CN107383778A - 一种抗静电耐高温的环氧胶黏剂及印制电路用层压板 - Google Patents

一种抗静电耐高温的环氧胶黏剂及印制电路用层压板 Download PDF

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CN107383778A
CN107383778A CN201710602744.4A CN201710602744A CN107383778A CN 107383778 A CN107383778 A CN 107383778A CN 201710602744 A CN201710602744 A CN 201710602744A CN 107383778 A CN107383778 A CN 107383778A
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component
epoxy adhesive
laminate
bisphenol
nano
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杨菲
师剑英
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SHAANXI SHENGYI SCI TECH Co Ltd
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SHAANXI SHENGYI SCI TECH Co Ltd
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Abstract

本发明公开了一种抗静电耐高温的环氧胶黏剂及印制电路用层压板。本发明提出一种抗静电耐高温的环氧胶黏剂，包含以下组分：组分A：纳米级半导体材料与非离子型表面活性剂的混合物；组分B：双酚A型环氧树脂；组分C：复合型固化剂；组分D：咪唑类化合物，还可包括组分E：无机填料，所述无机填料包括氢氧化铝和氧化锑中的一组或两种混合物。本发明的环氧胶黏剂采用纳米级导电氧化锌，其与非离子型表面活性剂具有极强的协同降低电阻率效应，在大大减少纳米级导电氧化锌使用量的情况下，可以实现降低电阻率，而且以上二者协同，不会出现板材处于高温条件下，非离子表面活性剂迁移甚至渗出进而导致物理性能下降等问题。

Description

一种抗静电耐高温的环氧胶黏剂及印制电路用层压板
技术领域
本发明涉及印制电路用层压板领域，具体涉及制备一种抗静电耐高温的环氧胶黏剂及印制电路用层压板。
背景技术
作为电子产品不可或缺的基材，覆铜板的应用领域非常广阔。当其用于电能表、万用表等精密性电子产品中时，就对其抗静电性要求非常高。目前传统的覆铜板由于使用了环氧树脂、玻璃布等具有极高表体电阻率的高绝缘性材料，会使精密性电子产品在运行过程中不断积聚静电荷并且释放缓慢，导致大量静电荷最终堆积在产品内部，形成很高的静电场，进而会造成产品发生局部放电现象，影响精密仪器的准确性和精密性，严重时甚至导致产品局部击穿，造成电子元器件烧毁，产品失效。
发明内容
为了消除印制电路用层压板用于精密电子产品中工作时产生的静电，赋予印制电路用层压板一定的抗静电性，满足印制电路用层压板的耐高温性，本发明提供了一种具有抗静电耐高温特性的胶黏剂及采用该胶黏剂制成的印制电路用层压板，涉及到的金属箔包括但不限于铜箔、铝箔、铜铝箔等。
本发明采用如下技术方案：
本发明提供一种抗静电耐高温的环氧胶黏剂，包含以下组分：
组分A：纳米级半导体材料与非离子型表面活性剂的混合物；
组分B：双酚A型环氧树脂；
组分C：复合型固化剂；
组分D：咪唑类化合物。
特别的，以有机固形物质量份数计，上述的胶黏剂包含以下组分，组分 A：10～50份，组分B：50～90份，组分C：2～15份，组分D：0.1～0.5份，其中组分A中纳米级半导体材料与非离子型表面活性剂的质量比为 10:1～4:1。
