Spray pyrolysis has been widely used to prepare homogeneous and uniform ceramic powders with high purity. In this study, we are proposing ultrasonic spray pyrolysis followed by heat treatment to produce SiOx/C composite powders, where sucrose was used as a carbon source. Furthermore, high energy ball milling of the as-prepared powders in the presence of acetylene black was conducted to activate its electrochemical properties by reducing the particle size and improving the functionalization of the SiOx composite particles. SiOx/C nanocomposite finally obtained at a sucrous concentration of 0.1 mol L-1 showed superior electrochemical properties, and the SiOx/C nanocomposite electrode delivered the first discharge and charge capacities of 1252 and 819 mAh g-1, respectively, with an initial columbic efficiency of 65% at a current density of 50 mAh g-1 in the potential range from 0.01 to 3 V versus Li/Li+.