王丽娟,廖娟,宋宁,黄剑,刘伟飞,罗意昕,樊小伟,唐云志,谭育慧.脉冲法制备低轮廓微纳表面结构电子铜箔[J].表面技术,2024,53(22):202-209.
WANG Lijuan,LIAO Juan,SONG Ning,HUANG Jian,LIU Weifei,LUO Yixin,FAN Xiaowei,TANG Yunzhi,TAN Yuhui.Preparation of Electronic Copper Foils with Low-profile and Micro-nano Surface Structures by Pulsed Method[J].Surface Technology,2024,53(22):202-209 |
| 脉冲法制备低轮廓微纳表面结构电子铜箔 |
| Preparation of Electronic Copper Foils with Low-profile and Micro-nano Surface Structures by Pulsed Method |
| 投稿时间：2023-12-16 修订日期：2024-04-22 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.22.018 |
| 中文关键词: 粗化处理 纳米铜颗粒 超低轮廓 剥离强度 添加剂 |
| 英文关键词:coarsening treatment copper nanoparticles ultra-low profile peel strength additives |
| 基金项目:江西省自然科学基金(20202ACB20200);江西省重点研发计划项目(20212BBE51018，0224BBE51045) |
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| Author | Institution |
| WANG Lijuan | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
| LIAO Juan | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
| SONG Ning | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
| HUANG Jian | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
| LIU Weifei | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
| LUO Yixin | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
| FAN Xiaowei | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
| TANG Yunzhi | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
| TAN Yuhui | Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Jiangxi Ganzhou 341000, China |
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| 中文摘要: |
| 目的 随着5G通信高频高速传输技术的发展，亟需开发出低轮廓、高剥离、微细纳米铜颗粒结构的电子铜箔，以满足5G材料低介电、低损耗的要求。方法 开发了一种复合添加剂的粗化液体系，通过脉冲电沉积制备了低轮廓电子铜箔，表面形成了微纳米铜颗粒。利用扫描电子显微镜、接触角测试、激光共聚焦显微镜和电化学测试等技术手段表征了脉冲占空比和复合添加剂粗化对纳米铜颗粒形貌、铜箔表面粗糙度和剥离强度的影响。结果 调节脉冲占空比能有效控制纳米铜颗粒微观形貌。当占空比为20%、40%和60%时，平均尺寸小于80 nm，纳米铜颗粒微观形貌差异不明显，均呈现出近似圆球状的形貌。占空比为80%的条件下，得到了平均尺寸为59 nm的圆球状纳米级微细瘤点。此时铜箔表面粗糙度Rz为0.817 μm，剥离强度为0.95 N/mm。此外，复合添加剂使纳米铜颗粒平均粒径从274 nm降低至77.4 nm。电化学测试发现，加入复合添加剂后极化曲线由−0.49 V正移至−0.39 V，这说明复合添加剂的加入能够显著提升镀液的去极化能力。结论 当脉冲占空比为80%时，颗粒尺寸最小，铜箔同时具有极低轮廓与高剥离强度的性能。复合添加剂体系能够有效细化纳米铜颗粒，稳定其形貌。对高频高速传输中降低信号传输损耗具有重要意义。 |
| 英文摘要: |
| With the development of high-frequency and high-speed transmission, the copper foil, as one of the key the materials, is facing the challenge of a new era (low dielectric, low profile, high peeling, micro-fine copper nanoparticles structure has become the mainstream of the development of electronic copper foil). In this paper, a coarsening liquid system with compound additives was developed for the first time. Copper nanoparticles were formed on the surface of the copper foil by pulse and direct current electrodeposition. The effects of pulse duty cycle and coarsening of composite additives on the appearance of copper nanoparticles, surface roughness, and peel strength of the copper foil were characterized by scanning electron microscopy (SEM), contact angle measurement (CAM), confocal laser confocal microscopy (CLSM), and electrochemical testing. The results showed that the micro-morphology of copper nanoparticles could be controlled effectively by adjusting the pulse duty ratio. When the duty cycle was 20%, 40% and 60%, the particle size of copper nanoparticles was 74.8 nm, 73 nm and 77 nm, respectively. The difference of the microscopic morphology of nanoparticles was not obvious, and they all showed approximately spherical morphology. The Rz value of copper foil surface roughness was maintained at 0.9 μm stably, and the peel strength was 0.93 N/mm, 0.95 N/mm and 0.97 N/mm, respectively, showing a slightly increasing trend. The spheroidal nanoscale tumors with an average size of 59 nm were obtained under the condition of 80% duty cycle. At this time, the surface roughness Rz of copper foil was 0.817 nm, and the peel strength was 0.95 N/mm. It was also found that the copper nanoparticles obtained by DC coarsening showed irregular and stacked island-like morphology, and the pulsed process was more effective in reducing the particle size of the copper nanoparticles compared with DC, maintaining the homogeneity of the particle morphology of the nanoparticles, and reducing the phenomenon of particle size grading. The contact angle test showed that as the particle size of the copper tumor increased, the contact angle on the surface of the copper foil increased. The calculated surface free energy reflected the ability of the copper tumor to increase the surface area of the copper foil and improve the bonding ability with the substrate. In addition, the SEM and CLSM showed that the composite additive had a significant effect on reducing the particle size of copper nanoparticles, and the average particle size of nanoparticles was reduced from 274 nm to 77.4 nm under the same roughening process. The electrochemical tests found that the polarization curve shifted significantly in the range from −0.49-−0.39 V after the addition of composite additives, which demonstrated that the addition of composite additives significantly improved the depolarizing ability of the plating solution. In conclusion, when the pulse duty cycle is 80%, the size of the copper tumor is minimized, and the copper foil has the performance of very low profile and high peel strength at the same time. The composite additive system can effectively refine the copper tumor particles and stabilize the morphology of the copper tumor. This study is of great significance for the reduction of signal transmission loss in high-frequency and high-speed transmission. |
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