本发明的环氧胶黏剂还包括组分E：无机填料，所述无机填料包括氢氧化铝和氧化锑中的一种或两种混合物。
其中，以有机固形物质量份数计，所述组分E为3～10份。
本发明的双酚A型环氧树脂的溴含量在质量分数20％～35％之间，所述双酚A型环氧树脂包括环氧当量为400～500eq/100g的双酚A型环氧树脂，或环氧当量为300～400eq/100g双酚A型环氧树脂和环氧当量为 450～500eq/100g的双酚A型环氧树脂的混合物；所述纳米级半导体材料包括纳米级导电氧化锌，所述纳米级导电氧化锌的粒径为100nm～1μm，白度＞98，所述纳米级导电氧化锌颗粒表面不经过偶联剂处理。
本发明的非离子型表面活性剂包括选自如下结构式(α)的化合物或化合物的混合物：
式中，R表示-H、-CH3、-C2H5、-COH、-COCH3、-COC2H5中的一种， n表示1～4的整数。
本发明的复合型固化剂包括双氰胺与酚醛树脂，所述酚醛树脂包括苯酚型酚醛树脂、双酚A型环氧树脂、含氮型酚醛树脂及含磷型酚醛树脂中的一种或多种。
本发明还提供一种预浸料，所述预浸料包括基材，所述基材上附着有上述环氧胶黏剂。
在此基础上，本发明还提供一种层压板，所述层压板包括多个叠合的预浸料，所述预浸料包括基材，所述基材上附着有环氧胶黏剂。
本发明还提供一种印制电路用层压板，所述印制电路用层压板包括多个叠合的预浸料，每个预浸料的单面或双面覆有金属箔，所述预浸料包括基材，所述基材上附着有环氧胶黏剂。
与现有技术相比，本发明的有益效果是：
1、本发明的环氧胶黏剂采用纳米级导电氧化锌，其与非离子型表面活性剂具有极强的协同降低电阻率效应，在大大减少纳米级导电氧化锌使用量的情况下，可以实现降低电阻率，而且以上二者协同，不会出现板材处于高温条件下，非离子表面活性剂迁移甚至渗出进而导致物理性能下降等问题；
2、本发明的环氧胶黏剂采用含羟基和醚键结构的表面活性剂，其耐高温性能好，能够与环氧树脂交联，交联后剩余的羟基和醚键能够赋予环氧胶黏剂低电阻率特性，故制备的印制电路用层压板体积电阻率较低，抗静电性好；
3、本发明的环氧胶黏剂采用双酚A型环氧树脂为主体树脂，该树脂组合物的预浸料、层压板、印制电路用层压板，具有高耐热性、高弯曲强度、较高的玻璃化转变温度，并具有优良的耐化学性及机械加工性能。同时树脂中的溴与无机填料协同作用，又赋予该树脂组合物的预浸料、层压板、印制电路用层压板优异的阻燃性。
具体实施方式
本发明的纳米级导电氧化锌的粒径在100nm～1μm之间，否则粒径太小在树脂中很难分散均匀，粒径分布太宽会导致电阻率降低不明显，达不到降低高耐热抗静电环氧树脂组合物电阻率的效果，所述的纳米级导电氧化锌颗粒表面不经过偶联剂的处理若处理过，则偶联剂会使纳米级导电氧化锌颗粒“有机化”，有机化后的纳米级导电氧化锌颗粒会被环氧树脂完全包裹，不能发挥其降低电阻率的作用。与常用的导电粉体相比，纳米级导电氧化锌为白色抗静电粉末，其粒度分布均匀，具有良好的流动性和分散性，且其结构中每个粒子都是独立半导体，因此分散在树脂中时粉体结构不容易被破坏，制成的高耐热抗静电环氧胶黏剂的电阻值稳定。同时，其具有吸收紫外光的功能。
本发明所述的纳米级导电氧化锌为半导体材料，但若单独使用，则其降低电阻率效果不明显，而采用非离子型表面活性剂与其复合，可在纳米级导电氧化锌表面形成更多的吸水性基团如羟基、醚键等，从而降低电阻率，因此高耐热抗静电环氧树脂组合物的电阻率可明显降低。
本发明的非离子型表面活性剂由于结构中存在苯环，所以其骨架在保持一定柔性的同时刚性相对较好，故非离子型表面活性剂耐热性较好。而其结构中的羟基则能能够赋予高耐热抗静电环氧树脂组合物较低电阻。但是由于非离子型表面活性剂用量必须严格控制，一旦过大则会随着湿度的增加而逐渐迁移至材料表面，而与纳米级导电氧化锌复合使用，其用量则可以大大降低，又能满足树脂组合物的低电阻特性。故组分A的用量以10～50重量份为宜，并且，为保证纳米级半导体材料与非离子型表面活性剂良好的协同降电阻特性以及避免非离子型表面活性剂的析出，纳米级半导体材料与非离子型表面活性剂的重量比在10:1～4:1之间为宜。
