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Vapor-exposure test cell (VETC) designed to be used in testing thin-film electrodes on solid electrolytes electrochemically at high temperature. Use of VETC much simpler and less expensive than testing alkali-metal thermal-to-electric converter (AMTEC) fuel cell, electrolysis cell, or other entire device containing solid electrolyte and electrodes of material and configuration to be characterized.
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Previous work reported from JPL has included characterization of electrode kinetics and alkali atom transport from electrodes including Mo, W, WRh(sub x), WPt(sub x)(Mn), in sodium AMTEC cells and vapor exposure cells, and Mo in potassium vapor exposure cells. These studies were generally performed in cells with small area electrodes (about 1 to 5 cm(sup 2)), and device geometry had little effect on transport. Alkali diffusion coefficients through these electrodes have been characterized, and approximate surface diffusion coefficients derived in cases of activated transport. A basic model of electrode kinetic at the alkali metal vapor/porous metal electrode/alkali beta'-alumina solid electrolyte three phase boundary has been proposed which accounts for electrochemical reaction rates with a collision frequency near the three phase boundary and tunneling from the porous electrode partially covered with adsorbed alkali metal atoms. The small electrode effect in AMTEC cells has been discussed in several papers, but quantitative investigations have described only the overall effect and the important contribution of electrolyte resistance. The quantitative characterization of transport losses in cells with large area electrodes has been limited to simulations of large area electrode effects, or characterization of transport losses from large area electrodes with significant longitudinal temperature gradients. This paper describes new investigations of electrochemical kinetics and transport, particularily with WPt(sub 3.5) electrodes, including the influence of electrode size on the mass transport loss in the AMTEC cell. These electrodes possess excellent sodium transport properties making verification of device limitations on transport much more readily attained.
Previous work reported from JPL has included characterization of electrode kinetics and alkali atom transport from electrodes including Mo, W, WRh x (Mn), in sodium AMTEC cells and vapor exposure cells; and Mo in potassium vapor exposure cells. These studies were generally performed in cells with small area electrodes (about 1 to 5 cm 2 ), and device geometry had little effect on transport. Alkali metal diffusion coefficients through these electrodes have been characterized, and approximate surface diffusion coefficients were derived in cases of activated transport. A basic model of electrode kinetics and transport at the alkali metal vapor/pourous metal electrode/alkali beta"-alumina solid electrolyte (BASE) three phase boundary has been proposed which accounts for electrochemical reaction rates with a collision frequency near the three phase boundary and tunneling from the porous electrode partially covered with adsorbed alkali metal atoms. The small electrode effect in AMTEC cells has been discussed in several papers, but quantitative investigations have described only the overall effect and the important contribution of electrolyte resistance. The quantitative characterization of transport losses in cells with large area electrodes has been limited to simulations of large area electrode effects, or characterization of transport losses from large area electrodes with significant longitudinal temperature gradients. This paper describes new investigations of electrochemical kinetics and transport, with four 14.4 cm 2 WPt 3.5 electrodes, including the influence of electrode size on the mass transport loss in the AMTEC cell. These electrodes exhibit very slow sintering, as well as excellent sodium transport properties, making them attractive candidates for AMTEC power conversion use. However, the facile sodium transport in WPt 3.5 electrodes makes characterization of the transport process difficult.
A simple pharmacokinetic model and a specially designed dermal vapor exposure chamber which provides respiratory protection were used to determine the rate of penetration of hydrazine and 1,1-dimethylhydrazine (UDMH) vapor through the skin of rats. Parameters for the pharmacokinetic model were determined from intravenous and inhalation exposure data. The model was then used to estimate the skin permeation coefficient for hydrazine or UDMH vapor from the dermal-vapor exposure data. This analysis indicates that UDMH vapor has a relatively high permeability through skin (0.7 cm/hr), a value somewhat higher than was obtained for hydrazine by the same procedure (0.09 cm/hr). Based on these skin permeability results, a skin-only vapor exposure limit giving protection equivalent to the inhalation Threshold Limit Value (TLV) could be calculated. The current TLV's for UDMH and hydrazine are 0.5 and 0.1 ppm, respectively. The corresponding skin-only TLV equivalents, for personnel wearing respiratory protection, are 32 ppm for UDMH and 48 ppm for hydrazine. Should the proposed lowering to the TLV's for these compounds to 0.01 ppm be adopted, the equivalent skin-only TLV's would become 0.64 ppm for UDMH and 4.8 for hydrazine.
