Soft-Chemical Method for Synthesizing Intermetallic Antimonide Nanocrystals from Ternary Chalcogenide.

The synthesis of intermetallic antimonides usually depends on either the high-temperature alloying technique from high-purity metals or the flux method in highly poisonous Pb-melt. In this paper, we introduced a soft-chemical method to synthesize intermetallic antimonides from ternary chalcogenide precursors under an argon atmosphere below 200 °C. Powder X-ray diffraction and compositional analysis clearly indicate that a new phase of the Ag3Sb nanocrystal was synthesized from the Ag3SbS3 precursors. Three types of trialkylphosphines (TAPs) were applied as desulfurization agents, and the transformation mechanism was elucidated. The capability of the desulfurization agent follows the sequence of triphenylphosphine (TPP) > tributylphosphine (TBP) > trioctylphosphine (TOP). Besides, this TAP-driven desulfurization route to synthesize the intermetallic phase could also be possible for AgSbSe2 and Sb2S3. Therefore, this paper provides an efficient and mild technique for the fabrication of intermetallic nanocrystals.