CN103384904A - 各向异性导电膜 - Google Patents

各向异性导电膜 Download PDF

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CN103384904A
CN103384904A CN2012800003761A CN201280000376A CN103384904A CN 103384904 A CN103384904 A CN 103384904A CN 2012800003761 A CN2012800003761 A CN 2012800003761A CN 201280000376 A CN201280000376 A CN 201280000376A CN 103384904 A CN103384904 A CN 103384904A
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浜地浩史
石松朋之
林慎一
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Dexerials Corp
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Abstract

由水分引起的粘结性的降低得到抑制、保存稳定性优异的各向异性导电膜是导电性颗粒分散在绝缘性粘结剂中的各向异性导电膜，含有1～20wt%、优选5～15wt%沸石。该沸石的平均微孔径为3～5埃，沸石的平均粒径小于导电性颗粒的平均粒径。优选前者为后者的10%～80%。具体来说，沸石的平均粒径优选0.1μm～8μm，导电性颗粒的平均粒径为1μm～10μm。

Description

各向异性导电膜
技术领域
本发明涉及用于将电子部件的端子之间各向异性导电连接的、有用的各向异性导电膜。
背景技术
作为布线材料，使用在绝缘性粘结剂中分散有导电性颗粒的各向异性导电膜。作为各向异性导电膜，希望使用附着性好、低温快速固化的导电膜，因此提出了在自由基聚合性的丙烯酸系粘合剂中使用硅烷偶联剂的方案(专利文献1)。
作为各向异性导电膜中使用的硅烷偶联剂，已知有官能团不同的各种偶联剂。然而，无论何种硅烷偶联剂，都具有下述问题点：若将各向异性导电膜长期保存，则会因空气中的水分而水解，部分缩合而低聚，羟基减少，各向异性导电膜的附着力降低。
另一方面，在用各向异性导电膜导通连接的连接结构体中，存在因通电而由电极析出金属离子，发生迁移的情况，为了降低所述金属离子的浓度，防止迁移的发生，提出了使构成各向异性导电膜的绝缘性粘结剂中含有无机离子交换体的方案(专利文献2)。然而，即使含有无机离子交换体，也无法除去各向异性导电膜中多余的水分，各向异性导电膜在长期保存后的粘结性降低无法消除。
现有技术文献
专利文献
专利文献1：日本特开2002-167555号公报；
专利文献2：日本特开平10-245528号公报。
发明内容
发明要解决的课题
相对于上述现有技术，本发明的目的是：提供由水分引起的粘结性的降低得到抑制、保存稳定性优异的各向异性导电膜。
解决课题的手段
本发明人发现，若使构成各向异性导电膜的绝缘性粘结剂中含有特定的沸石，则水分被捕捉到沸石中，各向异性导电膜的保存稳定性提高。
即，本发明提供各向异性导电膜，其为导电性颗粒分散在含有硅烷偶联剂的绝缘性粘结剂中的各向异性导电膜，其中沸石的含量为1～20wt%，该沸石的平均微孔径为3～5埃，沸石的平均粒径小于导电性颗粒的平均粒径。
本发明还提供使用上述各向异性导电膜的各向异性导电连接方法、以及利用上述各向异性导电连接方法的各向异性导电连接器。
发明效果
本发明的各向异性导电膜在构成导电膜的绝缘性粘结剂中含有平均微孔径为3～5埃的沸石颗粒，故各向异性导电膜中多余的水分被吸附。因而，即使构成各向异性导电膜的绝缘性粘结剂中含有硅烷偶联剂，也可以防止其水解。因此，即使各向异性导电膜在长期保存后也可以维持充分的粘结强度。
另外，本发明的各向异性导电膜中所含的沸石颗粒的平均粒径小于各向异性导电膜中所含的导电性颗粒的平均粒径，故导电性颗粒引起的端子间的导通不会被沸石颗粒抑制，即使长期保存后仍可以得到初期的低导通电阻。
具体实施方式
下面具体地说明本发明。
本发明的各向异性导电膜的特征在于：绝缘性粘结剂中含有特定的微孔径的沸石。沸石是以铝硅酸盐为骨架的多孔结晶性物质。沸石包括：具有特定组成的合成沸石、天然沸石、以及以工业废弃物为原料生产的人工沸石，在本发明中，从控制微孔径或粒径的角度考虑，优选使用合成沸石。
