Citation: CAO Yin-Liang, LI Zhi-Lin, WANG Feng, LIU Jing-Jun, JI Jing, WANG Jian-Jun, ZHANG Liang-Hu, QIN Shi-Yong. Electrochemical Preparation of Ni-Sn Active Cathode and Its Electrocatalytic Hydrogen Evolution Reaction Mechanisms in Alkaline Solution[J]. Acta Physico-Chimica Sinica, ;2013, 29(07): 1479-1486. doi: 10.3866/PKU.WHXB201305083
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A simple galvanostatic electrodeposition method was used to synthesize an active Ni-Sn electrode on a Cu foil substrate. Characterization by high-resolution transmission electron microscopy (HRTEM), energy-dispersive spectroscopy (EDS), and X-ray diffraction (XRD) revealed that the crystal structures of the deposited films transformed from amorphous structures composed of Ni crystal embryos and amorphous Ni-Sn to Ni3Sn4/ Ni3Sn2 mixed crystals with increasing Sn content. Scanning electron microscope (SEM) images indicated that the amorphous Ni-Sn electrode possessed a smooth surface with uniform distribution of small particles, whereas the Ni3Sn4/Ni3Sn2 mixed crystalline electrode exhibited a rough surface composed of lamellar structures. The polarization curves measured in 1 mol·L-1 NaOH solution at 25℃ indicated that the amorphous Ni-Sn electrode showed a smaller overpotential (85 mV) and better electrocatalytic performance for hydrogen evolution than the mixed crystalline electrode. Electrochemical impedance spectroscopy (EIS) results showed that the hydrogen evolution reaction occurs on the Ni-Sn alloy electrode under a mixture of Volmer and Heyrovsky control. The higher activity of the amorphous Ni-Sn electrode was attributed to the faster charge transfer and electrochemical adsorption and desorption rates of hydrogen atoms compared with those on the mixed crystalline electrode.
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