Synthesis of Nanoscale Antimony Powder Using Aluminum as a Reducing Agent: Characterization and Sintering Microstructure

Antimony (Sb) is a key material in high-capacity potassium and sodium batteries, particularly in the fabrication of Sb–carbon composites. In this work, nanoscale Sb powder was synthesized directly from SbCl3, using Al powder as a reducing agent. The reduction process was carried out by gradually adding Al powder to an SbCl3—acetone solution under continuous cooling and stirring, owing to the highly exothermic nature of the reaction. Acetone was found to be an effective solvent, enabling the formation of Sb nanoparticles with an average particle size of 50 nm and a crystallite size of 25 nm. The purity of the produced powder was nearly 100%, as confirmed via SEM/EDS and XRD analyses. XRD patterns of both commercial and synthesized Sb powders displayed identical and ideal Sb reflections, while FTIR spectra further confirmed their structural similarity. Sintering studies revealed relative densities of 99% for pellets prepared from both commercial and synthesized powders. SEM/EDS examinations of the raw powders and sintered pellets provided complementary microstructural and compositional insights. Overall, this study demonstrates the feasibility of producing high-purity nanoscale Sb powder through a simple, single-step redox process that is both cost-effective and efficient.