李立清,冯罗,吴盼旺,吴婧杰,黄志强,许永章,杨佳棋,季淑蕊.新型次磷酸钠体系化学镀铜添加剂及其对镀液和镀层性能的影响[J].表面技术,2020,49(7):329-337.
LI Li-qing,FENG Luo,WU Pan-wang,WU Jing-jie,HUANG Zhi-qiang,XU Yong-zhang,YANG Jia-qi,JI Shu-rui.Novel Electroless Plating Copper Additives for Sodium Hypophosphite System and Its Effect on the Properties of Plating Bath and Coating[J].Surface Technology,2020,49(7):329-337
新型次磷酸钠体系化学镀铜添加剂及其对镀液和镀层性能的影响
Novel Electroless Plating Copper Additives for Sodium Hypophosphite System and Its Effect on the Properties of Plating Bath and Coating
投稿时间:2019-07-28  修订日期:2020-07-20
DOI:10.16490/j.cnki.issn.1001-3660.2020.07.041
中文关键词:  次磷酸钠  化学镀铜  聚乙烯吡咯烷酮  二苯胺磺酸钠  孔隙率  耐蚀性
英文关键词:sodium hypophosphate  electroless copper deposition  polyvinyl pyrrolidone  diphenylaminesulfonic acid sodium  porosity  corrosion resistance
基金项目:中国博士后基金(2016M592118);国家自然科学基金(21406097,U1607108);江西省博士后基金(2015KY11,2015RC17);江西省教育厅基金(GJJ190424)
作者单位
李立清 1.江西理工大学 材料冶金化学学部,江西 赣州 341000 
冯罗 1.江西理工大学 材料冶金化学学部,江西 赣州 341000 
吴盼旺 1.江西理工大学 材料冶金化学学部,江西 赣州 341000 
吴婧杰 2.陆军炮兵防空兵学院南京校区 教研保障中心新闻文化室,南京 210000 
黄志强 1.江西理工大学 材料冶金化学学部,江西 赣州 341000 
许永章 3.江西省信丰正天伟电子科技有限公司,江西 赣州 341600 
杨佳棋 1.江西理工大学 材料冶金化学学部,江西 赣州 341000 
季淑蕊 1.江西理工大学 材料冶金化学学部,江西 赣州 341000 
AuthorInstitution
LI Li-qing 1.Faculty of Materials Metallurgy and Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China 
FENG Luo 1.Faculty of Materials Metallurgy and Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China 
WU Pan-wang 1.Faculty of Materials Metallurgy and Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China 
WU Jing-jie 2.News Culture Office, Teaching and Research Security Center, PLA Army Academy of Artillery and Air Defense, Nanjing 210000, China 
HUANG Zhi-qiang 1.Faculty of Materials Metallurgy and Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China 
XU Yong-zhang 3.Jiangxi Xin Feng Zheng Tian Wei Technology Co. Ltd, Ganzhou 341600, China 
YANG Jia-qi 1.Faculty of Materials Metallurgy and Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China 
JI Shu-rui 1.Faculty of Materials Metallurgy and Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China 
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中文摘要:
      目的 将聚乙烯吡咯烷酮和二苯胺磺酸钠作为添加剂应用到次磷酸钠化学镀铜体系,并获取最佳应用效果的工艺和条件。方法 以PCB环氧树脂板为基材,通过电化学方法研究以聚乙烯吡咯烷酮和二苯胺磺酸钠为添加剂的次磷酸钠体系化学镀铜液及其性能,用称量法研究添加剂对沉积速率的影响,用扫描电镜和X射线能谱仪分析添加剂对沉铜表面质量的影响,用极化曲线法研究添加剂对沉铜表面孔隙率的影响,用交流阻抗法研究添加剂对沉铜表面耐蚀性的影响,同时测定镀液的稳定性。结果 在pH=10、温度为65 ℃的基础液(成分为5 g/L五水硫酸铜、30 g/L次磷酸钠、16 g/L柠檬酸钠、30 g/L硼酸、1 g/L硫酸镍)中,单独加入聚乙烯吡咯烷酮或二苯胺磺酸钠,都能起到很好的沉铜效果。它们的最佳质量浓度分别为20~28 mg/L和50~58 mg/L。当聚乙烯吡咯烷酮和二苯胺磺酸钠在最佳范围内组合使用时,获得的镀液更稳定,镀层孔隙率低、耐蚀性好、表面均匀,表面铜的质量分数达到95.52%,镀层显粉红色,沉积速率在1.5~2.5 μm/h范围内,符合PCB行业要求。结论 最佳的化学镀铜液配方和条件为:5 g/L五水硫酸铜、30 g/L次磷酸钠、16 g/L柠檬酸钠、30 g/L硼酸、1 g/L硫酸镍、20~28 mg/L聚乙烯吡咯烷酮、50~58 mg/L二苯胺磺酸钠,pH=10,温度65 ℃。研究成果对电镀铜添加剂的开发和应用有重要意义。
英文摘要:
      The work aims to apply polyvinyl pyrrolidone and diphenylaminesulfonic acid sodium to the electroless copper plating system of sodium hypophosphite as additives, and to obtain the process and condition of the optimum application results. Based on PCB epoxy resin board, the electroless copper plating system of sodium hypophosphite with polyvinyl pyrrolidone and diphenylaminesulfonic acid sodium as additives and its performance were investigated by the electrochemical method. The effect of additives on deposition rate was studied by heavy method; the effect of additives on the surface quality was analyzed by SEM and EDS; the effect of additives on the surface porosity was studied by the polarization curve method; the effect of additives on the corrosion resistance was studied by AC impedance; and the stability of plating solution was also measured. The results show that, when pH=10 and at 65 ℃, both polyvinyl pyrrolidone and diphenylaminesulfonic acid sodium had good properties for electroless copper deposition in base solution including CuSO4 5 g/L, NaH2PO2 30 g/L, Na3C6H5O7•2H2O 16 g/L, H3BO3 30 g/L, NiSO4 1 g/L, and their best dosages were 20~28 mg/L and 50~58 mg/L respectively. When used polyvinyl pyrrolidone and diphenylaminesulfonic acid sodium as combined additive in the range of their best dosage, the plating solution was more stable, the porosity of the coating was low, the corrosion resistance was good, the surface was uniform, and the copper content on the surface was up to 95.52%. Furthermore, the coating was pink and the deposition rate was in the range of 1.5~ 2.5 μm/h, which all met the requirements of PCB industry. Therefore, the best novel electroless copper deposition solution are that, CuSO4 5 g/L, NaH2PO2 30 g/L, Na3C6H5O7•2H2O 16 g/L, H3BO3 30 g/L, NiSO4 1 g/L, polyvinyl pyrrolidone 20~28 mg/L, diphenylaminesulfonic acid sodium 50~58 mg/L when pH=10 and at 65 ℃. The research results are of great significance to the development and application of electroless copper deposition additives.
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