Abstract: Several methods are set forth for preparing polymetallic spinels by coprecipitating two or more metal compounds in a proportion to provide a total of eight positive valences when combined in the oxide form in the spinel crystal lattice. The methods disclosed require coprecipitation of the metals in the hydroxide form or convertible to the hydroxide-oxide form, calcining the coprecipitate, and finally sintering the calcined material at about one-half its melting point or greater, thereby forming a spinel which has a density of greater than 50 percent of the theoretical density of spinel crystal. Also disclosed are techniques for preparing spinels having more than two metals incorporated into the spinel lattice, as well as a separate oxide phase associated with the spinel crystallites, and slipcasting compositions.