本发明的双酚A型环氧树脂的溴含量需控制在20～35％之间，以满足树脂组合物阻燃的需求。该B组分的用量以50～90重量份为宜，最佳为60～80。
本发明中的组分C，即复合型固化剂，具体为双氰胺与一种或多种酚醛树脂的混合物，进一步的，酚醛树脂可以为苯酚型酚醛树脂、双酚A型环氧树脂、含氮型酚醛树脂、含磷型酚醛树脂。优先选用苯酚型酚醛树脂和双酚A型酚醛树脂，因为其与双酚A型环氧树脂相容性较好并且交联程度更好。该C组分用量以2～15重量份为宜，低于2重量份，固化物玻璃化转变温度提高不多，超过15重量份固化物耐热性变差。
本发明中的D组分，作为树脂组合物的固化物促进剂，可以是2-甲基咪唑、2-乙基-4-甲基咪唑，2-苯基咪唑中的至少一种化合物。
本发明可还含有E组分，即无机填料。所述无机填料，主要用来调节树脂组合物的物理性质，该无机填料为氢氧化铝、氧化锑、二氧化硅、二氧化酶、碳酸钙、滑石粉等通用的无机填充剂，该无机填充剂可依据目的而作选择，尤其是氢氧化铝和氧化锑可以作为溴类树脂的阻燃助剂，可优先选用。无机填料的用量相对环氧组合物中的有机固形物来讲，最好为3～10重量份，最佳为5～8重量份。
本发明的组分含量中的有机固形物是指固体形态的有机聚合物。
本发明的基材包括玻璃纤维布或无纺布。
本发明组分B溴含量控制在15～23％，锑含量控制在2～4％。
本发明的金属箔包括铜箔、铝箔、铜铝箔等，其材质不限。例如采用铜箔，则印制电路用层压板即为覆铜箔。
下面结合具体实施方式对本发明进行详细说明，但本发明并非局限在实施例范围，下文中无特别说明，其“份”代表质量份，其％代表“质量％”。
本发明环氧胶黏剂的常规制备方法为：先将复合型固化剂放入，加入液态溶剂，如二甲基甲酰胺，搅拌至完全溶解后，再加入树脂和非离子型表面活性剂，加入固化促进剂咪唑类化合物，继续搅拌至均匀状态，最后加入纳米级导电氧化锌，用丙酮适当调整溶液的固体含量至65％～75％，即可制得高耐热抗静电环氧胶黏剂。使用该胶黏剂浸透玻璃纤维布或无纺布等织物，将浸好的玻璃纤维布或无纺布在170℃的烘箱中加热3分钟即制成预浸料。
本发明中的层压板包括加热和加压、使两片或两片以上的预浸料粘合在一起而制成的层压板、粘合在层压板的一面或两面的金属箔。所述层压板是使用上述的预浸料8片和一盎司(35μm)的金属箔2片叠合在一起，通过热压机中层压，从而压制成双面金属箔的层压板。所述层压板须满足以下要求：①层压时料温70～130℃时升温速率应控制在1.5～2.5℃/min；②层压的压力设置，外层料温100～130℃时施加满压，满压压力为50kgf/cm2左右；③固化时控制粘结片温度在170℃，保温40min。
按照上述方法，采用如下实施例及对比例中的配比，覆以金属箔，制成层压板(8张预浸料)，测其表体电阻率、热导率、耐热性、吸水性等性能。其中，表中各个符号代表：
(A1)纳米级导电氧化锌
EC-400S(上海力慎化学品有限公司商品名)；
(A2)主链含有端羟基或醚键、苯环的非离子表面活性剂
(A2-1)GWC-8010(深圳市特斯顿科技有限公司商品名)；
(A2-2)T-8006(深圳市特斯顿科技有限公司商品名)；
(B)双酚A型环氧树脂
(B-1)SQEB-450A80(山东圣泉化工股份有限公司商品名)；
(B-2)GEBR556A75(宏昌电子材料股份有限公司商品名)；
(C)复合型固化剂
(C-1)双氰胺(宁夏大荣化工冶金有限公司商品名)；
(C-2)PHL6635(韩国翰森特种化学公司商品名)；
(C-3)PS 6313(日本群荣化学工业株式会社商品名)；
(D)固化促进剂：2-苯基咪唑(日本四国化成株式会社商品名)
(E)无机填料
(E-1)氢氧化铝(纯度99％以上)
(E-2)二氧化硅(纯度99％以上)
表1组合物的配方(一)(质量份)
实施例1 实施例2 实施例3 实施例4 实施例5 实施例6
A1 45 30 32 30 30 9
A2-1 5 3 8 5
A2-2 5 1
B-1 65 65 65 90
