A tungsten disulfide powder comprised of macro-spherical particles of tungsten disulfide having an average particle diameter of from about 5 to about 50 micrometers is prepared by successively treating spray-dried powders of ammonium metatungstate with heat in air and sulfidizing the resultant tungsten trioxide in a carbon disulfide-containing atmosphere at about 750 C. The tungsten disulfide powder may also be formed to have a bimodal particle size distribution of the macro-spherical particles and smaller, dispersed micro- to submicron-sized fine particles.