Gao Xiaoying,Wang Haojun*,Zhou Yanwen,et al.Research on process parameters and properties of non-cyanide copper plating in HEDP system[J].Plating & Finishing,2025,(04):42-49.
doi: 10.3969/j.issn.1001-3849.2025.04.007HEDP体系无氰镀铜的工艺参数和性能研究
- Title:
- Research on process parameters and properties of non-cyanide copper plating in HEDP system
- Keywords:
- electroplated copper; hydroxyethylphosphonic acid; orthogonal experiment; fatigue performance; hydrogen embrittlement performance
- 分类号:
- TQ153.2
- 文献标志码:
- A
- 摘要:
- 采用羟基乙叉二膦酸体系的无氰镀铜槽液在30CrMnSiA基体上沉积镀铜层,研究了电流密度、槽液温度和铜离子浓度对沉积速率、分散能力和镀层结合力的影响;同时研究了电流密度对电流效率的影响,温度对光亮区电流密度的影响;同时研究了无氰镀铜和氰化镀铜在氢脆性能和疲劳性能上的差异。结果表明:镀层沉积速率和电流密度、电镀温度和铜离子浓度呈正相关。在正交试验参数范围内,电流密度对沉积速率的影响最大,其次是温度,最后是铜离子浓度;在正交试验的参数范围内,电流密度对镀液分散性的影响最大,其次是温度,最后是铜离子浓度;HEDP电镀铜的电流效率在电流密度2 A/dm2时达到了最大值;随着镀液温度升高,光亮区域范围的电流密度逐渐增大,温度为65 ℃时,半光亮区域的电流密度上限可达4.5 A/dm2;无氰镀铜和氰化镀铜对基材的氢脆性能和疲劳性能的影响几乎一致,在可接受范围内。
- Abstract:
- A cyanide-free copper plating bath was used to deposit a copper plating layer on a 30CrMnSiA substrate using a hydroxyethylidene phosphonic acid system. The effects of current density, bath temperature, and copper ion concentration on deposition rate, dispersion ability, and coating adhesion were studied; At the same time, the influence of current density on current efficiency and the influence of temperature on current density in the bright region were studied; At the same time, the differences in hydrogen embrittlement and fatigue performance between cyanide free copper plating and cyanide copper plating were studied. The results indicate that the deposition rate of the coating is positively correlated with current density, electroplating temperature, and copper ion concentration. Within the range of orthogonal experimental parameters, the current density has the greatest impact on deposition rate, which is actually temperature, followed by copper ion concentration; Within the parameter range of orthogonal experiment, current density has the greatest impact on the dispersion of plating solution, followed by temperature, and finally copper ion concentration; The current efficiency of HEDP copper electroplating reaches its maximum value at a current density of 2 A/dm2; As the temperature of the plating solution increases, the current density in the bright area gradually increases. At a temperature of 65 ℃, the upper limit of the current density in the semi bright area can reach 4.5 A/dm2; The effects of cyanide free copper plating and cyanide copper plating on the hydrogen embrittlement and fatigue properties of the substrate are almost identical and within an acceptable range
参考文献/References:
[1].王玥, 冯立明. 电镀工艺学[M]. 北京: 化学工业出版社, 2018: 147.
[2].霍栓成. 镀铜[M]. 北京: 北京工业出版社, 2007: 109.
[3].沈品华. 现代电镀手册(上册)[M]. 北京: 机械工业出版社, 2010: 131-151.
[4].张允诚, 胡如南, 向荣. 电镀手册[M]. 北京: 国防工业出版社, 1997: 1011-1012.
[5].柳玉波. 表面处理工艺大全[M]. 北京: 中国计量出版社, 1996: 139-142.
[6].秦足足, 李建三, 徐金来, 等. 国内外无氰镀铜工艺研究进展[J]. 电镀与涂饰, 2015, 34(3): 149-152.
[7].Krishnan R M, Kanagasabapathy M, Jayakrishnan S, et al. Electroplating of copper from a non-cyanide electrolyte[J]. Plating and Surface Finishing, 1995, 82(7): 56-59.
[8].黄崴, 曾振欧, 谢金平, 等. HEDP溶液体系镀铜添加剂的研究[J]. 电镀与涂饰, 2014, 33(3): 95-99.
[9].杨防祖, 余嫄媚, 黄令, 等. 亚硫酸盐/硫代硫酸盐体系无氰镀铜[J]. 电镀与涂饰, 2009, 28(3): 1-3.
[10].杨防祖, 吴伟刚, 林志萍, 等. 钢铁基体上柠檬酸盐碱性无氰镀铜[J]. 电镀与涂饰, 2009, 28(6): 1-4.
[11].杨防祖, 宋维宝, 黄令, 等. 钢铁基体酒石酸盐碱性无氰镀铜[J]. 电镀与精饰, 2009, 31(6): 1-4.
[12].蒋义锋, 陈明辉, 杨防祖, 等. 新型钢铁无氰镀铜工艺及其应用[J]. 电镀与涂饰, 2012, 31(8): 7-10.
[13].张志梁, 储荣邦.钢铁基体直接强酸性镀铜工艺[J]. 表面工程与再制造, 2021, 21(2): 19-22.
[14].何建平. 无氰电镀工艺的研究现状及解决问题的途径[J]. 电镀与涂饰, 2005, 24(7): 42-45.
