Bismuth sulfide chalcogenide was successfully synthesized inside the ampoule by conventional high temperature solid state solvothermal reaction of bismuth and sulfur. It was prepared by adjusting stoichiometric amount of the bismuth and sulfur heated in evacuated sealed quartz ampoule at 850 °C for 12h. Based on XRD principles, numerous approaches such as use of Scherrer equation, Hall – Williamson method for crystallite size estimation of  Bi₂S₃  powder. Structural properties were studied by XRD reveals that this product belongs to the orthorhombic phase, and shows that crystallite size increase as the peak broadening decreases; and  cell constants a= 4.005 A°, b= 11.14 A°, c= 11.29A°, which are in good agreement with the standard JCPDS card data were calculated.