Supercritical Fluid-Assisted Fabrication of Pd Nanoparticles/Graphene Using a Choline Chloride–Oxalic Acid Deep Eutectic Solvent for Enhancing the Electrochemical Oxidation of Glycerol

[Image: see text] A green method for synthesizing Pd nanoparticles/graphene composites from a choline chloride–oxalic acid deep eutectic solvent (DES) without a reducing agent or a surfactant is reported. Deep eutectic solvents are usually composed of halide salts and hydrogen-bond donors, and many are biocompatible and biodegradable. The merits of deep eutectic solvents include that they serve as reducing agents and dispersants, and Pd nanoparticles are tightly anchored to graphene. The size and dispersion of Pd particles are improved when supercritical carbon dioxide (scCO(2)) is used because it has gaslike diffusivity and near-zero surface tension, which results in excellent wettability between the scCO(2) and the carbon surface. The prepared sc-Pd NPs/GR/SPCE shows excellent activity toward glycerol oxidation compared to composites not fabricated by scCO(2) processes. This study demonstrates the potential of using this scCO(2)-assisted protocol combined with deep eutectic solvents to further construct nanoparticles/graphene composites.