Thermal control coating samples were subjected to cesium ion beam and vapor exposures. Degradation of solar absorptance and infrared emittance were measured. Solar cells and samples selected from surfaces on the ATS-F spacecraft likely to experience ion or vapor impingement were bombarded by 10-volt cesium ions. Other samples were subjected to high levels of cesium vapor. Aluminum and white paint were backsputtered by 550-volt cesium ions onto selected samples. For direct bombardment, the threshold for ion-induced property changes was above five-thousand trillion ions/sq cm. With material sputtered from a 450-sq cm target onto samples 36 cm distant, the threshold for noticeable effects was above 5 times 10 to the 17-th power ions/sq cm.
The influence of substrate imperfections on the nucleation and growth of fcc metals on alkali halides is discussed. Films deposited on well characterized substrated under well defined vacuum evaporation conditions are investigated. The experimental results of this work are correlated with similar work by other investigators. Models which have been proposed by various authors to explain experimental results are critically examined and areas of difficulty are pointed out. The influence of defects on nucleation rate and the orientation of the film is emphasized. Specific examples of impurity effects, irradiation effects and the influence of amorphous layers are discussed in detail. Evidence is shown that the formation of multiply twinned particles is a result of coalescence and growth. The only consistent model for the orienting influence of impurities is shown to be a chemical reaction effect. It is demonstrated that an alkali metal impurity is very likely responsible for the orienting influence of both water vapor exposure and irradiation. A negative result is found for the reported possibility of an orienting influence being transmitted through an amorphous layer.
For many years the metalworking industry has cleaned metal and composite substrates with chlorinated solvents. Recently, however, health and disposal related environmental concerns have increased regarding chlorinated solvents, including 1,1,1-trichloroethane, trichloroethylene, methylene chloride, or Freon'. World leaders have instituted a production ban of certain ozone depleting chlorofluorocarbons (CFC's) by 1996. The Occupational Safety and Health Administration (OSHA) has instituted worker vapor exposure limitations for virtually all of the solvents used in solvent-based cleaners. In addition, the United States Environmental Protection Agency (EPA) has defined nearly all solvent-based cleaners as 'hazardous'. Cradle to grave waste responsibility is another reason manufacturers are trying to replace chlorinated solvents in their cleaning processes. Because of these factors, there now is a world wide effort to reduce and/or eliminate the use of chlorinated solvents for industrial cleaning. Waterbased cleaners are among the alternatives being offered to the industry. New technology alkaline cleaners are now available that can be used instead of chlorinated solvents in many cleaning processes. These waterbased cleaners reduce the release of volatile organic compounds (VOC's) by as much as 99 percent. (The definition and method of calculation of VOC's now varies from region to region.) Hazardous waste generation can also be significantly reduced or eliminated with new aqueous technology. This in turn can ease worker exposure restrictions and positively impact the environment. This paper compares the chemical and physical properties of this aqueous cleaners versus chlorinated solvents.
In order to model the lifetime of the electrochemical cell in an Alkali Metal Thermal to Electric Converter (AMTEC), studies of TiN Electrodes on Beta-alumina solid electrolytes (BASE) have been made to determine the performace parameters over time. The first of a series of experiments in which TiN electrodes are studied in a Vapor Exposure Test Cell is described here, with preliminary results from electrochemical measurements made on the cell. The TiN electrodes tested here perform well, with minimal degradation over 1000 hours of operation at 850 degree C.