B-2 50 65
C-1 1 1 1 1 1 3
C-2 12 12 12 12 12 8
D 0.1 0.1 0.1 0.1 0.1 0.1
E-1
E-2
表2组合物的配方(二)(质量份)
实施例7 实施例8 实施例9 实施例10 实施例11 实施例12
A1 30 30 30 30 24 24
A2-1 3 3 4
A2-2 5 2 6 6 2
B-1 50 68
B-2 65 65 68 68
C-1 1 0.3 1 4 1 1
C-2 14 1.7 12 8 13 13
D 0.5 0.1 0.1 0.1 0.1 0.1
E-1 5 1 5 1 1
E-2 5 2 1 5 5
表3组合物的配方(三)(质量份)
对比例1 对比例2 对比例3 对比例4 对比例5 对比例6
A1 4 4 50 50 30
A2-1 2 4 5 5 5
A2-2
B-1 45 30 100 70
B-2 45 10 70
C-1 1 2 1 2 1 1
C-2 13 13 12 12
C-3 12 8
D 0.1 0.1 0.1 0.1 0.1 0.1
E-1 3 3 3 3 3 3
E-2 3 3 3 3 3 3
表4特性评估(一)
实施例1 实施例2 实施例3 实施例4 实施例5 实施例6
表面电阻率/MΩ 8.14E+04 6.25E+04 4.12E+04 9.52E+03 5.89E+04 6.23E+03
体积电阻率/MΩ 9.89E+05 7.36E+05 5.21E+05 8.35E+04 6.42E+05 2.36E+04
耐浸焊性(分层) ○ ○ ○ ○ ○ ○
热导率/(W/(m.k)) 0.58 0.58 0.59 0.58 0.57 0.56
耐燃烧性 V-0 V-0 V-0 V-0 V-0 V-0
吸水性/％ 0.18 0.16 0.19 0.15 0.14 0.16
弯曲强度/(N/mm2) 630 620 613 619 614 613
玻璃化转变温度/℃ 116 112 119 117 115 112
表5特性评估(二)
实施例7 实施例8 实施例9 实施例10 实施例11 实施例12
表面电阻率/MΩ 5.96E+03 6.35E+04 4.23E+04 2.15E+04 5.76E+03 6.52E+03
体积电阻率/MΩ 8.63E+04 7.12E+05 5.69E+05 6.05E+05 6.35E+04 5.89E+04
耐浸焊性(分层) ○ ○ ○ ○ ○ ○
热导率/(W/(m.k)) 0.58 0.60 0.62 0.61 0.60 0.60
耐燃烧性 V-0 V-0 V-0 V-0 V-0 V-0
吸水性/％ 0.19 0.15 0.14 0.17 0.13 0.16
弯曲强度/(N/mm2) 612 625 617 635 625 615
玻璃化转变温度/℃ 118 120 121 117 118 119
表6特性评估(三)
对比例1 对比例2 对比例3 对比例4 对比例5 对比例6
表面电阻率/MΩ 9.56E+09 6.65E+08 4.25E+04 2.15E+08 6.75E+08 6.28E+08
体积电阻率/MΩ 8.63E+10 7.28E+09 5.94E+05 6.05E+09 5.36E+09 3.57E+09
耐浸焊性(分层) ○ × × ○ × ×
热导率/(W/(m.k)) 0.56 0.54 0.55 0.54 0.54 0.53
耐燃烧性 V-0 V-0 V-0 V-0 V-0 V-0
吸水性/％ 0.12 0.14 0.20 0.17 0.25 0.28
弯曲强度/(N/mm2) 617 619 612 621 610 608
玻璃化转变温度/℃ 112 109 90 117 117 115
击穿电压/kV 40 8 15 29 35 37
以上特性的测试方法如下：
(a)表体电阻率
按照IPC-TM-650 2.5.17.1所规定的方法进行测试。
(b)热导率
