CN105778505A - 一种有机硅树脂组合物以及使用它的白色预浸料和白色层压板 - Google Patents

一种有机硅树脂组合物以及使用它的白色预浸料和白色层压板 Download PDF

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CN105778505A
CN105778505A CN201410829372.5A CN201410829372A CN105778505A CN 105778505 A CN105778505 A CN 105778505A CN 201410829372 A CN201410829372 A CN 201410829372A CN 105778505 A CN105778505 A CN 105778505A
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white
resin composition
prepreg
silicon resin
mol ratio
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CN201410829372.5A
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CN105778505B (zh
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唐国坊
叶素文
孙鹏
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Shengyi Technology Co Ltd
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Shengyi Technology Co Ltd
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Priority to CN201410829372.5A priority Critical patent/CN105778505B/zh
Priority to TW104111511A priority patent/TWI530533B/zh
Priority to KR1020177020793A priority patent/KR101909851B1/ko
Priority to JP2017534733A priority patent/JP6510650B2/ja
Priority to EP15871613.4A priority patent/EP3239245B1/en
Priority to US15/539,479 priority patent/US10336905B2/en
Priority to PCT/CN2015/080533 priority patent/WO2016101537A1/zh
Publication of CN105778505A publication Critical patent/CN105778505A/zh
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Abstract

本发明提供了一种有机硅树脂组合物以及使用它的预浸料和层压板。所述预浸料通过将含有缩合型硅树脂、催化剂、助剂、白色填料和溶剂作为必须成分的有机硅树脂组合物胶液浸渍于增强材料如片状玻纤纤维基材中，然后干燥而得。该预浸料通过硅树脂利用缩合反应聚合交联而成网状结构。由于有机硅树脂具有超高耐热及耐黄变性，本发明将硅树脂代替传统的有机树脂应用在LED白色覆铜板中，不但能满足LED的高耐热性要求，还可替代陶瓷基板成为新型散热基板的基材。

