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化学进展 2023, Vol. 35 Issue (2): 233-246 DOI: 10.7536/PC220805 前一篇   后一篇

• 综述 •

面向电子应用的聚合物化学镀前表面处理技术

邬学贤1, 张岩1,2, 叶淳懿1, 张志彬1, 骆静利1, 符显珠1,*()   

  1. 1 深圳大学材料学院 深圳 518055
    2 深圳湾实验室坪山生物医药研发转化中心 深圳 518118
  • 收稿日期:2022-08-05 修回日期:2022-10-25 出版日期:2023-02-24 发布日期:2023-02-15
  • 作者简介:
    符显珠 深圳大学材料学院教授,博士生导师,从事电化学能源材料与器件及电子材料与制程研究。2007年厦门大学化学系博士毕业,2008-2012年在加拿大阿尔伯塔大学做博士后并到美国伯克利国家实验室进行访问研究,曾于中国科学院深圳先进技术研究院工作。近5年以通讯作者在Nature Catalysis、Journal of the American Chemical Society、Angewandte Chemie、Energy & Environmental Science、Science Bulletin(《科学通报》)等期刊发表SCI论文100多篇。
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Surface Pretreatment of Polymer Electroless Plating for Electronic Applications

Xuexian Wu1, Yan Zhang1,2, Chunyi Ye1, Zhibin Zhang1, Jingli Luo1, Xianzhu Fu1()   

  1. 1 College of Materials Science and Engineering, Shenzhen University,Shenzhen 518055, China
    2 Pingshan Biomedical R&D Transformation Center, Shenzhen Bay Laboratory,Shenzhen 518118, China
  • Received:2022-08-05 Revised:2022-10-25 Online:2023-02-24 Published:2023-02-15
  • Contact: *e-mail: xz.fu@szu.edu.cn

聚合物表面金属化在电子产品的导电互连、电磁屏蔽、导热散热、装饰保护等方面起着重要作用。与真空溅射等方法相比,化学镀是一种金属镀层均匀、低成本、易规模化生产、不需昂贵设备的聚合物表面金属化技术。近年来面向电子信息应用(如芯片制造、5G通信、柔性电子)的环氧树脂、聚酰亚胺(PI)、液晶聚合物(LCP)、聚四氟乙烯(PTFE)、聚二甲基硅氧烷(PDMS)、聚对苯二甲酸乙二酯(PET)、聚氨基甲酸酯(PU)、聚苯乙烯(PS)等聚合物化学镀技术得到积极研究。聚合物化学镀前表面处理,尤其是粗化和活化方法对于化学镀性能至关重要。粗化处理对镀层与基底的结合力、镀层对基底的完整包覆程度有明显影响;同时活化方法对化学镀的速度、镀层的厚度产生影响。在面向电子应用的聚合物化学镀前处理中,粗化过程如化学刻蚀、等离子体处理和接枝处理等,以及活化过程如离子吸附还原、催化剂直接吸附和墨水打印书写等也出现了许多新进展。本文对电子应用中各种聚合物基体化学镀前粗化和活化处理技术的最新进展进行了总结,旨在为应用于电子信息的化学镀新技术发展提供参考。

关键词： 化学镀, 聚合物, 表面改性, 粗化, 活化

Metallization of polymer surface plays an important role in conductive interconnect, electromagnetic shielding, thermal management, decoration and protection of electronic products. Compared with vacuum sputtering and other methods, electroless plating has advantages of uniform coating, low cost and easy large-scale production. In recent years, polymer used for electronic applications such as epoxy resin, polyimide (PI), liquid crystal polymer (LCP), polytetrafluoroethylene (PTFE), polydimethylsiloxane (PDMS), polyethylene terephthalate (PET), polyurethane (PU), polystyrene (PS) have been actively studied. Coarsening treatment has obvious influence on the binding force of coating and the degree of coating on the substrate. At the same time, the activation method affects the speed and thickness of electroless plating. In the surface pretreatment of polymer electroless plating, coarsening and activation methods have a great influence on the coating properties, especially for LCP and other polymers that will be used in 5G equipment. In polymer electroless plating pretreatment, coarsening processes such as chemical etching, plasma treatment and graft treatment, as well as activation processes such as ion adsorption reduction, catalyst direct adsorption and ink printing also have many new developments. In this paper, the latest development of coarsening and activation pretreatment of various polymer substrates in electronic applications is summarized, in order to provide reference for the development of electroless plating technology for electronic circuits.

