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.