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NiSCo catalytic cathodes were obtained by electrodeposition in a typical Watt cellwith addition of NH2 CSNH2 and CoCl2. Using CoCl2 concentration, current density,temperature and pH value as main factors, an orthogonal experiment was designed todetermine the optimum technological conditions according to HER overpotentials. Theoptimum technological conditions were obtained from the minimum HER overpoten-tial -70m V. The corresponding electrochemical parameters (Tafel slope b, exchangecurrent density to) were determined by steady-state polarization curves. The contentof S, Co and its microstructure were measured by EPMA and XRD.

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