Abstract In this paper, a Co3O4- and CNT-doped 3D PbO2 electrode was fabricated through galvanostatic electrodeposition in a Pb(Ac)2-NH2SO3H solution, and the electrochemical properties were systematically investigated in a zinc electrolyte. The XRD results show that the deposit is a mixture of an α + β phase (a dominant β-PbO2 phase with a minor α-PbO2 phase present), and the SEM images show that Co3O4 and CNT have been simultaneously deposited with PbO2. The 3D-Ti/PbO2-(4 g·L−1) Co3O4-(0.4 g·L−1) CNT electrode exhibits a voltammetric charge 5 times larger than that of the 3D-Ti/PbO2 electrode, which indicates outstanding electrocatalytic activity. The oxygen evolution reaction overpotential and cell voltage are only 394 mV and 3.74 V at 500 A∙m−2, respectively. In addition, the obtained electrode showed a high current efficiency of 95.3% and a service life of 26 h under a current density of 20,000 A∙m−2. Hence, this study offers a facial synthesis route to prepare composite electrodes for zinc electrowinning and provides deep insight into the relationship among doping substances, microstructures and electrocatalytic activity.

中文翻译：

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用于锌电积的高表面积 Co3O4 和 CNT 掺杂 3D-Ti/PbO2 电极的简单一步合成

摘要 本文在 Pb(Ac)2-NH2SO3H 溶液中通过恒电流电沉积制备了 Co3O4 和 CNT 掺杂的 3D PbO2 电极，并在锌电解液中系统地研究了其电化学性能。XRD 结果表明沉积物是 α + β 相（主要 β-PbO2 相和少量 α-PbO2 相）的混合物，SEM 图像显示 Co3O4 和 CNT 与 PbO2 同时沉积。3D-Ti/PbO2-(4 g·L-1) Co3O4-(0.4 g·L-1) CNT 电极的伏安电荷是 3D-Ti/PbO2 电极的 5 倍，表明其具有出色的电催化活性. 析氧反应过电位和电池电压在 500 A∙m−2 时分别仅为 394 mV 和 3.74 V。此外，所获得的电极显示出高达 95 的电流效率。3%，在 20,000 A∙m−2 的电流密度下使用寿命为 26 小时。因此，本研究为制备用于锌电积的复合电极提供了一种面部合成途径，并深入了解了掺杂物质、微观结构和电催化活性之间的关系。