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Rhodium sulfate exists as a whitish-red or translucent liquid. Its molecular weight is 566.05. At the molecular level, it's composed of two rhodium atoms bonded to three sulfate molecules, which themselves are composed of a sulfate atom bonded to four oxygen atoms.
The specification describes novel rhodium sulfate complex solutions which have a minimum of metal to metal complexing and are mostly complexed through the sulfate groups. Use of these solutions as electrolytes for plating rhodium results in electroplated layers with improved brightness and reduced stress.
Rhodium plated electrodes are used in the soda industry for electrolysis of salt water, and for electrodes for domestic water treatment. Rhodium plating is used widely in the jewelry industry. In the electronics industry, rhodium plating is used for electrical contacts in, e.g., ferreed switches.
The rhodium sulfate complex that is formed by standard hydrolysis is shown in FIG. 1. It is characterized by rhodium-rhodium bonding as well as bonding through the sulfate groups. By controlling the hydrolysis reaction, as described below, the rhodium to rhodium bonding is essentially eliminated and the rhodium sulfate complexes as shown in FIG. 2, with a simple bridge between the sulfate groups.
The technique for preparing this rhodium sulfate complex is described by the flow chart of FIG. 3. Rhodium is refluxed in sulfuric acid as shown to produce a rhodium sulfate concentrate. Rhodium sulfate is then neutralized with a mild base, in this case, ammonium hydroxide, by the two procedures shown in the figure. The first, Process A, is the conventional hydrolysis in which the acid and base are simply combined, with both reagents typically at room temperature. The neutralization reaction is exothermic, and the solution characteristically heats to a temperature substantially above room temperature. In the process of the invention, Process B, the neutralization reaction is controlled by cooling the rhodium sulfate to a temperature below room temperature, e.g., below 20° C., and maintaining the reagent mixture at a temperature below 25° C. during the reaction. This can be achieved by actively cooling the reaction vessel. In practice, it was found that using a jacketed reaction vessel, and flowing cool or cold water, e.g. water at 10° C., through the vessel jacket, the temperature of the reagent mixture can be controlled to a temperature below 25° C. Without active cooling during the reaction, as described above, the reagent mixture heats to a temperature above 25° C.
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