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The electrochemical oxidation of sodium borohydride (NaBH4) on Pt electrode in alkaline electrolyte with the addition of thiourea has been studied by means of cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and chronopotentiometry (CP). NaBH4 is readily to react with hydroxyl groups to release hydrogen through either direct oxidation or catalytic hydrolysis. The experimental results demonstrated that the addition of an appropriate amount of thiourea to the alkaline electrolyte resulted in the suppression of catalytic hydrolysis and diffusion of borohydride ions through the separation membrane.