The effect of these three NCs is studied here by assessing their electrocatalytic activity studies. To perform the electrochemical measurements, thin film electrodes were initially fabricated for each NCs using a spray coating technique. This involved depositing a slurry of the individual NCs and carbon black (CB) onto a carbon paper substrate. It is crucial to maintain the geometric and electronic structure of the individual NCs during this loading process to preserve their inherent electrocatalytic properties. The stability of these NCs during this process was assessed using XAFS data. The significant overlap between the pre-edge peak position of XANES spectra at the Cu K-edge for of loaded NCs with the individual NCs, indicating no notable changes in their electronic states (Figure ). Additional FT-EXAFS spectra verified that the ligand environment remained intact during the loading process, as evidenced by a consistent peak at ~1.8 Å, attributed to Cu-P or Cu-S bonds (Figure ). Moreover, TEM images further validated the discrete nature of each NC after being loaded onto the CB surface, showing that their sizes were preserved (Figure ).