CN112266742B - 一种性能优异的导电胶的制备方法 - Google Patents
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Abstract
本发明涉及一种性能优异的导电胶的制备方法,包括:将10~20份乙烯基硅油、1~5份含氢硅油、1~10份气相二氧化硅依次加入双行星搅拌釜内,在120~140℃条件下搅拌分散并真空脱水2小时,冷却至45℃以下,将5~15份有机溶剂、0.001~0.005份抑制剂、0.5~1.5份附着力促进剂加入双行星搅拌釜内,混合15分钟,将0.01~0.05份催化剂加入双行星搅拌釜内,混合15分钟,然后将65~85份导电填料加入搅拌釜内,N2封存包装即可;本发明制备的导电胶,单组分,易于施胶,制作工艺简单,固化后胶层无气泡,对多种基材具有很好的粘接力,可靠性好。
Description
技术领域
本发明涉及一种性能优异的导电胶的制备方法,尤其涉及一种固化后胶层没有气泡,粘接强度良好的加成型有机硅导电胶的制备方法,属于高分子材料领域。
背景技术
导电胶是一种同时具备导电性能和粘接性能的胶黏剂,它可以将多种导电材料连接在一起,使被连接材料间形成导电通路。它是通过将导电填料填充在有机聚合物基体中,通过加热或其他方式发生固化,使其具有与金属相近的导电性能,并具有一定的粘接强度。
根据使用的有机聚合物基体不同,目前,市场上使用较多的导电胶可以分为以下几种:环氧体系、丙烯酸体系、有机硅体系等。其中,环氧体系具有粘接面广,粘接强度高,力学性能优良等优点,但其内聚强度高,固化应力大,固化速度有些慢;丙烯酸体系具有固化速度快,粘接性好等优点,但其耐热性差,固化时表面会有氧阻聚现象。有机硅体系可室温固化,也可加热固化,固化时应力小,固化后的导电胶弹性好,对大多数基材粘接力好,耐热性、耐老化性、耐候性优异,非常适合用于芯片及太阳能叠瓦组件的封装,也是目前用量最多的一种导电胶体系。但有机硅体系也存在一些缺陷,其固化后的胶层中经常会有一些小气泡存在,这就降低了粘接强度和可靠性。
发明内容
本发明提供一种性能优异的导电胶的制备方法,本发明制备的加成型有机硅导电胶固化后胶层没有气泡,对多种基材附着性良好,有效地提升了粘接强度和可靠性。
本发明所述的一种性能优异的导电胶的制备方法,包括:将10~20份乙烯基硅油、1~5份含氢硅油、1~10份气相二氧化硅依次加入双行星搅拌釜内,在120~140℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa,冷却至45℃以下,将5~15份有机溶剂、0.001~0.005份抑制剂、0.5~1.5份附着力促进剂加入双行星搅拌釜内,混合15分钟,将0.01~0.05份催化剂加入双行星搅拌釜内,混合15分钟,然后将65~85份导电填料加入搅拌釜内,在真空状态下混合30分钟,真空度不小于-0.098MPa,N2封存包装即可。
导电填料作为导电胶的关键材料,也是决定导电胶成本的主要因素。导电填料主要有金、银、铜、镍等电阻率较低的金属粉末。金粉具有优异的导电性和化学稳定性,是最理想的导电填料,但价格昂贵,一般只在要求较高的情况下使用。铜粉和镍粉具有较好的导电性,成本低,但在空气中容易氧化,使导电性变差。银粉价格居中,具有很好的导电性和导热性,它在空气中不易氧化,即使被氧化了,生成的银氧化物也有较好的导电性。因此,在市场上,尤其是对可靠性要求高的电气装置上,以银粉为导电填料的导电胶应用最多。
我们在用银粉制作加成型有机硅导电胶时发现,固化后的胶层中经常会有一些小气泡存在,对粘接强度和可靠性会有潜在的不良影响。经过大量实验,我们发现气泡的产生主要是由于银粉在有机硅体系中浸润性不是太好造成的。本专利选择适当材料,采用特殊工艺对银粉表面进行化学处理,改善其在体系中的浸润性和相容性,从而实现固化后的胶层中没有气泡,改善了粘接强度和可靠性。在上述技术方案的基础上,本发明还可以做如下改进。
