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Various aqueous citrate electrolyte compositions for the Ni-Mo electrodeposition are explored in order to deposit Ni-Mo alloys with Mo-content ranging from 40 wt% to 65 wt% to find an alloy composition with superior catalytic activity towards the hydrogen evolution reaction (HER). The depositions were performed on copper substrates mounted onto a rotating disc electrode (RDE) and were investigated via scanning electron microscopy (SEM), X-ray fluorescence (XRF) and X-ray diffraction (XRD) methods as well as linear sweep voltammetry (LSV) and impedance spectroscopy. Kinetic parameters were calculated via Tafel analysis. Partial deposition current densities and current efficiencies were determined by correlating XRF measurements with gravimetric results. The variation of the electrolyte composition and deposition parameters enabled the deposition of alloys with Mo-content over the range of 40-65 wt%. An increase in Mo-content in deposited alloys was recorded with an increase in rotation speed of the RDE. Current efficiency of the deposition was in the magnitude of <1%, which is characteristic for the deposition of alloys with high Mo-content. The calculated kinetic parameters were used to determine the Mo-content with the highest catalytic activity for use in the HER.
This study presents the correlation between electrolyte pH, surface morphology, chemical speciation and electro-catalytic oxygen evolution activity of additive-free electrodeposited NiFe catalysts for application in anion exchange membrane water electrolysis. Spherical morphologies were identified at pH 0, shifting towards honey-combed structures at pH 4 with increasing surface area, especially at pH 3. Further, the electrolyte pH was found to influence the NiFe composition and electro-catalytic activity. Enhanced OER activity was noted at pH 2 with overpotentials of 214 mV at 10 mA cm−2 and 267 mV at 100 mA cm−2. The results reveal that the electrolyte pH is a parameter not only influencing the morphology but also tailoring the surface area, Fe oxide and Fe hydroxide composition and consequently the catalytic activity. Further, the outcomes highlight the electrolyte pH as a key process parameter that should be adjusted according to the application, and may substitute the addition of electrolyte-additives, proposing a simpler method for improving catalyst electrodeposition.