Contents

1 Introduction

2 Application of polymer electroless plating in electronic field

2.1 Mechanism of electroless plating

2.2 Conductive interconnect

2.3 Electromagnetic shielding

2.4 Heat management

3 Polymer surface coarsening method

3.1 Chemical etching

3.2 Plasma treatment

3.3 Grafting treatment

4 Activation method before polymer electroless plating

4.1 Catalyst metal ion adsorption and reduction

4.2 Direct catalyst adsorption

4.3 Direct ink writing and graphic printing

5 Polyimide (PI) pretreatment method for electroless plating

6 Polyethylene terephthalate (PET) pretreatment method for electroless plating

7 Polyurethane (PU) pretreatment method for electroless plating

8 Polydimethylaminosiloxane (PDMS) pretreatment method for electroless plating

9 Polystyrene (PS) pretreatment method for electroless plating

10 Polypropylene (PP) pretreatment method for electroless plating

11 Polytetrafluoroethylene (PTFE) pretreatment method for electroless plating

12 Liquid crystal polymer (LCP) pretreatment method for electroless plating

13 Conclusion and outlook

Key words: electroless plating, polymer, surface modification, coarsening, activation
()
图1 化学镀工艺的流程示意图
Fig.1 Schematic flow diagram of the electroless plating process.
图2 电子领域中化学镀常用的基底材料和粗化、活化方法示意图。粗化:化学刻蚀、接枝、等离子体处理;活化:离子交换、墨水打印、胶体活化
Fig.2 Schematic diagram of commonly used substrate materials and roughening and activation methods for electroless plating in the field of electronics. Roughening: chemical etching, grafting, plasma treatment; activation: ion exchange, ink printing, colloidal activation.
图3 (a)PCB导电互连示意图;(b)在聚合物基底上进行化学镀制备电磁屏蔽层示意图[50];(c)在元器件之上通过一层聚合物绝缘层再进行化学镀进行热量管理的示意图[51]
Fig.3 (a) Schematic diagram of conductive interconnection of PCB; (b) Schematic diagram of electromagnetic shielding layer prepared by electroless plating on a polymer substrate[50]; (c) Schematic representation of heat management by electroless plating of components with a layer of polymer insulation[39]
图4 (a) 接枝改性过程示意图[4];(b) 粗化后试样接触角的变化[4];(c)接枝流程原理图[67];(d,e)胶带撕拉镀层结合力测试[38]
Fig.4 (a) Schematic diagram of graft modification process[4]; (b)Change of contact angle of samples after roughening[4]; (c) process of grafting; (d,e) Adhesive force test of tape pulling coating[36]
图5 (a)离子交换活化流程图[2];(b)胶水稳定性测试[1];(c)催化剂直接吸附活化流程图[53]
Fig.5 (a) Flow diagram of ion exchange activation[2]; (b) Glue stability test[1]; (c) Flow diagram of catalyst direct adsorption activation[53]
图6 催化剂吸附化学镀原理图
Fig.6 Schematic of catalyst adsorption electroless plating
图7 (a)聚酰亚胺结构式;(b)聚酰亚胺化学镀后百格刀测试[47];(c)聚酰亚胺化学镀后弯折实验与导电性变化测试[56];(d)聚酰亚胺化学刻蚀粗化后离子交换活化流程图[1];(e)聚酰亚胺化学刻蚀和接枝粗化后再活化流程图[30]
Fig.7 (a) Structural formula of polyimide; (b) 100-square-knife test after electroless polyimide plating[47]; (c) bending test and conductivity change test after electroless polyimide plating[56] ; (d) Flow chart of ion exchange activation after chemical etching and roughening of polyimide[1]; (e) Flow chart of activation after chemical etching and grafting of polyimide[30]
图8 (a)PET结构式;(b)PET化学镀后弯折和导电线路测试[59];(c)PET经过等离子体处理粗化后Pd催化剂直接吸附活化示意图[52];(d)PET化学镀制备的导电器件[63]
Fig.8 (a) PET structural formula; (b) PET electroless plating after bending and conductive circuit test[59]; (c) Schematic diagram of direct adsorption and activation of Pd catalyst after PET roughening by plasma treatment[52]; (d) Conductive wire prepared by PET electroless plating device[72]
表1 PI常用粗化与活化方法汇总
Table 1 Summary of commonly used methods for coarsening and activation of PI
Method Roughening
reagent		 Roughening
conditions		 Activating
reagent		 Activation
conditions		 ref
1 VTMS 60 ℃/15 min PdCl2
NH4OH		 / 58
METAC 80 ℃/1 h
KPS
2 KOH 5 min AuCl3.3H2O

