Chemical route for formation of intermetallic Zn4Sb3 phase

Synthesis of intermetallic zinc antimonide phases via low temperature solution route was investigated. Trial experiments were carried out under inert atmosphere at 70 deg. C using metallic Zn, SbCl3 and NaBH4 as reactants and tetrahydrofuran (THF), dimethylsulfoxide (DMSO) as organic media. Powder X-ray analysis confirmed the nucleation and growth of ZnSb phases in presence of excess Zn. SEM analysis revealed the existence of core-shell structure comprising of Zn core and Sb shell. Such particles get transformed into Zn4Sb3 crystalline phases upon thermal treatment at 300 deg. C/6 h in a silica tube closed under high secondary vacuum. - Graphical abstract: TEM observation of the Zn4Sb3 powder synthesized by soft chemistry.