[15].方景礼. 电镀添加剂理论与应用[M]. 北京: 国防工业出版社, 2006: 280.
[16].史塔古夫. 纳米电化学[M]. 北京: 化学工业出版社, 2010: 84-100.
[17].储荣邦, 关春丽, 储春娟. 焦磷酸盐镀铜生产工艺[J]. 材料保护, 2006, 39(10): 58-66.
[18].毕晨, 刘定富, 曾庆雨, 等. 六种辅助配位剂对丁二酰亚胺体系无氰镀铜的影响[J]. 电镀与涂饰, 2016, 35(16): 829-833.
相似文献/References:
[1]文庆杰*,彭华领,稽 海,等.表面活性剂对HEDP镀铜层致密度的影响[J].电镀与精饰,2020,(3):12.[doi:10.3969/j.issn.1001-3849.2020.03.003]
WEN Qingjie*,PENG Hualing,JI Hai,et al.Influences of Surfactant on the Density of HEDP Copper Plating Layer[J].Plating & Finishing,2020,(04):12.[doi:10.3969/j.issn.1001-3849.2020.03.003]
[2]冀林仙*,王跃峰.多场耦合研究PCB电镀铜[J].电镀与精饰,2022,(11):18.[doi:10.3969/j.issn.1001-3849.2022.11.004]
JI Linxian*,WANG Yuefeng.Research on Copper Electrodeposition of PCB Based on Multi-Physics Coupling[J].Plating & Finishing,2022,(04):18.[doi:10.3969/j.issn.1001-3849.2022.11.004]
[3]向 静,阮海波*,王 翀,等.添加剂竞争吸附机理研究及通孔电镀应用[J].电镀与精饰,2022,(11):85.[doi:10.3969/j.issn.1001-3849.2022.11.015]
XIANG Jing,RUAN Haibo*,WANG Chong,et al.Study on Competitive Adsorption Mechanism of Additives and Its Application of Though Holes Plating[J].Plating & Finishing,2022,(04):85.[doi:10.3969/j.issn.1001-3849.2022.11.015]
[4]张东升,吴 宁,任 兵,等.HEDP体系电镀铜层结合力的影响因素研究[J].电镀与精饰,2023,(7):53.[doi:10.3969/j.issn.1001-3849.2023.07.007]
Zhang Dongsheng,Wu Ning,Ren Bing,et al.Study on influencing factors on the adhesion of electroplated copper coating in HEDP system[J].Plating & Finishing,2023,(04):53.[doi:10.3969/j.issn.1001-3849.2023.07.007]
[5]郑家翀,何 为,陈先明,等.镀镍磷金属片表面处理对电镀铜生长状态影响的研究[J].电镀与精饰,2024,(1):84.[doi:10.3969/j.issn.1001-3849.2024.01.013]
Zheng Jiachong,He Wei,Chen Xianming,et al.Effect of surface treatment on growth state of electroplating copper for nickel-phosphorus plated metal[J].Plating & Finishing,2024,(04):84.[doi:10.3969/j.issn.1001-3849.2024.01.013]
[6]刘颖*,邢希瑞,田栋,等.酸性一价铜电镀铜的工艺及能效分析[J].电镀与精饰,2024,(4):99.[doi:10.3969/j.issn.1001-3849.2024.04.014]
Liu Ying*,Xing Xirui,Tian Dong,et al.Energy efficiency analysis of copper electroplating employing acidic cuprous solution[J].Plating & Finishing,2024,(04):99.[doi:10.3969/j.issn.1001-3849.2024.04.014]
[7]陈 洁,宗高亮,代禹涵,等.巯基吡啶异构体对电镀铜填盲孔的影响研究[J].电镀与精饰,2024,(9):1.[doi:doi: 10.3969/j.issn.1001-3849.2024.09.001]
Chen Jie,Zong Gaoliang,Dai Yuhan,et al.Study on the influence of pyrithione isomers on filling blind holes in electroplated copper[J].Plating & Finishing,2024,(04):1.[doi:doi: 10.3969/j.issn.1001-3849.2024.09.001]
[8]性能影响研究.退火对TSV电镀铜膜层性能影响研究[J].电镀与精饰,2024,(10):42.
Yu Xianxian*,Jiang Chuang,Zhang Cuicui.Effect of annealing on the properties of electroplated copper in TSV[J].Plating & Finishing,2024,(04):42.
[9]杨彦章,陈志华,钟上彪,等.doi: 10.3969/j.issn.1001-3849.2025.03.0014PEG在电子电镀铜中的作用机制及应用[J].电镀与精饰,2025,(03):96.
Liu Binyun*,Zhan Dongping.The mechanism and application of PEG in electronic electroplating of copper Yang Yanzhang1,2, Chen Zhihua2, Zhong Shangbiao 2,Ye Shaoming3,[J].Plating & Finishing,2025,(04):96.
[10]方 正,韦相福,杨广柱,等.doi: 10.3969/j.issn.1001-3849.2025.03.015盲孔数值仿真电镀铜研究进展[J].电镀与精饰,2025,(03):106.
Hu Xiaoqiang,Chen Dedeng.Advances in numerical simulation of copper electroplating in blind vias Fang Zheng1, Wei Xiangfu1,2, Yang Guangzhu1, Mao Xianchang1,3, Wei Song3*,[J].Plating & Finishing,2025,(04):106.