An experimental investigation was conducted to determine (1) the ground-hold and space-hold thermal performance of a multilayer insulation (MLI) system mounted on a spherical, liquid-hydrogen propellant tank and (2) the degradation to the space-hold thermal performance of the insulation system that resulted from both thermal cycling and exposure to moisture. The propellant tank had a diameter of 1.39 meters (4.57ft). The MLI consisted of two blankets of insulation; each blanket contained 15 double-aluminized Mylar radiation shields separated by double silk net spacers. Nineteen tests simulating basic cryogenic spacecraft thermal (environmental) conditions were conducted. These tests typically included initial helium purge, liquid-hydrogen fill and ground-hold, ascent, space-hold, and repressurization. No significant degradation of the space-hold thermal performance due to thermal cycling was noted.
Exposure of unprotected humans to altitudes above 63,000 ft results in ebullism. Ebullism occurs when the vapor pressure of tissues is less than the ambient pressure and the tissues spontaneously 'boil'. This may result in rapid unconsciousness, cardiac vaporlock, pulmonary collapse, cerebral anoxia, and sometimes even death. Potential places for this include EVA accidents in space, aircraft experiencing rapid decompression at high altitudes with cabin or pressure suit failure, and accidents during pressure suit training exercises. The pathophysiology of ebullism was studied in the 40's to 60's using animal models. There is one report of a prolonged, unprotected human exposure and several anecdotal of unprotected short term exposures to near vacuum. In addition to pulmonary and neurologic concerns, unprotected exposure of the head may result in freezing of the corneal surface of the eye. Surface eye freezing may impair vision and significantly impact mission completion. At this time, little data are available on the effectiveness of conventional treatment protocols, such as hyperbaric oxygen, for ebullism induced injuries. Research is needed to assess the efficacy of other adjunctive therapies such as high frequency ventilation and cerebral protective drugs that are still under development.
The permeation resistance of chlorinated polyethylene (CPE) used in chemical protective clothing against the aerospace fuels hydrazine, monomethylhydrazine (MMH), and uns-dimethylhydrazine (UDMH) was determined by measuring breakthrough times and time-averaged vapor transmission rates using an ASTM F 739 permeation cell. Two exposure scenarios were simulated: a 2 hour (h) fuel vapor exposure, and a liquid fuel "splash" followed by a 2 h vapor exposure. To simulate internal suit pressure during operation, a positive differential pressure of 0.3 in. water (75 Pa) on the collection side of the permeation apparatus was used. Breakthrough was observed after exposure to liquid MMH, and to vapor and liquid UDMH. No breakthrough was observed after exposure to vapor and liquid hydrazine, or vapor MMH. A model was then used to calculate propellant concentrations inside a totally encapsulating chemical protective suit based on the ASTM permeation data obtained in the present study. Concentrations were calculated under conditions of fixed vapor transmission rate, variable breathing air flow rate, and variable splash exposure area. Calculations showed that the maximum allowable permeation rates of hydrazine fuels through CPE were of the order of 0.05 to 0.08 ng sq cm/min for encapsulating suits with low breathing air flow rates (of the order of 5 scfm or 140 L/min). Above these permeation rates, the 10 parts per billion (ppb) threshold limit value time - weighted average could be exceeded for chemical protective suits having a CPE torso. To evaluate suit performance at ppb level concentrations, use of a sensitive analytical method such as cation exchange high performance liquid chromatography with amperometric detection was found to be essential.
Cooled target collection techniques and high pressure mass spectrometric sampling were used to measure the relative rates of oxidative vaporization and to identify the volatile products emanating from samples of chromia and Mg-doped lanthanum chromite. The materials were exposed to partial pressures of KCl with and without H2O in one atmosphere of slowly flowing oxygen at elevated temperatures. Chromia and fresh samples of lanthanum chromite exhibited enhanced rates of oxidative vaporization upon exposure to these reactants. Mass spectrometric identification showed that the enhancements resulted from the heterogeneous formation of complex molecules of the type KCl sub 1,2,3 CrO3 and KOH sub l,2 CrO3. Lanthanum chromite that had undergone prolonged oxidative vaporization exhibited no enhanced oxidation upon exposure to the reactants.
