By using the soluble salt of transition metalz Zn, Cd, Pb, Mn, Co, Ni, Cu, Ag, Sb and Bi, selenious acid or its solutl salt, or antimonous acid or its soluble salt as raw material, and hydrazine hydrate, sodium borohydride, potassium borohydride, hydroxylamine or hydrazine sulfate as reductant, and through hydrothermal reduction reaction at 100-200 deg.c in a sealed container for 2 hr to 5 days, selenides or tellurides of the said metals as semiconductor material may be synthesized. Unlike available synthesis process, which needs high temperature, toxic feedstock and complex technological course, the present invention has the advantages of low-cost material, simple apparatus, easy control, good technological reproducibility, stable product quality, etc.