Cu(NO3)2 and (NH4)6H2W12O40·4H2O were used to prepare W/Cu nanosized composite powder by sol-gel technique. The influences of heat treatment process, pH value of the solution and the amount of an addition agent on particle size were investigated by DSC, XRD and TEM. The results show that, at a certain heat treatment temperature, the W/Cu nanoparticle size increases with the pH value or the amount of the addition agent increasing.