The permeation resistance of chlorinated polyethylene (CPE) used in totally encapsulating chemical protective suits against the aerospace fuels hydrazine, monomethylhydrazine, and uns-dimethylhydrazine was determined by measuring the breakthrough time (BT) and time-averaged vapor transmission rate (VTR) using procedures consistent with ASTM F 739 and ASTM F 1383. Two exposure scenarios were simulated: a 2 hour (h) fuel vapor exposure, and a liquid fuel "splash" followed by a 2 h vapor exposure. To simulate internal suit pressure during operation, a positive differential pressure of 0.3 in. water (75 Pa) on the collection side of the permeation apparatus was used. Using the available data, a model was developed to estimate propellant concentrations inside an air-line fed, totally encapsulating chemical protective suit. Concentrations were calculated under simulated conditions of fixed vapor transmission rate, variable breathing air flow rate, and variable splash exposure area. Calculations showed that the maximum allowable permeation rates of hydrazine fuels through CPE were of the order of 0.05 to 0.08 ng/sq cm min for encapsulating suits with low breathing air flow rates (of the order of 5 scfm or 140 L min-1). Above these permeation rates, the 10 parts-per-billion (ppb) threshold limit value time-weighted average could be exceeded. To evaluate suit performance at 10 ppb threshold-limiting value/time-weighted average level concentrations, use of a sensitive analytical method such as cation exchange high performance liquid chromatography with amperometric detection was found to be essential. The analytical detection limit determines the lowest measurable VTR, which in turn governed the lowest per meant concentration that could be calculated inside the totally encapsulating chemical protective suit.
Permeation resistance was determined by measuring the breakthrough time and time-averaged vapor transmission rate of monomethylhydrazine (MMH) through two types of personal protective equipment (PPE). The two types of PPE evaluated were the totally encapsulating ILC Dover Chemturion Model 1212 chemical protective suit with accessories, and the FabOhio polyvinyl chloride (PVC) splash garment. Two exposure scenarios were simulated: (1) a saturated vapor exposure for 2 hours (h), and (2) a brief MMH 'splash' followed by a 2-h saturated vapor exposure. Time-averaged MMH concentrations inside the totally-encapsulating suit were calculated by summation of the area-weighted contributions made by each suit component. Results show that the totally encapsulating suit provides adequate protection at the new 10 ppb Threshold Limit Value Time-Weighted Average (TLV-TWA). The permeation resistance of the PVC splash garment to MMH was poorer than any of the totally encapsulating suit materials tested. Breakthrough occurred soon after initial vapor or 'splash' exposure.
Compatibility data for aluminum alloy 2219-T87 and titanium alloy Ti-6Al-4V were obtained while these alloys were exposed to both liquid and vapor fluorine and FLOX at -320 F + or -10 F. These data were obtained using a new low cost compatibility method which incorporates totally sealed containers and double dogbone test specimens and propellants in the simultaneous exposure to vapor and liquid phases. The compatibility investigation covered a storage period in excess of one year. Pitting was more severe in the 2219-T87 aluminum alloy than in the Ti-6Al-4V titanium alloy for both fluorine and FLOX exposure. The degree of chemical attack is more severe in the presence of FLOX than in fluorine and phase. The mechanical properties of the two alloys were not affected by storage in either of the two propellants.
Based on cooled target collection methods and high pressure mass spectrometer sampling, oxidative vaporization rates and emanating volatile products were evaluated for interactions of KCl(g) with Cr2O3 and LaCrO3 in oxidizing environments. It was found that: (1) increased rates of oxidative vaporization upon exposure to the reactants are exhibited by chromia and fresh lanthanum chromite samples, and (2) these increased rates result from the heterogeneous formation of complex molecules such as KCl sub 1,2,3CrO3 and KOH sub 1,2CrO3. No increased rates were observed for lanthanum chromite subjected to prolonged oxidative vaporization.
Application of colloidal silica more than doubles bond strength of ceramic tile/substrate attachments. "Densification" process strengthens surface where tile attaches to felt strain-isolator pad, redistributing stresses and preventing failures at that point. First, isopropyl alcohol is applied to bottom tile surface. Second, aqueous mixture of cementing colloidal silica and reinforcing ball-milled silica particles is painted on tile. Finally, after drying, tile is rewaterproofed by exposure to vapors or methyltrimethoxysilane and acetic acid.