Electrochemical behavior of Sb(III)/Sb during the preparation of Sb particles in deep eutectic solvent

The electrochemical behavior of Sb(III)/Sb has been preliminarily clarified during the preparation of antimony (Sb) particles in choline chloride-ethylene glycol deep eutectic solvent (ChCl-EG DES) at 333 K. Cyclic voltammetry reveals that the reduction of Sb(III) to Sb on Ti electrode is a quasi-reversible process and the diffusion coefficient DSb(III) remains in the range of 1.822×10−7 to 5.938×10−7 cm2·s−1 at 333 K. The effect of SbCl3 concentration (10–100 mM) on the cathodic and anodic polarization processes is discussed by linear sweep voltammetry. Meanwhile, the chronoamperometry analysis demonstrates that the initial nucleation of Sb on Ti electrode is fit well with the three-dimensional progressive nucleation model at 10 mM SbCl3, and then transformed into a non-three-dimensional nucleation process at 50–100 mM. Additionally, cauliflower-shaped Sb particles in size of 1–1.2 μm can be deposited onto a Ti substrate at different applied potentials (−0.525 V to −0.675 V) and reaction times (10–600 s), which are formed by the aggregation of multiple spherical grains. Increasing the concentration of Sb(III) induces the formation of snowflake-shaped Sb particles.