Now this synthesized powder was mixed with calculated amount of H3BO3 and Mg for further SHS to improve the conversion of product. The mixture was synthesized and the product was leached and dried as per process sequence of SSHS. The phase analysis of the product prepared by DSHS was carried out by XRD technique and the wet chemical analysis was also repeated. The high-resolution TEM (HRTEM) study of DSHS ZrB2 powder was investigated by (JEOL JEM-2010, Tokyo, Japan).