Indium Antimonide (InSb) compound semiconductor were grown under vacuum 10^-5 torr in vacuum coating unit using Indium (99.999 %) and Antimony (99.999 %) metal powder as a source materials with various composition using formula In_1-xSb_x (where x is variable having value 0.2 to 0.4) for preparation of ten compound semiconductors. Each compound semiconductor was prepared by heating from 373 K to 473 K, for 5 hours, and this process was repeated five times. X-ray diffraction studies of ten samples to confirm the polycrystallinity of compound semiconductor and these samples show preferential orientation along the (111), (220), (311),(422) and (400) planes. The grain size (D), Dislocation density (ä) and lattice parameter (a) of compound semiconductor were evaluated with XRD data. The grain size increased from 3.4 A^o to 6.5 A^o with increasing of boat temperature from 373 K to 473 K, and Dislocation density were decreased with increase of temperature.