镀液流动对泡沫炭真空超声化学镀铜的影响

doi:10.15541/jim20150276

无机材料学报 ›› 2016, Vol. 31 ›› Issue (1): 69-74.DOI: 10.15541/jim20150276

镀液流动对泡沫炭真空超声化学镀铜的影响

杨柳¹, 刘秀军¹, 李同起², 韩瑞连¹, 冯志海²

(1. 天津工业大学环境与化学工程学院, 天津 300387; 2. 航天材料及工艺研究所先进功能复合材料技术国防科技重点实验室, 北京 100076)

收稿日期:2015-06-10 修回日期:2015-07-26 出版日期:2016-01-20 网络出版日期:2015-12-15
作者简介:杨柳(1990–), 女, 硕士研究生. E-mail: yangliuqsd2008@163.com
基金资助:
国家重点实验室基金(9140C560109130C569199);国家自然科学基金(51102070)

Effect of Plating Solution Flow Pattern on Preparation of Electroless Copper- Plated Carbon Foam under Vacuum and Ultrasonic Conditions

YANG Liu¹, LIU Xiu-Jun¹, LI Tong-Qi², HAN Rui-Lian¹, FENG Zhi-Hai²

(1. School of Environmental and Chemical Engineering, Tianjin Polytechnic University, Tianjin 300387, China; 2. National Key Laboratory of Advanced Functional Composite Materials, Aerospace Research Institute of Materials and Processing Technology, Beijing 100076, China)

Received:2015-06-10 Revised:2015-07-26 Published:2016-01-20 Online:2015-12-15
About author:YANG Liu. E-mail: yangliuqsd2008@163.com
Supported by:
State Key Laboratory Program (9140C560109130C569199);National Natural Science Foundation of China (51102070)

摘要/Abstract

摘要：

真空超声辅助化学镀铜, 可以在大体积泡沫炭内部孔隙表面镀铜, 但沉铜分布不均。在此基础上, 本研究强制镀液在泡沫炭内部充分流动, 并探究流动方式对镀层性能的影响。相比于镀液单向流动, 镀液双向流动实现了铜增量的均匀分布, 轴向切片铜的增重率超过7.10%, 整块泡沫炭铜的增重率为7.68%; 镀层均匀致密, 平整光滑, 厚度超过5 μm, 各向分布差异很小; 镀层无CuO、Cu₂O杂质; 机械性能、电学性能都得到均匀地提高, 压缩强度从0.70 MPa增大至1.54 MPa, 电导率从700 S/cm 增加至1724 S/cm。

关键词: 流动镀, 化学镀铜, 泡沫炭, 真空辅助

Abstract:

Electroless plating with assistance of vacuum and ultrasonic is an effective method to coat copper onto the inner surface of bulk carbon foam. However, it is difficult to obtain uniform copper coating. In present work, the copper coating’s uniformity was improved by forcing plating solution inside the carbon foam on basis of vacuum and ultrasonic assistance during eletroless plating process. And effect of the flow pattern on plated copper’s properties was investigated. Compared with one-direction flow of plating solution, a bidirectional flow made the weight gain rate of single cut piece >7.10% and the total weight increased up to 7.68%. The copper coating at thickness >5 µm; with better uniformity was compact, smooth and no CuO or Cu₂O. The mechanical and electrical properties of Cu/carbon foam were evenly enhanced. The compression strength was increased from 0.70 MPa to 1.54 MPa, and the conductivity from 700 S/cm to 1724 S/cm.

Key words: plating solution flow, electroless copper plating, carbon foam, vacuum assisted

中图分类号:

TB333

杨柳, 刘秀军, 李同起, 韩瑞连, 冯志海. 镀液流动对泡沫炭真空超声化学镀铜的影响[J]. 无机材料学报, 2016, 31(1): 69-74.

YANG Liu, LIU Xiu-Jun, LI Tong-Qi, HAN Rui-Lian, FENG Zhi-Hai. Effect of Plating Solution Flow Pattern on Preparation of Electroless Copper- Plated Carbon Foam under Vacuum and Ultrasonic Conditions[J]. Journal of Inorganic Materials, 2016, 31(1): 69-74.

图/表 11

图1 超声真空流动装置

Fig. 1 Schematic of vacuum and ultrasonic assisted flow electroless copper plating

表1 镀液组成及工艺条件

Table 1 Plating solution composition and process conditions

Steps	Composition	Conditions
Degreasing	60 g/L NaOH 20 g/L Na₂CO₃ 20 g/L Na₃PO₄	50℃, 20 min
Roughening	60% HNO₃	25℃, 20 min
Sensitization	5% HCl 20 g/L SnCl₂	25 min
Activation	30 g/L AgNO₃	25 min; Vacuum, 10 min
Electroless copper plating	20 g/L CuSO₄•5H₂O 26 g/L Na₂EDTA•2H₂O 20 g/L C₁₁H₁₃KO₈•4H₂O 20 mL/L 2, 2-Bipyridine 20 mL/L methanal(37%)	Room temperature pH 12.2-12.5 Vacuum: 0.04-0.06 MPa Ultrasonic: 42 kHz, 100 W

图2 镀铜泡沫炭轴向切割示意图

Fig. 2 Ordinate cutting of Cu/carbon foam

图3 不同镀液流动方式铜增重率的轴向分布曲线

Fig. 3 Copper coating weight gain rate vs height in different plating solution flow patterns

图4 泡沫炭内部孔隙表面的铜沉积过程示意图

Fig. 4 Schematic of copper deposition on pore surface

表2 镀液流动方式对镀层宏观表面形态轴向分布的影响(自A端向B端)

Table 2 Macroscopic morphology of copper coating vs. height in different plating solution flow patterns (From A to B)

	CF2	CF3
Color	Bright red→Black	Copper red; Well-distributed
Compactness	Density↓ Porosity↑	Uniform and dense; Well-distributed
Smoothness	Leveling↓ Surface roughness↑	Smoothy and flat; Well-distributed

图5 不同镀液流动方式镀层微观表面形貌轴向分布

Fig. 5 SEM images of copper coating vs. height in different plating solution flow patterns

图6 不同镀液流动方式镀层厚度轴向分布

Fig. 6 Coating thickness vs. height in different plating solution flow patterns

图7 不同镀液流动方式镀铜泡沫炭压缩强度轴向分布

Fig. 7 Compressive strength of Cu/carbon foam vs height in different plating solution flow pattern

图8 不同流动方式镀铜泡沫炭电导率轴向分布曲线

Fig. 8 Conductivity of copper coating vs height in different plating flow patterns

图9 双向流动镀的镀铜泡沫炭的XRD图谱

Fig. 9 XRD patterns of Cu/carbon foam obtained at a bidirectional flow of plating solution

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镀液流动对泡沫炭真空超声化学镀铜的影响

Effect of Plating Solution Flow Pattern on Preparation of Electroless Copper- Plated Carbon Foam under Vacuum and Ultrasonic Conditions

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