按照IPC-TM-650 2.6.547所规定的方法进行测试。
(c)耐浸焊性
按照IPC-TM-650 2.4.13.1所规定的方法进行测试，表中的符号○表示无变化，×表示发生分层
(d)耐燃烧性
依据UL94法测定。
(e)吸水性
按照IPC-TM-650 2.6.2.1所规定的方法进行测试。
(f)弯曲强度
按照IPC-TM-650 2.4.4所规定的方法进行测试。
(g)玻璃化转变温度
根据差示扫描量热法，按照IPC-TM-650 2.4.25所规定的方法进行测试。
综上述结果可知，依据本发明制备的覆铜板可达到较低表体电阻率(良好的抗静电性)、耐热性好、阻燃性好、导热率较高、吸水性适中的功效，同时弯曲强度高，机械加工性好。本发明充分利用纳米级导电氧化锌和非离子型表面活性剂之协同降低电阻率特性，将板材的表体电阻率控制在 103～105MΩ之间，从而达到抗静电的功效。
从对比例中可以看出，缺失A1或A2中的任何一个，该层压板的体积电阻率或表面电阻率均不能达到103～105MΩ，不能达到抗静电效果。
以上所述，仅为本发明的较佳实施例，对于本领域的普通技术人员来说，可以根据本发明的技术方案和技术构思作出其他各种相应的改变和变形，而所有这些改变和变形都应属于本发明权利要求的保护范围。

Claims (10)

1.一种抗静电耐高温的环氧胶黏剂，其特征在于，包含以下组分：
组分A：纳米级半导体材料与非离子型表面活性剂的混合物；
组分B：双酚A型环氧树脂；
组分C：复合型固化剂；
组分D：咪唑类化合物。
2.如权利要求1所述环氧胶黏剂，其特征在于，以有机固形物质量份数计，包含以下组分，组分A：10～50份，组分B：50～90份，组分C：2～15份，组分D：0.1～0.5份，其中组分A中纳米级半导体材料与非离子型表面活性剂的质量比为10:1～4:1。
3.如权利要求1所述环氧胶黏剂，其特征在于，所述环氧胶黏剂还包括组分E：无机填料，所述无机填料包括氢氧化铝和氧化锑中的一种或两种混合物。
4.如权利要求3所述环氧胶黏剂，其特征在于，以有机固形物质量份数计，所述组分E为3～10份。
5.如权利要求1所述环氧胶黏剂，其特征在于，所述双酚A型环氧树脂的溴含量在质量分数20％～35％之间，所述双酚A型环氧树脂包括环氧当量为400～500eq/100g的双酚A型环氧树脂，或环氧当量为300～400eq/100g双酚A型环氧树脂和环氧当量为450～500eq/100g的双酚A型环氧树脂的混合物；所述纳米级半导体材料包括纳米级导电氧化锌，所述纳米级导电氧化锌的粒径为100nm～1μm，白度＞98，所述纳米级导电氧化锌颗粒表面不经过偶联剂处理。
6.如权利要求1所述环氧胶黏剂，其特征在于，所述非离子型表面活性剂包括选自如下结构式(α)的化合物或化合物的混合物：
式中，R表示-H、-CH3、-C2H5、-COH、-COCH3、-COC2H5中的一种，n表示1～4的整数。
7.如权利要求1所述环氧胶黏剂，其特征在于，所述复合型固化剂包括双氰胺与酚醛树脂，所述酚醛树脂包括苯酚型酚醛树脂、双酚A型环氧树脂、含氮型酚醛树脂及含磷型酚醛树脂中的一种或多种。
8.一种预浸料，其特征在于，所述预浸料包括基材，所述基材上附着有权利要求1或2所述环氧胶黏剂。
9.一种层压板，其特征在于，所述层压板包括多个叠合的预浸料，所述预浸料包括基材，所述基材上附着有权利要求1或2所述环氧胶黏剂。
10.一种印制电路用层压板，其特征在于，所述印制电路用层压板包括多个叠合的预浸料，每个预浸料的单面或双面覆有金属箔，所述预浸料包括基材，所述基材上附着有权利要求1或2所述环氧胶黏剂。
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JP7331248B2 (ja) 2019-10-22 2023-08-22 エルジー・ケム・リミテッド 半導体用接着剤組成物およびその硬化物を含む半導体用接着フィルム

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