In this paper, the milling process of WO3 and aluminum particles is studied. Influences of rotate rate, milling time and ball-to-powder weight ratio on the morphology and grain size of the particles are studied by scanning electronic microscope and X-ray diffraction techniques. Al particle size decreases firstly and then increases with increasing milling time, while Al grain size decreases gradually as the milling time increases. WO3 particle is distributed uniformly in Al particles after milling for 9h, and has no marked change as further extension of milling time. With increasing the ball-to-powder weight ratio and rotate rate, both particle size and grain size of Al decreases. milling parameters have almost no effect on the grain size of the WO3 particles.