电化学阳极氧化构建Pb3D-PbO2结构.doc

doi：10.3969/j.issn.1007-7545.2019.0 doi：10.3969/j.issn.1007-7545.2019.01.001 王瑞祥，陈芳会，张斌，钟晓聪，徐志峰 (江西理工大学 冶金与化学工程学院，江西 赣州341000) 摘要：引入多孔基底是提高铅基复合阳极铅基底与氧化涂层结合稳定性的有效方法。采用恒电位阳极氧化技术在金属铅表面构建多孔PbO2结构，研究了氯化铵、氟化铵、醋酸铵、草酸铵4种侵蚀剂对PbO2多孔结构形貌的影响，并优选出氟化铵为侵蚀剂；进一步研究氧化电压、温度、水添加量、氟化铵添加量、氧化时间对PbO2多孔结构形貌的影响，在下述较优工艺条件下，可以在铅表面构建孔洞较均一的多孔PbO2结构：氧化电压15 V、温度25 ℃、水添加量1.25%、氟化铵添加量每100 mL乙二醇0.3 g、氧化时间6 h。 关键词：Pb/PbO2；孔洞结构；阳极氧化；侵蚀剂 中图分类号：TF812；TG174.4 文献标志码：A 文章编号：1007-7545（2019）01-0000-00 Preparation of Pb/3D-PbO2 by Electrochemcial Anodization WANG Rui-xiang, CHEN Fang-hui, ZHANG Bin, ZHONG Xiao-cong, XU Zhi-feng (School of Metallurgical and Chemical Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, Jiangxi, China) Abstract：Introduction of porous substrate is an effective method to improve bond stability between Pb substrate and oxide coating of lead-based composite anodes. Porous PbO2 structure was constructed on surface of Pb by potentiostatic anodization technique. Effects of etchants (ammonium chloride, ammonium fluoride, ammonium acetate and ammonium oxalate) on morphology of PbO2 structure were studied to select ammonium fluoride as etchant due to uniform holes in PbO2 structure. Furthermore, effects of anodization voltage, temperature, water concentration, ammonium fluoride concentration, and anodization time on morphology of PbO2 structure were investigated. Pb/3D-PbO2 structure with relatively uniform holes can be constructed on Pb surface under the optimum conditions including anodization voltage of 15 V, temperature of 25 ℃, water concentration of 1.25%, ammonium fluoride concentration of 0.3 g for 100 mL ethylene glycol, and anodization time of 6 h. Key words：Pb/PbO2; porous structure; anodization; etchant 铅及铅合金由于具有价格低廉、稳定性好的优点广泛应用于有色金属电解沉积工序，如锌、铜、锰、钴、镍等[1-5]。然而，在高浓度硫酸、高电流密度服役条件下，传统铅基阳极仍然存在析氧过电位高、服役寿命不理想的缺点[6-8]。改善铅基阳极析氧活性和耐腐蚀性能的途径主要有两类：一是优化铅基阳极的合金成分和金相结构；二是在铅（铅合金）表面镀上析氧活性高的氧化物涂层。其中，铅基涂层阳极节能效果明显而受到广泛关注。铅基涂层阳极是通过电镀、涂覆等方式实现铅（铅合金）与氧化物涂层结合。通过调控涂层的成分和制备工艺，可以获得致密、