间歇超声搅拌辅助化学镀制备核壳型镍包铜粉  

Preparation of core-shell nickel-coated copper composite powder by electroless plating with the assistance of alternative ultrasonic vibration and mechanical stirring

作　　者：朱康杰 张涵 赵珩宇 史文南 杨向民[2] 张震[2] 方斌[2] ZHU Kangjie;ZHANG Han;ZHAO Hengyu;SHI Wennan;YANG Xiangmin;ZHANG Zhen;FANG Bin(School of Materials Science and Engineering,East China University of Science and Technology,Shanghai 200237,China;School of Physics,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]华东理工大学材料科学与工程学院,上海200237 [2]华东理工大学物理学院,上海200237

出　　处：《电镀与涂饰》2024年第9期12-25,共14页Electroplating & Finishing

基　　金：国家级大学生创新创业训练计划项目(202410251087)。

摘　　要：[目的]通过优化化学镀配方和工艺,提升镍包铜粉的分散均匀性和镀层品质,以增强其作为导电填料在电子浆料中的抗氧化和导电性能。[方法]先采用Pd Cl_(2)体系活化铜粉,然后在间歇超声搅拌辅助下,采用酸性体系进行化学镀镍,制备出核壳型镍包铜粉。利用扫描电子显微镜(SEM)和X射线衍射仪(XRD)分析了Ni镀层的微观形貌和晶体结构,研究了活化液组分、镀液配方和搅拌方式对化学镀的影响。通过扫描电镜观察、能谱面扫分析和热重分析,检验了在较优条件下制备的镍包铜粉的镍层包覆效果和抗氧化性能。[结果]铜粉活化的较优配方为:Pd Cl_(2)0.50 mmol/L,盐酸2.40 mol/L,聚氧乙烯20油醚2.0 g/L。铜粉化学镀镍的较优配方为:硫酸镍0.037 5 mol/L,乙酸钠0.15 mol/L,乙酸0.27 mol/L,聚氧乙烯20油醚2.0 g/L,聚乙烯吡咯烷酮1.5 g/L,还原剂溶液(次磷酸钠3.367 mol/L)滴加速率2.5 mL/h。化学镀过程中采用30 s超声振荡和30 s机械搅拌交替进行的间歇超声搅拌方式有利于制备出镀层均匀致密和颗粒分散性良好的镍包铜粉。[结论]在较优条件下制备的镍包铜粉具有镀覆率高、镍层致密、颗粒分散均匀、抗氧化性能好等优点。[Introduction]The electroless plating bath and process parameters need to be optimized to enhance the dispersibility and coating quality of nickel-coated copper powder,thereby improving its antioxidation and conductivity when being used as conductive fillers in electronic paste.[Method]The copper powder was activated in a PdCl_(2)-containing solution firstly,followed by electroless plating in an acidic bath with the assistance of alternative ultrasonic vibration and mechanical stirring to produce core-shell-structured nickel-coated copper powder.The micromorphology and crystal structure of the nickel coating were characterized by scanning electron microscopy(SEM)and X-ray diffraction(XRD).The effects of the compositions of activation solution and plating as well as different stirring methods on the electroless plating quality were studied.The nickel coating coverage and anti-oxidizability of the nickel-coated copper powder prepared under the optimized conditions were characterized through SEM observation,energy-dispersive spectroscopic(EDS)mapping,and thermogravimetric analysis.[Result]The composition of activation solution for copper powder was optimized as follows:PdCl_(2)0.50 mmol/L,HCl 2.40 mol/L,and polyoxyethylene(20)oleyl ether 2.0 g/L.The composition of electroless plating bath was optimized as follows:nickel sulfate 0.0375 mol/L,sodium acetate 0.15 mol/L,acetic acid 0.27 mol/L,polyoxyethylene(20)oleyl ether 2.0 g/L,and polyvinylpyrrolidone 1.5 g/L.The dropping rate of reductant solution(i.e.3.367 mol/L sodium hypophosphite)was determined as 2.5 mL/h.[Conclusion]The nickel-coated copper powder prepared under the optimized conditions exhibited high coating coverage,good compactness,uniform dispersion,and excellent anti-oxidizability.

关 键 词：镍包铜粉 化学镀 间歇超声搅拌 导电填料 抗氧化性能 

分 类 号：TQ153.12[化学工程—电化学工业]