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Spark emission spectroscopy analyzes surface contamination of metals. This technique controls the quality of surface preparations and is useful in fundamental investigations of surface properties of metals.
The isothermal kinetics of H2, H2S, and O2 chemisorption onto epitaxially grown (III) oriented Fe films were studied. The measurements were made using the techniques of chemisorption induced resistance change and Auger electron spectroscopy (for adsorbed sulfur and oxygen). Also the origin of the chemisorption induced resistance change for these systems and its applicability to kinetic measurements were established. The chemisorption kinetics were interpreted as dissociative chemisorption via an adsorbed molecular species. The applicable rate constants were established. In none of the studies were the rate constants observed to be coverage dependent. By comparing the temperature dependence of the rate constants with absolute rate theory, the binding energies and activation energies of all the kinetic processes were obtained for the H2/Fe system. The initial sticking coefficient was pressure dependent for both the H2/Fe and H2S/Fe systems. This results from the step between the adsorbed molecular state and the dissociated chemisorbed state being the rate limiting step for absorption at certain pressures and temperatures. Estimates were obtained for the temperature dependence of the rate constants for the O2/Fe system.
(Previously announced in Star as N83-173335)
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Explore the source record for details and available documents.
Explore the source record for details and available documents.
When working with high concentrations of hydrogen peroxide, it is critical that the storage container be constructed of the proper materials, those which will not degrade to the extent that container breakdown or dangerous decomposition occurs. It has been suggested that the only materials that will safely contain the peroxide for a significant period of time are metals of stainless steel construction or aluminum use as High Test Hydrogen Peroxide (HTP) Containers. The stability and decomposition of HTP will be also discussed as well as various means suggested in the literature to minimize these problems. The dangers of excess oxygen generation are also touched upon.
Metal outgassing currently limits the pressures attained in vacuum chambers. The dominant residual gas in a carefully degassed metal system is usually hydrogen. The atomic hydrogen within bulk metals could be removed by diffusion processes if surface effects did not interfere. It is proposed that removing the surface hydrogen during vacuum bakeout by continuous electron bombardment (or similar irradiation) would allow the diffusion to proceed and lead to lower outgassing rates and operating pressures.
The effect of high pressure hydrogen on the crack growth rate of various nickel-base alloys was studied at ambient temperature. Considerable enhancement of the cyclic flaw growth rate was observed for Inconel 718, wrought and cast, and Waspaloy, a nickel-base alloy similar to Inconel 718. Only slight enhancement of the flaw growth rate for Alloy 903 was observed.
Current practices and future requirements for the storage, transmission and distribution of hydrogen are reviewed in order to identify inadequacies to be corrected before hydrogen can achieve its full potential as a substitute for fossil fuels. Consideration is given to the storage of hydrogen in underground solution-mined salt caverns, portable high-pressure containers and dewars, pressure vessels and aquifers and as metal hydrides, hydrogen transmission in evacuated double-walled insulated containers and by pipeline, and distribution by truck and internal distribution networks. Areas for the improvement of these techniques are indicated, and these technological deficiencies, including materials development, low-cost storage and transmission methods, low-cost, long-life metal hydrides and novel methods for hydrogen storage, are presented as challenges for research and development.
Mossbauer effect study of hydrogen adsorption onto metal surface by cathodic charging
It is shown that while MgII k line emission decreases for metal deficient stars, the Ly alpha emission increases. The sum of chromospheric hydrogen and metallic emission appears to be independent of metal abundances. The total chromospheric energy loss is estimated to be 0.0004 F sub bol. The chromospheric energy input does not seem to decrease for increasing age. The transition layer emission is reduced for metal deficient stars, but it is not known whether the reduction is larger than can be explained by curve of growth effects only. Coronal X-ray emission was measured for 4 metal deficient stars. Within a 12 limit it could still be consistent with the emission of solar abundance stars.
The utilization of a cold plasma in chlorination processing is described. Essential equipment and instruments were received, the experimental apparatus assembled and tested, and preliminary experiments conducted. The results of the latter lend support to the original hypothesis: a cold plasma can both significantly enhance and bias chemical reactions. In two separate experiments, a cold plasma was used to reduce TiCl4 vapor and chlorinate ilmenite. The latter, reacted in an argon-chlorine plasma, yielded oxygen. The former experiment reveals that chlorine can be recovered as HCl vapor from metal chlorides in a hydrogen plasma. Furthermore, the success of the hydrogen experiments has lead to an analysis of the feasibility of direct hydrogen reduction of metal oxides in a cold plasma. That process would produce water vapor and numerous metal by-products.
Direct optical observations of solid hydrogen to pressures in the 250-gigapascal range at 77 K are reported. Hydrogen samples appear nearly opaque at the maximum pressures. Measurements of absorption and Raman spectra provide evidence that electronic excitations in the visible region begin at about 200 gigapascals. The optical data are consistent with a band-overlap mechanism of metallization.
Apparatus exposes hot metal specimens in hydrogen atmospheres to sudden cooling. Heater surrounds pressure vessel initially. On command, heater slides downward on track, exposing vessel. Spray bar falls over vessel and directs high-pressure jets of cold water at it. Developed to evaluate susceptibilities of specimens to embrittlement by hydrogen. Cools specimens by 1,050 degrees F (580 degrees C) in 160 seconds.
Two electrochemical methods for the determination of hydrogen concentrations in metals are discussed and evaluated. The take-up of hydrogen at a pressure of 5000 psi by Waspaloy metal was determined experimentally at 24 C. It was found that the metal becomes saturated with hydrogen after an exposure time of about 1 hr. For samples charged with hydrogen at high pressure, most of the hydrogen is contained in the interstitial solid solution of the metal. For electrolytically charged samples, most of the hydrogen is contained as surface and subsurface hydrides. Hydrogen elimination rates were determined for these two cases, with the rate for electrolytically charged samples being greater by over a factor of two. Theoretical effects of high temperature and pressure on hydrogen take-up and elimination by bare and gold plated Waspaloy metal was considered. The breakthrough point for hydrogen at 5000 psi, determined experimentally, lies between a gold thickness of 0.0127 mm (0.0005 in.) and 0.0254 mm (0.001 in.) at 24 C. Electropolishing was found to greatly reduce the uptake of hydrogen at high pressure by Waspaloy metal at 24 C. Possible implications of the results obtained, as they apply to the turbine disk of the space shuttle main engine, are discussed.
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.
A particularly simple conversion of a scanning Auger system for ESD ion energy distributions and scanning ESD has been developed. This approach combines the advantages of the small spot-size electron guns and mapping systems developed for SAM with the capability of ESD for the detection of hydrogen. Our intended use for the device is detection and mapping of surface concentrations of hydrogen on metals. The characteristics of SESD are illustrated with the preliminary results of an investigation into the ESD properties of hydrogenic adsorbates on Nb. It is shown that the ESDIED exhibit distinct differences indicative of the surface preparation, and that the ESD ion angular distributions have an effect on the observed contrast relationships in SESD.