Antimony films were formed by electroless plating from a bath containing titanium trichloride as the reducing agent. The films were autocatalytically deposited to the intended thickness on the surface of non-conductive substrates activated by palladium. The optimum conditions lay in the pH range of 6.5∼8.5 at a temperature of 20°C, and the preferable bath composition was disodium EDTA 0.08M, trisodium citrate 0.32M, NTA 0.10M, antimony trichloride 0.08M and titanium trichloride 0.04M. It was observed from X-ray diffraction analysis that the crystal structure of the deposited films were greatly affected by plating conditions, especially pH, and films predominately oriented to the (006), (110) and (012) planes were formed at pH of 7.0∼7.5, 8.0 and 8.5, respectively.