所述银粉的预处理过程包括:将浓度为1%的醋酸钠水溶液加入搅拌釜中,然后加入银粉,在50℃条件下搅拌1小时,用水清洗三次至PH值为7-7.5,边搅拌边缓慢滴加偶联剂[2-(3,4-环氧环己基)乙烷基三甲氧基硅烷]浓度为2.0-5.0wt%的水溶液,水溶液用量为银粉总量的20-30%,在60℃条件下搅拌2小时,用水清洗至PH=7,干燥后用300目网过滤备用。
进一步,所述乙烯基硅油为含有两个或两个以上乙烯基的聚二甲基硅氧烷。具有如下结构式:
进一步,所述含氢硅油具有如下结构式:
进一步,所述气相二氧化硅为疏水型气相二氧化硅或亲水型气相二氧化硅的一种或几种的混合物。
进一步,所述有机溶剂为长链烷烃油、二甲苯中的一种或几种的混合物。
进一步,所述抑制剂为3-甲基-1-丁炔-3-醇、3,5-二甲基-1-己炔-3-醇、1-乙炔基-1-环己醇中的一种或几种的混合物。
进一步,所述附着力促进剂OM为自制的,其对增进体系的粘接效果非常明显。其结构式如下:
附着力促进剂OM制备方法如下:将1molγ-(2,3-环氧丙氧)丙基三甲氧基硅烷和1mol烯丙醇加入烧瓶中,开始升温,同时边搅拌边滴加1.0g水杨酸,升温至180℃,并在此温度下继续反应4.5小时。
进一步,所述催化剂为铂金催化剂。
进一步,所述导电填料为银粉。
本发明的有益效果是:本发明提供的一种性能优异的导电胶,单组分,易于施胶,制作工艺简单,固化后胶层无气泡,对多种基材具有很好的粘接力,可靠性好。
具体实施方式
以下对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
银粉的预处理:将浓度为1%的醋酸钠水溶液加入搅拌釜中,然后加入银粉,在50℃条件下搅拌1小时,用水清洗三次至PH值为7-7.5,边搅拌边缓慢滴加偶联剂[2-(3,4-环氧环己基)乙烷基三甲氧基硅烷]浓度为2.0-5.0wt%的水溶液,用量为银粉总量的20-30%,在60℃条件下搅拌2小时,用水清洗至PH=7,干燥后用300目网过滤备用。以下实施例中使用的银粉均为已处理后的。
实施例1
将10份乙烯基硅油(其中a=300,b=200)、1份含氢硅油(其中m=40,n=50,R=H)、1份亲水型气相二氧化硅依次加入双行星搅拌釜内,在120~140℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa,冷却至45℃以下,将5份长链烷烃油,0.001份3-甲基-1-丁炔-3-醇,0.5份附着力促进剂OM加入双行星搅拌釜内,混合15分钟,将0.01份铂金催化剂加入双行星搅拌釜内,混合15分钟,然后将65份银粉加入搅拌釜内,在真空状态下混合30分钟,真空度不小于-0.098MPa,N2封存包装即可。
实施例2
将20份乙烯基硅油(其中a=50,b=100)、5份含氢硅油(其中m=25,n=15,R=H)、10份疏水型气相二氧化硅依次加入双行星搅拌釜内,在120~140℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa,冷却至45℃以下,将10份长链烷烃油、5份甲苯,0.005份3,5-二甲基-1-己炔-3-醇,1.5份附着力促进剂OM加入双行星搅拌釜内,混合15分钟,将0.05份铂金催化剂加入双行星搅拌釜内,混合15分钟,然后将85份银粉加入搅拌釜内,在真空状态下混合30分钟,真空度不小于-0.098MPa,N2封存包装即可。
实施例3
将15份乙烯基硅油(其中a=200,b=150)、3份含氢硅油(其中m=35,n=20,R=H)、5份疏水型气相二氧化硅依次加入双行星搅拌釜内,在120~140℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa,冷却至45℃以下,将10份长链烷烃油,0.003份1-乙炔基-1-环己醇,1.0份附着力促进剂OM加入双行星搅拌釜内,混合15分钟,将0.03份铂金催化剂加入双行星搅拌釜内,混合15分钟,然后将75份银粉加入搅拌釜内,在真空状态下混合30分钟,真空度不小于-0.098MPa,N2封存包装即可。
