Barium titanate powder on nanometer scale was synthesized by means of co-precipitation. The thermal mass loss, crystal grain growth and phase transition of the barium titanate nanometer powder were investigated by TG (Thermogravimetric)-DTA (Differential scanning calorimetric) and XRD (X-ray powder diffractometer) at different heat treatment temperatures. The results show that amorphous barium titanate powder can transfer into tetragonal symmetry structure after heat treatment. When the heat treatment temperature is below 900℃, the grains grow rapidly because the activation energy at low temperature is greatly less than that at high temperature. By controlling theheat treatment temperature, the optimization of the barium titanate crystallite size and formation of tetragonal phase can be realized.