Abstract: W–Si alloy blocks were prepared by vacuum calcination, using the W and Si mixed powders as the raw materials, and the W–Si sputtering targets followed the requirements of semiconductor application were successfully prepared by crushing and sintering. The influence of calcination temperature and holding time on the phase composition, microstructure, oxygen content, and carbon content (mass fraction) of the alloyed block was investigated. The results indicate that the oxygen content and carbon content can be remarkably reduced by high temperature calcination process. In addition, the calcination temperature has an important effect on the removal of oxygen. The optimal preparation process is the calcination at 1250 ℃ for 5 h. Under this condition, the mass fraction of oxygen in the material can be reduced from 0.3000% to 0.0121%, and the elemental tungsten phase in the material is completely transformed into the tungsten−silicon alloy phase.