/		 56
PdCl2
CoCl2
AgNO3
CrCl3
3 KOH 5 min AgNO3 3 min 52
4 KOH 5 min NiCl2 5 min 2
5 KOH 5 min AgNO3 5 min 57
O Plasma treatment
表2 PET常用粗化与活化方法汇总
Table 2 Summary of commonly used coarsening and activation methods for PET.
Method Roughening
reagent		 Roughening
conditions		 Activating
reagent		 Activation
conditions		 ref
1 HCl ultrasound
5 min		 KH550 / 63
AgNO3
PVA
2 / / PM Print&
Plasma
treatment		 62,65,66
CH4N2S
AgNO3
BADGE
Hardener 593
3 Plasma
treatment		 / PdCl2 64
4 MPTES 2 h Cuf / 67
OAM
Paraffin
5 VTMS 15 min (NH4)2PdCl4 3min 53
METAC 80 ℃/60 min
MPTS
图9 (a)PU结构式;(b)PU表面化学镀制备电极[71];(c)PU导电线路最细可达28 μm[71];(d)PU海绵化学镀后弹性测试[24];(e)PU导电线路测试[71];(f)PU表面化学镀弯折实验[72];(g)PU海绵化学镀前处理流程图[72];(h)通过3D打印的PU并化学镀样品[73]
Fig.9 (a) PU structural formula; (b) electrode prepared by electroless plating on PU surface[71]; (c) PU conductive line as thin as 28 μm[71]; (d) elasticity test of PU sponge after electroless plating [24]; (e) PU conductive circuit test[79]; (f) PU surface electroless plating bending experiment [80]; (g) PU sponge electroless plating pretreatment flow chart[80]; (h) 3D printed PU and electroless plating samples[82].
表3 PU常用粗化与活化方法汇总
Table 3 Summary of commonly used coarsening and activation methods for PU
Method Roughening
reagent		 Roughening
conditions		 Activating
reagent		 Activation
conditions		 ref
1 NaOH 25 ℃/24 h AgNO3 25 ℃/1 h 23
Dopamine NH3·H2O
Tris·HCl
2 Tannic acid
KMnO4		 30 min (NH4)2PdCl4 15 min 69
SnCl2
3 H2SO4 / PdCl2 25 ℃/10 min 70
HCl
4 Na2S2O8 25 ℃/5 min PdSO4 10 min 72
H2SO4
5 H2CrO4 / SnCl2 15 min 71
H2SO4 HCl
AgNO3
6 Laser
irradiation		 1064 nm / / 22
7 KOH 50 ℃/2 h AgNO3 20 min 67
Laser
irradiation		 460 nm/3 minn
8 Chitosan 4 h PdCl2 10 min 23
NaH2PO2
9 METAC / (NH4)2PdCl 4 / 73
MPTS
图10 (a)PDMS结构式;(b)PDMS经过多巴胺接枝改性粗化后使用Ag+活化流程图[78];(c)PDMS精确选择性活化化学镀图案[16]
Fig.10 (a) Structural formula of PDMS; (b) flow chart of Ag+ activation after PDMS graft modification with dopamine[78]; (c) Electroless plating pattern of PDMS precise and selective activation[16]
图11 (a)PS结构式;(b)PS微球化学镀铜后的SEM图[85];(c) (d)PS微球经过热压后互相接触形成导电网络[82];(e)PS微球化学镀并经过热压形成三维导电结构流程图[82]
