(1. 重庆大学 化学化工学院,重庆 400044;
2. 湖北兴福电子材料有限公司,宜昌 443711;
3. 西南科技大学 固体废物处理与资源化教育部重点实验室,绵阳 621010)
摘 要: 采用双向脉冲电沉积法制备金属锰,研究双脉冲电源的正向平均电流密度、反向脉冲系数、一组正向脉冲工作时间和反向脉冲工作时间系数对电流效率、单位功耗、阴极金属锰和阳极泥的微观形貌的影响。结果表明:双脉冲电流可有效消除浓差极化,抑制析氢反应,反向电流可溶解镀层表面的枝晶;脉冲参数过高或者过低都会造成金属锰层微观缺陷不断增加,镀层表面平整度与光亮度下降;而反向周期性电流的增大或者施加时间的延长可有效地防止阳极钝化,减少阳极泥的产生量。双脉冲电源的优化参数为:当正向平均电流密度为350 A/m2、反向脉冲系数α=1/10、一组正向脉冲工作时间为150 ms、反向脉冲工作时间系数为1/15时,电沉积2 h的电流效率最高为80.25%,阳极泥的产生量最低为2.93 g,而且金属锰镀层致密均匀、气孔少、基本无枝晶产生。
关键字: 双向脉冲电沉积;电解金属锰;电流效率;微观形貌
(1. College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044, China;
2. Hubei Sinophorus Electronic Materials Co., Ltd., Yichang 443711, China;
3. Key Laboratory of the Ministry of Education of Solid Waste Disposal and Resources, Southwest University of Science and Technology, Mianyang 621010, China)
Abstract:The preparation of electrolytic manganese metal by bidirectional pulse electrodeposition was studied, the influence of positive average current density, reverse pulse coefficient, a set of forward pulse working time and reverse pulse working time coefficient on current efficiency, unit energy consumption, micro-morphology of the cathode metal manganese and the anode mud were investigated. The results show that bipolar pulse current can effectively eliminate the concentration polarization, inhibit the hydrogen evolution reaction, and dissolve the dendrite on the surface of the coating. Moreover, the irrationality of pulse parameter will cause the metal manganese layer micro defects increasing, coating surface smoothness and brightness decreasing, while the extended of average current density or the applied time can effectively prevent the anode passivation and reduce production of anode slime. The optimal parameters of bidirectional pulse are as follows: the current efficiency achieves 80.25% and the quality of anode mud is 2.93 g, when positive average current density is 350 A/m2, reverse pulse coefficient is 1/10, a set of forward pulse working time is 150 ms and reverse pulse working time coefficient is 1/15. Moreover, the metal manganese coating is dense and uniform, with few stomata and almost no dendrite formation.
Key words: bidirectional pulse electrodeposition; electrolytic manganese metal; current efficiency; micro-morphology