合成沸石由铝硅酸盐的含水金属盐形成，通过将其含水金属盐加热脱水，形成成为空洞的微孔，使平均微孔径为3～5埃，更优选约3埃左右。通过使平均微孔径为约3埃，水分子被吸附在微孔中；通过使平均微孔径为约4埃，有抑制固化之虞的硫化氢、有降低粘结力之虞的乙醇被吸附；通过使平均微孔径为约5埃，有降低粘结力之虞的石蜡类或烯烃类被吸附。与此相对，若平均微孔径大于5埃，水分子以外的分子被过度吸附，故水分子的吸附性降低。因此，从使绝缘性粘结剂中多余的水分被吸收到合成沸石中，提高连接可靠性的角度考虑，优选使形成各向异性导电膜的绝缘性粘结剂中含有平均微孔径为3～5埃，更优选约3埃的合成沸石。
对合成沸石的种类没有特别限制，可以使用通常用作吸附剂、催化剂等的沸石。例如，可以使用A型沸石、八面沸石型沸石(X型、Y型沸石)、L型沸石、发光沸石型沸石、MFI型沸石(ZSM-5型沸石)、8型沸石等。合成沸石的具体例子有分子筛3A、4A、5A(Union昭和(株)制)等。
在本发明中，使沸石的平均粒径小于各向异性导电膜中所含的导电性颗粒的平均粒径。优选使沸石的平均粒径为各向异性导电膜中所含的导电性颗粒的平均粒径的10～80%。这是因为：若沸石的平均粒径为导电性颗粒的平均粒径以上，则在各向异性导电膜压合时难以将导电性颗粒充分挤入，连接电阻变大。具体来说，沸石的优选平均粒径为0.1μm～8μm，导电性颗粒的优选平均粒径为1μm～10μm。需说明的是，若使沸石的平均粒径为5μm以下，更容易使导电性颗粒的平均粒径大于沸石的平均粒径，与不含沸石颗粒的情况相比，更容易防止连接电阻变大。
使各向异性导电膜中沸石的含量为1～20wt%，优选5～15wt%。若沸石的含量过少，则无法充分获得沸石对水分的吸附效果；反之，若沸石的含量过多，则连接电阻升高。
本发明的各向异性导电膜除了绝缘性粘结剂含有硅烷偶联剂，分散有沸石之外，对绝缘性粘结剂的组成、其中分散的导电性颗粒没有特别限制。例如，绝缘性粘结剂可以由成膜树脂、液状环氧化合物(固化成分)或者丙烯酸单体(固化成分)、固化剂等与硅烷偶联剂构成。
此处，成膜树脂例如有苯氧基树脂、环氧树脂、不饱和聚酯树脂、饱和聚酯树脂、聚氨酯树脂、丁二烯树脂、聚酰亚胺树脂、聚酰胺树脂、聚烯烃树脂等，可以将2种以上上述树脂并用。其中，从制膜性、加工性、连接可靠性的观点考虑，可以优选使用苯氧基树脂。
液状环氧化合物例如有双酚A型环氧化合物、双酚F型环氧化合物、酚醛清漆型环氧化合物、它们的改性环氧化合物、脂环式环氧化合物等，可以将2种以上上述化合物并用。这种情况下，固化剂例如有多胺、咪唑等阴离子系固化剂或锍盐等阳离子系固化剂、酚系固化剂等潜在性固化剂。
丙烯酸单体例如有(甲基)丙烯酸乙酯等。这种情况下，固化剂(自由基聚合引发剂)例如有有机过氧化物、偶氮二丁腈等。
硅烷偶联剂例如有环氧系硅烷偶联剂、丙烯酸系硅烷偶联剂等。这些硅烷偶联剂主要为烷氧基硅烷衍生物。
绝缘性粘结剂中可以根据需要配合填充剂、软化剂、促进剂、防老剂、着色剂(颜料、染料)、有机溶剂、离子捕捉剂等。
另一方面，作为绝缘性粘结剂中分散的导电性颗粒，可以使用金属颗粒、在树脂颗粒表面镀有金属的颗粒等。
关于导电性颗粒相对于绝缘性粘结剂的配合比例，若导电性颗粒过少，则导通可靠性降低；若过多则各向异性导电性降低，因此优选使导电性颗粒为0.1～20wt%，更优选为0.2～10wt%。
各向异性导电膜可以通过使导电性颗粒分散在上述绝缘性粘结剂中，将所得分散物在离型膜上制膜来制备。
本发明的各向异性导电膜与以往的各向异性导电膜同样，可以配置在柔性基板、刚性基板、电子部件等的要连接的端子之间，一边对端子间进行加压，一边进行加热、UV照射等，用于将端子间电气、机械连接的各向异性导电连接，由此能够制备具有高连接可靠性的各向异性导电连接器。本发明也包含该连接器。
实施例
下面通过实施例更具体地说明本发明。
比较例1
将60重量份苯氧基树脂(YP50，新日化Epoxy制造(株)制)与35重量份自由基聚合性树脂(EB-600，Daicel Cytec(株)制)、2重量份反应引发剂(Perhexa C、日油(株)制)、2重量份硅烷偶联剂(A-187、Momentive Performance Materials(同)制)混合，得到绝缘性粘结剂。向其中分散平均粒径5μm的导电性颗粒(AUL705，积水化学工业(株)制)，涂布在剥离膜上，用烘箱干燥，制备导电性颗粒密度为10000个/mm2、厚15μm的各向异性导电膜。
实施例1～5
