Abstract: A process for preparing molybdenum disilicide or a molybdenum disilicide/alumina composition is provided. In the first step of this process, a mixture containing molybdenum oxide, silica, aluminum and/or magnesium, and inorganic diluent is provided; the mixture may also contain organic surfactant and/or organic binder. In the second step of the process, the mixture is ignited, thereby causing a self-propagating reaction to occur. Thereafter, the combusted product is cooled and then washed with water, preferably until it contains less than about 0.1 percent of inorganic diluent. When the combusted product contains magnesia, the magnesia is leached from the product by treatment with nitric acid and sodium hydroxide.