低松比片状银粉作为导电相的聚合物浆料的制备技术及性能研究
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摘要
银具有良好的导电性、导热性和化学稳定性,是其它金属很难替代的。因此,立足于纯银浆料,致力于改善银在树脂中的分散性以减少银浆中银粉的用量的研究具有重要的意义。本课题使用一种松装密度较小的片状银粉作为导电相,来配制一种性能与常规银浆相近,但导电相用量显著降低的纯银浆料。
本文首先系统的阐述了国内外电子浆料发展状况,然后从浆料基本工艺条件的确定、粘合剂的选择、浆料最佳配比的确定和低松比片状银粉的微观分析及银粉、银浆市场状况四个方面来进行系统研究,得到如下结论：
通过大量的实验,我们确定配制银浆的最佳配方如下：树脂为聚氨酯树脂B Y 10 10,其质量含量占24%；增稠剂为缔合型增稠剂2026,占16%；混合溶剂(NBA+CYC+783慢干水),占16%；硅烷偶联剂,占4%；导电填料,低松比片状银粉(松装密度为0.43g/cm3),占40%,固化工艺条件为130℃下固化40min及研磨时间40min-50min。
低松比片状银粉的微观分析发现：(1)球状银粉的粒径最小,其相对应的松比和比表面积最大；片状银粉的松比与对应的比表面积有关,松比越大,其粉体的比表面积越大,而与其粉体的粒径没有很大的关系。
(2)通过SEM和EDS发现导电银浆中,随着银粉松比的减小,微观组织变得更致密,黑色孔洞会更少；松比小的表面分布的银粉反而越多,说明低松比浆料表面的致密性好。
市场分析可知,没有企业投入建立国际化一流开发、生产平台,这将制约了银粉、银浆项目在国内的发展,也无法实现产业化。而我们研究的低松比片状银粉做的银浆若用于市场,将净赚利润8010万元／年,经济效益显著。
Silver has excellent conductivity, thermal conductivity and chemical stability, resulting in the other metals are difficult to replace it. Therefore, based on the silver paste, it is of great significance to improve the silver in the resin dispersion of silver paste in order to reduce the amount of silver. In this topic, a bulk density smaller flake silver powder is used as conductive phase, and the preparation of a performance is similar to conventional silver paste, but the relative amount of conductive silver paste is significantly reduced.
This article first describes the system development of domestic and international electronic paste, and then there were carry out systematic research in four areas, including the basic process conditions determination of paste, the choice of adhesives, the determination of the best ratio of the paste, the micro-analysis of the lower loose density flake silver powder, the market conditions of the silver powder and silver paste. the following conclusions was drawn:
Through a large number of experiments, the best preparation of silver paste formula is get as follows:resin, polyurethane resin, BY1010, its quality content,24%; thickener for Associative Thickener 2026, accounting for 16%; mixed solvent (NBA+CYC+783 slowly dry-water), accounting for 16%; silane coupling agent, accounting for 4%; conductive filler, lower loose density flake silver powder (bulk density of 0.43g/cm3), accounting for 40%, curing process conditions of 130℃for 40min and the grinding time for curing 40min-50min.
Microstructure analysis of the lower loose density flake silver powder was found:(1) the size of spherical silver powder is the smallest and its corresponding surface area ratio is the largest. the bulk density of flake silver power was related to the corresponding ratio of surface area, the larger is the bulk density, and the larger of the surface area of its powder; but not much relationship with powder particle size.
It was found by SEM and EDS in conductive silver paste, with the bulk density of silver power was decreased, the microstructure of the conductive silver paste becomes more dense, black holes will be less; the distribution of silver of the lower loose density flake silver powder in conductive silver paste was much more, indicating the surface density of the lower loose density flake silver powder in conductive silver paste is good.
Market analysis shows that there is no businesses to invest in the establishment of an international first-class development, production platforms, which will restrict the silver powder, silver paste projects in national development, it can not be achieved industrialization. We study the lower loose density flake silver powder and silver paste, if applied to the market, it will get net profit 80.1 million yuan / year, with significant economic benefits.
