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The procedures used to prepare kilogram quanties of hafnium nitride and hafnium carbide powders and hot-pressed billets are described. In order to maintain high purity, all steps of the process were conducted in either a vacuum or a high purity atmosphere. Analyses conducted on the starting materials and at various stages of processing indicated that target impurity levels, i.e., less than 100 ppm oxygen, could not be attained but that high levels of contamination could be avoided.