The invention discloses a preparation method for solar battery materials with three-zone gap tin doped with copper, gallium and sulphur. According to the preparation method for the solar battery materials with the three-zone gap tin doped with the copper, the gallium and the sulphur, copper chloride, gallium chloride, thiourea and stannic chloride are dissolved into ethylene glycol and then are mixed uniformly, a solvothermal synthesis reaction is conducted in a sealed steel-bushing teflon reaction still, then a solvothermal product is washed, filtered and dried, and a product is obtained. It is inferred from the growth mechanism that the preparation method for solar battery materials with the three-zone gap tin doped with the copper, the gallium and the sulphur is suitable for the preparation for the solar battery materials with other transmission metal elements including VIII ( Co, Fe, Ir, Ni, Pd, Rh ) doped with the three-zone gap tin. The obtained product is good in crystallinity, high in purity and uniform in morphology and distribution; an obvious ligh-induced switching effect is possessed, when there is no light, the dark current is nearly zero, and when there is light, the current intensity rises quickly; The preparation method for the solar battery materials with the three-zone gap tin doped with the copper, the gallium and the sulphur has the advantages that the preparation technology is simple, the repeatability is good, the cost is low, the controllability is strong, and the material usage rate is high; sulfidizing is not needed, the resultant temperature is low, and green and environmental protection are possessed.