The integration technology of hydrogen preparation–hydrogen storage not only can utilize hydrogen energy efficiently but also can improve the selectivity of the electrode maximally. In the present work, the structure and composition of the PtNi catalyst was characterized by X‐ray diffraction (XRD); and its electrochemical properties, morphology, and surface binding energy were analyzed by cyclic voltammetry (CV) and linear scanning voltammetry (LSV), scanning electron microscopy equipped with energy‐dispersive spectrometry (SEM‐EDS), and X‐ray photoelectron spectroscopy (XPS), respectively. The effects of different acid etching treatments (e.g., etching time, etchant concentration, and etching temperature) on the structure and surface active sites were investigated by the orthogonal experiment. The experimental results reveal that after etching with 0.5 mol/L of perchloric acid for 0.5 h at 60°C, the electrode weight loss of the PtNi catalyst is mainly attributed to the large loss of Ni atoms in film layer. This results in the reduced alloy phase in film layer and the appearance of Pt characteristic diffraction peak. The relative content of Pt on the surface of the film electrode increases significantly, and the total number of active sites also increases correspondingly. The binding energy of Pt4f_7/2 decreases by 0.19 eV, and the number of active sites involved in hydrogen release decreases, indicative of the reduced promotion effect of the PtNi catalyst on hydrogen release.

中文翻译：

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酸蚀对PtNi催化剂结构和总暴露活性位的影响

制氢-储氢一体化技术不仅可以有效利用氢能，而且可以最大程度地提高电极的选择性。在本工作中，PtNi催化剂的结构和组成通过X射线衍射（XRD）表征。并通过循环伏安法（CV）和线性扫描伏安法（LSV），配备能谱仪（SEM-EDS）的扫描电子显微镜和X射线光电子能谱（XPS）分析了其电化学性质，形态和表面结合能）， 分别。通过正交实验研究了不同的酸蚀处理（例如，蚀刻时间，蚀刻剂浓度和蚀刻温度）对结构和表面活性部位的影响。实验结果表明，在60°C下用0.5 mol / L高氯酸腐蚀0.5 h后，PtNi催化剂的电极失重主要归因于膜层中Ni原子的大量损失。这导致膜层中的合金相减少并且出现Pt特征衍射峰。膜电极表面上Pt的相对含量显着增加，并且活性位点的总数也相应地增加。Pt4f的结合能 膜电极表面上Pt的相对含量显着增加，并且活性位点的总数也相应地增加。Pt4f的结合能 膜电极表面上Pt的相对含量显着增加，并且活性位点的总数也相应地增加。Pt4f的结合能_7/2降低了0.19 eV，参与氢释放的活性位点数量减少，表明PtNi催化剂对氢释放的促进作用降低。