Fig.11 (a) PS structural formula; (b) SEM image of PS microspheres after electroless copper plating[85]; (c) (d) PS microspheres contacted with each other after hot pressing to form a conductive network[82]; (e) PS microspheres electroless plating and Flow chart of forming a three-dimensional conductive structure by hot pressing[82]
表4 PDMS常用粗化与活化方法汇总
Table 4 Summary of common coarsening and activation methods for PDMS.
Method Roughening
reagent		 Roughening
conditions		 Activating
reagent		 Activation
conditions		 ref
1 O Plasma treatment 10 s AgClO4 spin coating &
UV treatment		 79
MPA
Ma-P1215
2 SnCl2 45 min Ag(NH3)2NO3 10 min 76
C2HF3O2
3 APTES 24 h AgNO3 Write&
Plasma
treatment		 77
Tris-HCl
Dopamine
4 Alkanethiol 3 min PdNO3 / 15
HNO3
5 APTMS 12 h Ag(NH3)2NO3 / 80
APTES 30 min
6 APTES 3 h SnCl2 / 78
Fe3O4
Au
表5 PS常用粗化与活化方法汇总
Table 5 Summary of common coarsening and activation methods for PS
Method Roughening
reagent		 Roughening
conditions		 Activating
reagent		 Activation
conditions		 ref
1 PVP 70 ℃/12 h SnCl2 45 ℃/40 min 81
styrene monomer Na2SnO3
PdCl2
HCl
2 NaOH 5 min Pd/Sn / 82,84
3 H2SO4 40 ℃/4 h SnCl2 / 85
HCl
AgNO3
NH4OH
C4H4O6KNa
4 FeCl3·6H2O 24 h Ag/Sn / 83
Pyrrole-1-propionic acid
monomer
Pyrrole monomer
表6 PP常用粗化与活化方法汇总
Table 6 Summary of commonly used coarsening and activation methods for PP
Method Roughening
reagent		 Roughening
conditions		 Activating
reagent		 Activation
conditions		 ref
1 DA-HCl 25 ℃/20 h HAuCl4 10 min 11
Tris-HCl
2 / Vacuum UV
treatment		 SnCl2 30 ℃/2 min 10
PdCl2
HCl
3 K2Cr2O7 15 min PdCl2 2 min 86
H2SO4 HCl
4 Py AgNO3 Print 13
5 TMS 10 min PdCl2 / 12
HCl
图12 (a)聚丙烯结构图;(b)聚丙烯表面化学镀制备电子器件[13];(c)聚丙烯化学镀后弯折测试[86];(d)聚丙烯在掩模板下经过紫外光照射粗化,然后使用催化剂直接吸附活化得到精确导电图案示意图[11]
Fig.12 (a) Structure diagram of polypropylene; (b) Electroless plating on polypropylene surface to prepare electronic devices[13]; (c) Bending test of polypropylene after electroless plating[86]; (d) Polypropylene roughened by ultraviolet light under the mask, and then use the catalyst for direct adsorption activation to obtain a precise conductive pattern[11]
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