实施例4
将15份乙烯基硅油(其中a=150,b=50)、3份含氢硅油(其中m=15,n=20,R=CH3)、7份疏水型气相二氧化硅依次加入双行星搅拌釜内,在120~140℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa,冷却至45℃以下,将5份长链烷烃油、5份甲苯、0.001份3-甲基-1-丁炔-3-醇,0.03份1-乙炔基-1-环己醇,0.7份附着力促进剂OM加入双行星搅拌釜内,混合15分钟,将0.025份铂金催化剂加入双行星搅拌釜内,混合15分钟,然后将75份银粉加入搅拌釜内,在真空状态下混合30分钟,真空度不小于-0.098MPa,N2封存包装即可。
将实施例1至4跟银粉未做处理的导电胶做性能对比测试,相关数据均在相同条件下测试所得,具体测试结果见下表1。
试验实施例
通过下面的试验测试本发明的一种性能优异的导电胶的性能。
试验实施例1
粘度试验:依据GB/T 2794-2013进行测试。
粘接强度:依据GB/T 7124-2008进行测试。
体积电阻:四探针法
测试项目 | 未处理型 | 实例1 | 实例2 | 实例3 | 实例4 |
固化后胶层有无气泡 | 多 | 无 | 无 | 无 | 无 |
粘度,Pa.s | 25.36 | 22.12 | 22.95 | 22.88 | 21.54 |
粘接强度,MPa | 2.29 | 3.38 | 3.25 | 3.43 | 3.59 |
体积电阻Ω.cm | 1.67*10<sup>-4</sup> | 2.27*10<sup>-5</sup> | 1.69*10<sup>-5</sup> | 2.08*10<sup>-5</sup> | 1.75*10<sup>-5</sup> |
从上表的测试结果可以看出本发明制备的性能优异的导电胶,固化后胶层无气泡,粘接强度明显高于常规方法制作的导电胶,体积电阻降低了一个数量级,从而提高了胶体的导电性,同时导电胶的粘度也有一些降低,改善了施胶的工艺性,其综合性能明显优于常规方法制作的导电胶产品。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.一种性能优异的导电胶的制备方法,其特征在于,包括:将10~20份乙烯基硅油、1~5份含氢硅油、1~10份气相二氧化硅依次加入双行星搅拌釜内,在120~140℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa,冷却至45℃以下,将5~15份有机溶剂、0.001~0.005份抑制剂、0.5~1.5份附着力促进剂加入双行星搅拌釜内,混合15分钟,将0.01~0.05份催化剂加入双行星搅拌釜内,混合15分钟,然后将65~85份导电填料加入搅拌釜内,在真空状态下混合30分钟,真空度不小于-0.098MPa,N2封存包装即可;
所述乙烯基硅油为含有两个或两个以上乙烯基的聚二甲基硅氧烷,结构式如下:
所述含氢硅油结构式如下:
所述导电填料为银粉,银粉的预处理过程包括:将浓度为1%的醋酸钠水溶液加入搅拌釜中,然后加入银粉,在50℃条件下搅拌1小时,用水清洗三次至pH值为7-7.5,边搅拌边缓慢滴加偶联剂[2-(3,4-环氧环己基)乙烷基三甲氧基硅烷]浓度为2.0-5.0wt%的水溶液,水溶液用量为银粉总量的20-30%,在60℃条件下搅拌2小时,用水清洗至pH=7,干燥后用300目网过滤备用。
3.根据权利要求1所述的制备方法,其特征在于,所述气相二氧化硅为疏水型气相二氧化硅或亲水型气相二氧化硅的一种或几种的混合物;有机溶剂为长链烷烃油、二甲苯中的一种或几种的混合物;所述抑制剂为3-甲基-1-丁炔-3-醇、3,5-二甲基-1-己炔-3-醇、1-乙炔基-1-环己醇中的一种或几种的混合物;所述催化剂为铂金催化剂。
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