本文首先系统的阐述了国内外电子浆料发展状况,然后从浆料基本工艺条件的确定、粘合剂的选择、浆料最佳配比的确定和低松比片状银粉的微观分析及银粉、银浆市场状况四个方面来进行系统研究,得到如下结论：
通过大量的实验,我们确定配制银浆的最佳配方如下：树脂为聚氨酯树脂B Y 10 10,其质量含量占24%；增稠剂为缔合型增稠剂2026,占16%；混合溶剂(NBA+CYC+783慢干水),占16%；硅烷偶联剂,占4%；导电填料,低松比片状银粉(松装密度为0.43g/cm3),占40%,固化工艺条件为130℃下固化40min及研磨时间40min-50min。
低松比片状银粉的微观分析发现：(1)球状银粉的粒径最小,其相对应的松比和比表面积最大；片状银粉的松比与对应的比表面积有关,松比越大,其粉体的比表面积越大,而与其粉体的粒径没有很大的关系。
(2)通过SEM和EDS发现导电银浆中,随着银粉松比的减小,微观组织变得更致密,黑色孔洞会更少；松比小的表面分布的银粉反而越多,说明低松比浆料表面的致密性好。
市场分析可知,没有企业投入建立国际化一流开发、生产平台,这将制约了银粉、银浆项目在国内的发展,也无法实现产业化。而我们研究的低松比片状银粉做的银浆若用于市场,将净赚利润8010万元／年,经济效益显著。
Silver has excellent conductivity, thermal conductivity and chemical stability, resulting in the other metals are difficult to replace it. Therefore, based on the silver paste, it is of great significance to improve the silver in the resin dispersion of silver paste in order to reduce the amount of silver. In this topic, a bulk density smaller flake silver powder is used as conductive phase, and the preparation of a performance is similar to conventional silver paste, but the relative amount of conductive silver paste is significantly reduced.
This article first describes the system development of domestic and international electronic paste, and then there were carry out systematic research in four areas, including the basic process conditions determination of paste, the choice of adhesives, the determination of the best ratio of the paste, the micro-analysis of the lower loose density flake silver powder, the market conditions of the silver powder and silver paste. the following conclusions was drawn:
Through a large number of experiments, the best preparation of silver paste formula is get as follows:resin, polyurethane resin, BY1010, its quality content,24%; thickener for Associative Thickener 2026, accounting for 16%; mixed solvent (NBA+CYC+783 slowly dry-water), accounting for 16%; silane coupling agent, accounting for 4%; conductive filler, lower loose density flake silver powder (bulk density of 0.43g/cm3), accounting for 40%, curing process conditions of 130℃for 40min and the grinding time for curing 40min-50min.
Microstructure analysis of the lower loose density flake silver powder was found:(1) the size of spherical silver powder is the smallest and its corresponding surface area ratio is the largest. the bulk density of flake silver power was related to the corresponding ratio of surface area, the larger is the bulk density, and the larger of the surface area of its powder; but not much relationship with powder particle size.
It was found by SEM and EDS in conductive silver paste, with the bulk density of silver power was decreased, the microstructure of the conductive silver paste becomes more dense, black holes will be less; the distribution of silver of the lower loose density flake silver powder in conductive silver paste was much more, indicating the surface density of the lower loose density flake silver powder in conductive silver paste is good.
Market analysis shows that there is no businesses to invest in the establishment of an international first-class development, production platforms, which will restrict the silver powder, silver paste projects in national development, it can not be achieved industrialization. We study the lower loose density flake silver powder and silver paste, if applied to the market, it will get net profit 80.1 million yuan / year, with significant economic benefits.
引文
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[10]电子浆料技术网.电子浆料用有机载体.
[11]郑瑞琪,余云照.合成胶粘剂丛书[M].北京：化学工业出版社,1985.125-154
[12]《化工百科全书》编辑委员会,化学工业出版社《化工百科全书》编辑部.树脂与塑料·《化工百科全书》专业卷(下)：p304,1015
[13]刘锡洹,王小升.导体浆料及其发展动向[J].化工时刊,1991,9:21-24.
[14]Xinjian Huang J.J.Pot,W.Th.Kok.Electrochemical characteristics of conductive carbon cement as matrix for chemically modified electrodes.Analytica Chimica Acta, 1995,300:5-14.
[15]R.Edelbro,A.Sandstrom,J.Paul.Full Potential calculations on the electron band-
structures of Sphalerite,Pyrite and Chalcopyrite.Applied Surface Science,2003,206: 300-313
[16]钱军民,李旭祥.环氧树脂改性研究进展[J].绝缘材料,2001,5:27-31
[17]《化工百科全书》编辑委员会,化学工业出版社《化工百科全书》编辑部.树脂与 塑料·《化工百科全书》专业卷(下)：p205,897
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[19]孙文通.碳膜电位器端头用铜银导电浆料的研究[J].电子元件与材料,1992,11(1):37-39
[20]钟庆东,杭建忠,等.导电涂料的研究进展[J].上海电力学院学报.2005,21(2)：143-160
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