Description

一种有机硅树脂组合物以及使用它的白色预浸料和白色层压板
技术领域
本发明涉及缩合型硅树脂代替传统的有机树脂得到的有机硅树脂组合物以及使用它的白色预浸料、层压板及覆铜板，其具有高耐热、高反射及优越的耐热老化和耐紫外光照老化性能。
背景技术
发光二极管(LED)是一种可以将电能直接转换为光能的半导体器件，具有节能、环保和寿命长等特点，LED的迅速发展和广泛应用，将引发照明领域的一场革命。
而安装LED的PCB基板，在加工和使用过程中，由于LED具有发光的特性，因此树脂层表面的光反射率应该越大越好；而且其印制线路板用覆铜板，在制作芯片LED的过程中要经过各种各样的受热过程；芯片LED在使用时，LED元件本身也会发热，LED发光时也会产生热应力，因而要求用于LED的白色覆铜板具有高的耐热性。
除了需要具有常规CCL的一般性能要求外，LED白色覆铜板还需具备一些特殊性能。LED用白色CCL不仅需要高的初态反射率，而且还需要它具备长期的保持反射率的特性(包括高热辐射板面不变色性，长期紫外线照射板面不变色性)，同时还需要具有高耐热性，以及高温下的高刚性。使白色CCL获得高的耐紫外线变色性及耐热变色性，主要依靠树脂组成中多种成分的性能改进或创新，来实现这一特殊性能的。
有机硅树脂的结构中既含有有机基团，又含有无机基团，这种特殊的组成和分子结构使得硅树脂兼有有机物的特性与无机物的功能于一身。有机硅树脂是热固性树脂，在高温热氧化作用时，仅仅发生侧链有机基的断裂，分解而逸出其氧化物，而主链的硅氧键很少破坏，最终生成-O-Si-O-形式的聚合物，其Si-O硅氧键键能在373KJ/mol，故其耐热性远优于一般有机树脂。甲基硅氧烷对紫外光几乎不吸收，含PhSiO1.5或Ph2SiO链节的硅氧烷也仅吸收280nm以下的光线，故有机硅树脂具有非常好的耐候性。此外，有机硅树脂具有突出的耐候性，是任何一直有机树脂所望尘莫及的，即使在紫外线强烈照射下，硅树脂耐黄变也非常优越。
因此，与一般的树脂相比，有机硅树脂具有优越的耐高低温、耐气候老化、电气绝缘、耐臭氧、阻燃和憎水等独特性能。
发明内容
鉴于有机硅树脂的超高耐热、耐黄变性以及耐候性，本发明的目的之一在于提供一种有机硅树脂组合物，使用该有机树脂组合物得到的白色预浸料、层压板以及覆铜板具有优异的耐热性、耐候性以及耐黄变性。
为了实现上述目的，本发明采用了如下技术方案：
一种有机硅树脂组合物，所述有机硅树脂组合物，包括：
所述白色填料的含量例如为8重量份、12重量份、16重量份、20重量份、24重量份、28重量份、32重量份、36重量份、40重量份、44重量份、48重量份、52重量份或56重量份。
所述催化剂的含量例如为0.0005重量份、0.001重量份、0.005重量份、0.01重量份、0.05重量份、0.1重量份、0.3重量份、0.5重量份、1.0重量份、1.5重量份或2.0重量份。
所述助剂的含量例如为0.5重量份、1重量份、2重量份、3重量份、4重量份、5重量份、6重量份、7重量份、8重量份或9重量份。
在本发明中，所述缩合型硅树脂主要为甲基硅树脂、甲基苯基硅树脂或苯基硅树脂中的任意一种或者至少两种的混合物。
在本发明中，所述缩合型硅树脂为脱水缩合、脱醇缩合或脱氢缩合中的任意一种，其反应结构如下所示：
在本发明中，所述缩合型硅树脂为R/Si＝1.0～1.7(摩尔比)(例如1.1、1.2、1.3、1.4、1.5、1.6或1.7)和Ph/(Me+Ph)＝0～1.0(摩尔比)(例如0.1、0.2、0.3、0.4、0.5、0.6、0.7、0.8、0.9或1.0)的甲基硅树脂、甲基苯基硅树脂或苯基硅树脂中的任意一种或者至少两种的混合物，其中Ph代表苯基基团，Me代表甲基基团，R代表有机官能团-CH3、-Ph、-OCH3、-OCH2CH3、-OH或-H。在缩合型硅树脂中，R/Si(摩尔比)过小，Ph/Si(摩尔比)过低，硅树脂固化后柔软性差，漆膜变硬，而R/Si(摩尔比)过大，Ph/Si(摩尔比)过高层压板硬度低，固化慢，热固性低，故所述缩合型硅树脂优选R/Si＝1.2～1.7(摩尔比)且Ph/(Me+Ph)＝0.2～0.6(摩尔比)的甲基苯基硅树脂。
在本发明中，所述白色填料为氧化铝、二氧化钛、氢氧化铝、二氧化硅或氧化锌中的任意一种或者至少两种的混合物，优选二氧化钛。
根据本发明，所述催化剂是环烷酸锌、环烷酸锡、环烷酸钴、环烷酸铁、环烷酸铈、羧酸锌、羧酸锡、羧酸钴、羧酸铁、羧酸铈、全氟磺酸、氯化磷腈、胺类、辛酸锌、异辛酸锌、季铵碱、钛酸酯或胍类化合物等中的任意一种或者至少两种的组合。
根据本发明，所述助剂为偶联剂或/和分散剂，所述偶联剂为硅烷偶联剂或/和钛酸酯偶联剂。
本发明所述的“包括”，意指其除所述组份外，还可以包括其他组份，这些其他组份赋予所述有机硅树脂组合物不同的特性。除此之外，本发明所述的“包括”，还可以替换为封闭式的“为”或“由……组成”。
例如，所述有机硅树脂组合物还可以含有各种添加剂，作为具体例，可以举出阻燃剂、抗氧剂、热稳定剂、抗静电剂、紫外线吸收剂、颜料、着色剂或润滑剂等。这些各种添加剂可以单独使用，也可以两种或者两种以上混合使用。
