Bimetallic Cu-Rh nanoparticles on diazonium-modified carbon powders for the electrocatalytic reduction of nitrates

4-Benzenethiol-functionalized high-surface-area graphite powder was prepared and decorated with bimetallic Cu100–xRhx nanoparticles (NPs) to serve as electrocatalysts for the reduction of nitrates. In the first step, the HSAG powder was grafted with in-situ-generated diazonium compounds from 4-aminothiophenol (ATP) in an acidic medium using NaNO2 for the diazotization process. The surface composition was tuned using different initial quantities of ATP. The surface XPS-determined S/C atomic ratio was found to increase stepwise with the initial quantity of amine. In a second step, the grafted and untreated HSAG powders were decorated with Cu100–xRhx NPs by a wet chemical method and the elemental composition of the end composites was assessed by EDS-SEM and ICP, whereas TEM and EDS-TEM served to characterize the NP morphology and their composition on the nanometer scale. In all cases, the NP size was invariably found to be ∼1.7 nm but with a size distribution becoming narrower under an increasing grafting ra...