Production of High-Purity Sb Nano-Powders for Advanced Functional Materials: Zn-Driven Reduction of SbCl3 in Organic Media

Antimony nanomaterials are becoming increasingly important in advanced functional applications, including catalysis, sensing, optoelectronics, and energy systems, motivating the development of reliable synthetic routes capable of producing high-purity Sb at the nanoscale. This study establishes a direct Zn-mediated reduction pathway for converting SbCl3 into elemental Sb using acetone, ethanol, and methanol as reaction media. SbCl3 was first dissolved in each solvent, followed by controlled addition of Zn powder under mild heating (60 °C), magnetic stirring, and ultrasonic agitation. Acetone proved the most effective medium, achieving ~94% of the theoretical Sb yield, while suppressing the formation of the SbOCl intermediate observed in alcoholic solvents. Structural and compositional analyses using XRD and SEM/EDS confirmed the formation of a pure phase, nanocrystalline Sb with mean crystallite sizes of ~25 nm in acetone, ~27 nm in ethanol, and ~21 nm in methanol. TGA/DTA measurements from room temperature up to 800 °C revealed oxidative conversion to off-white antimony oxide under O2 atmosphere and the formation of molten Sb droplets under N2 atmosphere, consistent with the expected thermal transitions of high-purity Sb. Overall, the findings demonstrate that Zn-driven reduction of SbCl3 in high-purity organic media provides an efficient and scalable approach for producing Sb nano-powders with solvent-dependent yields and nanoscale structural characteristics.