RI 6915 Rhenum And Rhenum-Tungsten Deposition By Thermochemical Reduction Of The Hexaflourides?A Preliminary Study

Near-optimum parameters were determined by the Bureau of Mines for vapor deposition of rhenium on heated copper substrates by hydrogen reduction of rhenium hexafluoride (ReF6). High-purity deposits of nearly 90-percent theo¬retical density were obtained with the reaction chamber at 250° C, with an H2 to ReF6 volume ratio of 25 to 1, and with an ReF6 flow rate of 5 grams per hour. Some rhenium deposited as a loose, black powder. When the established near-optimum parameters were carefully followed, this could be minimized but never completely avoided. Varying the reaction chamber pressure, both above and below atmospheric, yielded excessive quantities of rhenium powder. Deposition efficiencies, based on only the coherent metal, ranged between 70 and 75 percent. Massive deposits contained only spectrographic traces of impurities. The average microhardness (Knoop, 100-gram load) of vapor-deposited rhenium was 907. Limited research on the deposition of rhenium-tungsten alloys by reduction of the mixed hexafluorides produced deposits in which linear composition gradients were pronounced; this nonhomogeneity was attributed to the wide variation in optimum hydrogen-reduction temperatures of the two hexafluorides (250° C for ReF6 and 550° C for WF6). Using deposition temperatures between 250° and 550° C did not eliminate the composition variations.