A stable and efficient porous nickel phosphate (p-NiPO/Ti) electrocatalyst on titanium sheets was developed via electrochemical deposition and low-temperature phosphatization. For obtaining the optimal performance of the p-NiPO/Ti electrocatalyst, the optimized experimental parameters of deposition and phosphatization were determined by parallel experiments. After the preparation, XPS and XRD were used to validate the chemical and amorphous structure, with SEM and TEM simultaneously validating a distinct nanosheet/nanocluster crosslinked microstructure. In particular, with phosphatization conditions maintained at 300 °C for 10 min, the p-NiPO/Ti produced demonstrated excellent charge transfer and catalytic characteristics in 1.0 M KOH. The electrocatalytic results revealed that the optimal p-NiPO/Ti with excellent catalytic performance and excellent stability (~24 h) needs lower HER overpotentials (128 mV at 10 mA cm−2 and 242 mV at 100 mA cm−2) as inputs. This research provides a promising strategy with which to use transition metal materials as catalysts in alkaline electrocatalytic hydrogen production.
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