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Adsorption phenomena in noble metals rhodium, iridium, palladium, and gold - application of potentiostatic delta method
Under normal one-g conditions immiscible alloys segregate extensively during solidification due to sedementation of the more dense of the immiscible liquid phases. However, under low-g conditions it should be possible to form a dispersion of the two immiscible liquids and maintain this dispersed structure during solidification. Immiscible (hypermonotectic) gold-rhodium alloys were processed in the Marshall Space Flight Center 105 meter drop tube in order to investigate the influence of low gravity, containerless solidification on their microstructure. Hypermonotectic alloys composed of 65 atomic % rhodium exhibited a tendency for the gold rich liquid to wet the outer surface of the containerless processed samples. This tendency led to extensive segregation in several cases. However, well dispersed microstructures consisting of 2 to 3 micron diameter rhodium-rich spheres in a gold-rich matrix were produced in 23.4 atomic % rhodium alloys. This is one of the best dispersions obtained in research on immiscible alloy-systems to data.
Design and testing of six iridium versus iridium- 60 rhodium thermocouples
Metallographic studies and transition temperature measurements were made with isothermally annealed and water-quenched zirconium-rhodium alloys. The results clarify both the solid-state phase relations at the Zr-rich end of the Zr-Rh alloy system and the influence upon the superconducting transition temperature of structure and composition.
Very thin rhodium electro-deposit plating eliminates the need for corrosion-resistant protection on silver surfaces and has no effect on the pliability characteristics of the plated surface.
Contamination of thermocouples is minimized by use of pure alumina insulators and a controlled low-impurity-level high-vacuum environment. Average thermal electromotive force change for platinum-rhodium thermocouples was -2.8 deg K after 3700 hours exposure to a mean temperature of 1530 deg K.
CO adsorption on smooth polycrystalline platinum and rhodium electrodes at various potentials
The temperature variation of the solubility of hydrogen in rhodium, ruthenium, iridium, and nickel in equilibrium with H2 gas at 1 atm pressure has been measured by a technique involving saturating the solvent metal with hydrogen, quenching, and analyzing in resultant solid solutions. The solubilities determined are small (atom fraction of H is in the range from 0.0005 to 0.00001, and the results are consistent with the simple quasi-regular model for dilute interstitial solid solutions. The relative partial enthalpy and excess entropy of the dissolved hydrogen atoms have been calculated from the solubility data and compared with well-known correlations between these quantities.
An iridium versus iridium-40% rhodium thermocouple was studied. Problems associated with the use of this thermocouple for high temperature applications (up to 2000 C) were investigated. The metallurgical studies included X-ray, macroscopic, resistance, and metallographic studies. The thermocouples in the as-received condition from the manufacturer revealed large amounts of internal stress caused by cold working during manufacturing. The thermocouples also contained a large amount of inhomogeneities and segregations. No phase transformations were observed in the alloy up to 1100 C. It was found that annealing the thermocouple at 1800 C for two hours, and then at 1400 C for 2 to 3 hours yielded a fine grain structure, relieving some of the strains, and making the wire more ductile. It was also found that the above annealing procedure stabilized the thermal emf behavior of the thermocouple for application below 1800 C (an improvement from + or - 1% to + or - 0.02% within the range of the test parameters used).
Thermocouples were exposed to exhaust gases from the combustion of propane, 72-octane gasoline, and JP-4 fuel. Exposure increased the emissivity of the thermocouple wire, which increased its radiation error. Two methods are presented for determining the emittance of the wires. The emissivity of a clean platinum rhodium-platinum thermocouple was approximately 0.2 in the temperature range investigated, while the emittance of an exposed thermocouple coated with exhaust residue was about 0.5. The exposure caused negligible change in the thermoelectric power of the thermocouples.
Reduction of C60 with rhodium(0) on alumina and hydrogen in deuterated benzene (C6D6) at ambient temperature and pressure yields a mixture of hydrogenated compounds; C60H2 has been characterized as the major product in 14% yield based on 1H NMR.
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La-Rh system study by powder X ray diffraction, metallographic and differential thermal analysis, constructing equilibrium diagram and determining crystal structure data
Thorium phosphide anti-type microstructure of La-Rh system by X ray diffraction, discussing bcc structure, lattice constants, etc
Evaporated Rh films preparation at various substrate temperatures in vacuum UV, determining reflectance and optical constants
A scheme for the photochemical fixation of water is proposed which involves a five-step reaction sequence; the first step involves the 2 electron reduction of a metal by a coordinated carbonate ligand, with corresponding oxidation of the carbonate to CO2 and O2. Ligand field photolysis of trans- (RH(en)2 H2O CO3) ClO4, and (Rh(en)2 CO3) CLO4 have been studied in the solid state and in aqueous solution at various pH values. Both salts are photoinert in the solid phase, but are quite photoreactive in aqueous solution. In solution, the monodentate ion undergoes efficient isomerization to a mixture of cis and trans - (Rh(en)2 H2O CO3)+, presumably with water exchange. A minor pH increase upon photolysis is evidence of inefficient carbonate (CO3 =) release, with formation of (Rh(en)2 (H2O)2)3+. In contrast, aqueous solutions of the bidentate carbonato complex undergo efficient pH decrease upon ligand field photolysis. Changes in the electronic spectrum (200-500 nm) and pH changes indicate that the desired redox is occurring. The pH increase is due to the aqueous behavior of CO2.
Reflectance measurements were made of several metals illuminated from various angles with light at 14 wavelengths in the interval 46.5-283 A. The metals, Rh, Os, Pt and Au were deposited as 125 A films on a binding substrate through electron beam epitaxy. Measurements were made with a grazing incidence monochromator and a reflectometer. The data generally showed lowered reflectance with increasing angles of illumination and shorter wavelengths. The reflectance peak, however, was located at wavelengths of 100-160 A, particularly at large grazing incidences. The wavelengths correspond with the 5p to epsilon-d transition in all of the elements. Rh displayed the highest overall reflectance, and both Rh and Os were more efficient than Au or Pt.
AMTEC cells are under development as power resources for future outer planetary robotic space missions, where they must operate for very long times.