pressurized gaseous hydrogen (GH2) environment to assess its resistance to HEE. L-PBF NASA HR-2 has an average yield stress of 95 ksi, ultimate tensile stress of 165 ksi, and very high fracture elongation at 34 - 36% when tested in a 5 ksi high pressure hydrogen environment. The tensile property data confirms hydrogen has little influence on its ductility, strength, and fracture behavior. L-PBF NASA HR-2 is a promising option for many hydrogen sensitive LRE components that require exceptional resistance to HEE. The development of L-PBF NASA HR-2 is funded under the grants provided by Jacobs TIPI program and the Liquid Engine Office at NASA Marshall Space Flight Center. This paper will provide an overview of the L-PBF process development, material characterization, mechanical and thermophysical properties, and LRE hardware development for NASA HR-2.
NASA HR-2↗
Development of Laser Powder Bed Fusion NASA HR-2 for Hydrogen Sensitive Liquid Rocket Engine Applications
The National Aeronautics and Space Administration (NASA) has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. AM has provided new design and manufacturing opportunities to reduce cost and schedule, consolidate parts, and optimize performance. Laser Powder Bed Fusion (L-PBF) is one of the most commonly used AM processes to fabricate components that have complex shape and need fine feature resolution. Due to exposure to high pressure gaseous hydrogen, mechanical property degradation caused by hydrogen environment embrittlement (HEE) is a critical concern for many materials in liquid hydrogen propulsion systems. NASA has identified the need to develop and advance new materials in unique engine applications using liquid hydrogen as a propellant. One such material being developed at NASA Marshall Space Flight Center is L-PBF NASA HR-2 (Hydrogen Resistant-2), a high-strength Fe-Ni-based superalloy resistant to HEE. The chemistry of NASA HR-2 was formulated to meet requirements for key liquid rocket engine (LRE) components that operate in high-pressure hydrogen environments. Initial development and material characterization found NASA HR-2 has excellent L-PBF printability and its microstructure evolves well after heat treatment. This new alloy has undergone fundamental metallurgical evaluations, heat treatment studies, detailed microstructure characterization, and mechanical testing across a range of temperatures. Tensile testing was performed in pressurized gaseous hydrogen (GH2) environment to assess its resistance to HEE. L-PBF NASA HR-2 has an average yield stress of 95 ksi, ultimate tensile stress of 165 ksi, and very high fracture elongation at 34 - 36% when tested in a 5 ksi high pressure hydrogen environment. The tensile property data confirms hydrogen has little influence on its ductility, strength, and fracture behavior. L-PBF NASA HR-2 is a promising option for many hydrogen sensitive LRE components that require exceptional resistance to HEE. The development of L-PBF NASA HR-2 is funded under the grants provided by Jacobs TIPI program and the Liquid Engine Office at NASA Marshall Space Flight Center. This paper will provide an overview of the L-PBF process development, material characterization, mechanical and thermophysical properties, and LRE hardware development for NASA HR-2.
NASA HR-2↗
Development of Laser Powder Bed Fusion NASA HR-2 for Hydrogen Sensitive Liquid Rocket Engine Applications
The National Aeronautics and Space Administration (NASA) has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000s. AM has provided new design and manufacturing opportunities to reduce cost and schedule, consolidate parts, and optimize performance. Laser Powder Bed Fusion (L-PBF) is one of the most commonly used AM processes to fabricate components of complex shape requiring fine feature resolution. Due to exposure to high-pressure gaseous hydrogen, mechanical property degradation caused by hydrogen environment embrittlement (HEE) is a critical concern for many materials in liquid hydrogen propulsion systems. NASA has identified the need to develop and advance new materials in unique engine applications using liquid hydrogen as a propellant. One such material being developed at NASA Marshall Space Flight Center is L-PBF NASA HR-2 (Hydrogen Resistant-2), a high-strength Fe-Ni-based superalloy resistant to HEE. The chemistry of NASA HR-2 was formulated to meet requirements for key liquid rocket engine (LRE) components that operate in high-pressure hydrogen environments. Initial development and material characterization found that NASA HR-2 has excellent L-PBF printability, and its microstructure evolves well after heat treatment. This new alloy has undergone fundamental metallurgical evaluations, heat treatment studies, detailed microstructure characterization, and mechanical testing across a range of temperatures. Tensile testing was performed in a pressurized gaseous hydrogen (GH2) environment to assess its resistance to HEE. L-PBF NASA HR-2 has an average yield stress of 95 ksi, an ultimate tensile stress of 165 ksi, and a very high fracture elongation of 34 - 36% when tested in a high-pressure (5 ksi) hydrogen environment. The tensile property data confirms hydrogen has little influence on HR-2’s ductility, strength, and fracture behavior. L-PBF NASA HR-2 is a promising option for many hydrogen-sensitive LRE components that require exceptional resistance to HEE. This paper will provide an overview of the L-PBF process development, material characterization, mechanical and thermophysical properties, and LRE hardware development for NASA HR-2.
Po S Chen↗
Study of Capacity and Voltage Degradation in Nickel-Hydrogen Cells
The objective of this study is to understand the causes of the nickel hydrogen (NiH2) cell degradetion: storage, cycling, and reversal.
Vaidyanathan, Hari↗
Creep-rupture behavior of seven iron-base alloys after long term aging at 760 deg in low pressure hydrogen
Seven candidate iron-base alloys for heater tube application in the Stirling automotive engine were aged for 3500 hours at 760 C in argon and hydrogen. Aging degraded the tensile and creep-rupture properties. The presence of hydrogen during aging caused additional degradiation of the rupture strength in fine grain alloys. Based on current design criteria for the Mod 1 Stirling engine, N-155 and 19-9DL are considered the only alloys in this study with strengths adequate for heater tube service at 760 C.
Witzke, W. R.↗