Indium sulfide In2S3 thick films are deposited on glass substrates using spray technique over the optimum conditions experiments (Ts = 340 °C, S/In = 2). The films are polycrystalline and have thickness of about 1.8 μm. These films are annealed in a vacuum sealed pyrex tubes (10−5 torr). Physico-chemical characterizations by SEM observation, X-ray diffraction and EDX analysis are undertaked on these films. This treatment has improved crystallinity of samples. It has allowed thus to stabilize β and γ varieties of In2S3 material. In2O3 and In6S7 phases have appeared with very weak intensities at high temperatures. The best structure quality are obtained at 300 °C for the optimum annealed temperature (Ts = 340 °C, S/In = 2), for which samples are constituted in dominance by γ phase oriented preferentially towards (1 0 2). The grain size is 42 nm of this phase. Chemical composition of such films has changed relatively to non-treated film but it seems not be affected by treatment temperature. Atomic molar ratio S/In is obtained for 0.9. Optical study shows that these layers are transparent in the visible and optical direct band gap increases as function of annealed temperature.