减压干燥有效微孔径为3埃的沸石(Zeorum A-3，Tosoh(株)制)，使水分挥发，粉碎后用筛子进行分级。所得沸石颗粒的平均粒径为3.5μm。
除将该沸石颗粒按表1所示比例加入绝缘性粘结剂中以外，与比较例1同样操作，制备实施例1～5的各向异性导电膜。
实施例6
减压干燥有效微孔径为4埃的沸石(Zeorum A-4，Tosoh(株)制)，使水分挥发，粉碎后用筛子进行分级，制备平均粒径3.0μm的沸石颗粒。
除将该沸石颗粒按表1所示比例加入绝缘性粘结剂中以外，与比较例1同样操作，制备实施例6的各向异性导电膜。
实施例7
减压干燥有效微孔径为5埃的沸石(Zeorum A-5，Tosoh(株)制)，使水分挥发，粉碎后用筛子进行分级，制备平均粒径3.0μm的沸石颗粒。
除将该沸石颗粒按表1所示比例加入绝缘性粘结剂中以外，与比较例1同样操作，制备实施例7的各向异性导电膜。
比较例2
减压干燥有效微孔径为3埃的沸石(Zeorum A-3，Tosoh(株)制)，使水分挥发，粉碎后用筛子进行分级，制备平均粒径10μm的沸石颗粒。
除将该沸石颗粒按表1所示比例加入绝缘性粘结剂中以外，与比较例1同样操作，制备比较例2的各向异性导电膜。
比较例3
除含有5.0 wt%平均粒径3.5μm的二氧化硅颗粒(HPS-3500，东亚合成(株)制)代替沸石以外，与实施例1同样操作，制备比较例3的各向异性导电膜。
评价
对于实施例1～7和比较例1～3中得到的各向异性导电膜，如下测定(a)连接电阻和(b)粘结强度。另外，将各向异性导电膜在85℃、85%RH放置500小时进行保存稳定性加速试验后，同样地测定(a)连接电阻和(b)粘结强度。这些结果示于表1中。
(a) 连接电阻的测定方法
准备作为评价用基材的Sony Chemical＆Information Device公司(株)制COF (50μm螺距、Cu 8μm厚-镀Sn、聚酰亚胺38μm厚-Sperflex基材)和评价用ITO β-玻璃。以使用缓冲材料150μm厚Teflon (注册商标)的模具宽度(ツール幅)1.5mm的临时压合机，在70℃、1MPa、1秒下将切成1.5mm的各向异性导电膜临时压合到ITO β-玻璃上，接下来，将COF用相同压合机在80℃、0.5MPa、0.5秒下临时固定，最后在190℃、3MPa、10秒下用模具宽度1.5mm的正式压合机压合，制成组装体。
使用数字式万用表(横河电机(株)制)以四端子法(电流1mA)测定该组装体的连接电阻值。
(b) 粘结强度的测定方法
使用无碱β-玻璃代替ITO β-玻璃，与(a)同样地制作组装体，用拉伸试验机(AND公司制)测定该组装体的粘结强度。这种情况下，测定速度为50mm／秒，测定将COF提升90°时的粘结强度。
表1
Figure 2012800003761100002DEST_PATH_IMAGE002
由表1可知，不含沸石的比较例1的各向异性导电膜在保存稳定性加速试验后粘结强度大幅降低；含有粒径比导电性颗粒大的沸石的比较例2的各向异性导电膜在压合时未将导电性颗粒充分挤入，因此连接电阻高；含有二氧化硅代替沸石的比较例3的各向异性导电膜在保存稳定性加速试验后的粘结强度也大幅降低；与此相对，含有粒径比导电性颗粒小的沸石的实施例1～7的各向异性导电膜在保存稳定性加速试验后粘结强度也高，连接电阻非常低，特别是沸石的平均微孔径为3埃、沸石的含有量为5～15wt%的实施例2、4的各向异性导电膜，连接电阻低，保存稳定性加速试验后的粘结强度优异，连接可靠性高。

Claims (6)

1. 各向异性导电膜，其为导电性颗粒分散在含有硅烷偶联剂的绝缘性粘结剂中的各向异性导电膜，沸石的含量为1～20wt%，
该沸石的平均微孔径为3～5埃，
沸石的平均粒径小于导电性颗粒的平均粒径。
2. 权利要求1记载的各向异性导电膜，其中沸石的含量为5～15wt%。
3. 权利要求1或2记载的各向异性导电膜，其中沸石的平均粒径为导电性颗粒的平均粒径的10%～80%。
4. 权利要求1～3任一项中记载的各向异性导电膜，其中沸石的平均粒径为0.1μm～8μm，导电性颗粒的平均粒径为1μm～10μm。
5. 各向异性导电连接方法，其是将权利要求1～4任一项中记载的各向异性导电膜配置在相向的端子间，对端子间进行加热加压而连接的。
6. 各向异性导电连接器，其使用权利要求1～4任一项中记载的各向异性导电膜将电子部件之间各向异性导电连接。
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