本发明的目的之二在于提供一种树脂胶液，其是将如上所述的有机硅树脂组合物溶解或分散在溶剂中得到。
作为本发明中的溶剂，没有特别限定，作为具体例，可以举出甲苯、二甲苯、正己烷、环己烷或异丙醇等。
本发明的目的之三在于提供一种白色预浸料，其包括增强材料及通过含浸干燥后附着在增强材料上的如上所述的有机硅树脂组合物。
本发明的白色预浸料通过硅树脂利用缩合反应聚合交联而成网状结构。
示例性的预浸料的制备方法为：
将缩合型硅树脂、催化剂、助剂、白色填料、溶剂以及任选地其他组分得到的有机硅树脂胶液浸渍于增强材料如片状玻纤纤维基材中，然后干燥而得。
本发明的目的之四在于提供一种白色层压板，所述白色层压板含有至少一张如上所述的白色预浸料，其通过将至少一张如上所述的预浸料加热加压成型得到。
本发明的目的之五在于提供一种白色覆铜箔层压板，所述白色覆铜箔层压板包括至少一张叠合的如上所述的白色预浸料及压覆在叠合后的预浸料的一侧或两侧的铜箔。
与已有技术相比，本发明具有如下有益效果：
本发明利用有机硅的高耐热性、优越的耐候性及耐紫外光照，替代传统树脂不耐热、易黄变等缺点，通过将缩合型硅树脂、催化剂、白色填料、助剂以及任选地其他组分复配，得到具有优异的耐热性、耐候性以及耐黄变性的有机硅树脂组合物，同时与加成型硅树脂相比，缩合型硅树脂与铜箔具有更好的剥离强度，将缩合型硅树脂应用在LED白色覆铜板中，使其同样具有优异的耐热性、耐候性以及耐黄变性。
此外，本发明将有机硅树脂代替传统的有机树脂应用在LED白色覆铜板中，不但能满足LED的高耐热性要求，而且还可克服陶瓷基板存在的成本高、加工性差的缺点，在小型、薄型的LED照明产品、液晶显示器背光源等方面的散热基板上得到广泛的应用，是一种可替代陶瓷基板的新型散热基板的基材。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案。
实施例1
称取R/Si＝1.1(摩尔比)，Ph/(Me+Ph)＝0(摩尔比)的甲基硅树脂100份，溶于100份甲苯溶剂中，待溶解完全后，用精准取液器量取0.003份的辛酸锌催化剂和0.5份硅烷偶联剂γ-缩水甘油醚氧丙基三甲氧基硅烷(美国，道康宁制造)，投入到硅树脂溶液中，搅拌均匀后，添加5.5份白色颜料金红石型二氧化钛，室温下搅拌1h，乳化20min，得白色硅树脂胶液。
用此白色硅树脂清漆浸渍重量为104g/cm2的玻璃纤维布，在110℃干燥10min得到树脂含量为58％的预浸料。将8片预浸料重叠，在该层叠体上下表面配置35μ的电解铜箔，在200℃、表面压力30kgf/cm2、30mmHg以下的真空下进行120min的加压成型，获得厚度为1.0mm的双面覆铜层压板。
实施例2
称取R/Si＝1.5(摩尔比)，Ph/(Me+Ph)＝0.4(摩尔比)的甲基苯基硅树脂100份，溶于100份甲苯溶剂中，待溶解完全后，用精准取液器量取0.005份乙酰丙酮钴催化剂和1.2份γ-缩水甘油醚氧丙基三甲氧基硅烷(美国，道康宁制造)，投入到硅树脂溶液中，搅拌均匀后，添加30份白色颜料金红石型二氧化钛，室温下搅拌1h，乳化20min，得白色硅树脂胶液。
除了使用该树脂胶液外，与实施例1同样进行，获得预浸料和厚度为1.0mm的双面覆铜层压板。
实施例3
称取R/Si＝1.6(摩尔比)，Ph/(Me+Ph)＝0.8(摩尔比)的甲基苯基硅树脂100份，溶于100份甲苯溶剂中，待溶解完全后，用精准取液器量取0.1份的环烷酸铝催化剂和1.8份W-903(德国，BYK公司制造)，投入到硅树脂溶液中，搅拌均匀后，添加25份白色颜料锐钛矿型二氧化钛和10份二氧化硅填料，室温下搅拌1h，乳化20min，得白色硅树脂胶液。
除了使用该树脂胶液外，与实施例1同样进行，获得预浸料和厚度为1.0mm的双面覆铜层压板。
实施例4
称取R/Si＝1.7(摩尔比)，Ph/(Me+Ph)＝1.0(摩尔比)的苯基硅树脂100份，溶于100份甲苯溶剂中，待溶解完全后，用精准取液器量取0.1份的环烷酸铝催化剂和6.8份W-903(德国，BYK公司制造)，投入到硅树脂溶液中，搅拌均匀后，添加25份白色颜料锐钛矿型二氧化钛和35份氧化铝填料，室温下搅拌1h，乳化20min，得白色硅树脂胶液。
除了使用该树脂胶液外，与实施例1同样进行，获得预浸料和厚度为1.0mm的双面覆铜层压板。
实施例5
称取R/Si＝1.1(摩尔比)，Ph/(Ph+Me)＝0(摩尔比)的甲基硅树脂50.0份和R/Si＝1.7(摩尔比)，Ph/(Ph+Me)＝0.9(摩尔比)的甲基苯基硅树脂50.0份，溶于100份甲苯溶剂中，待溶解完全后，用精准取液器量取1.8份的钛酸酯催化剂和1.8份W-903分散剂(德国，BYK公司制造)，投入到硅树脂溶液中，搅拌均匀后，添加25份白色颜料锐钛矿型二氧化钛和35份二氧化硅填料，室温下搅拌1h，乳化20min，得白色硅树脂胶液。
除了使用该树脂胶液外，与实施例1同样进行，获得预浸料和厚度为1.0mm的双面覆铜层压板。
对比例1
称取甲基乙烯基硅树脂100份(乙烯基质量分数为1.0％)，溶入50份粘度为500mPa.s的甲基乙烯基硅油中，溶解均匀后加入2.9份甲基含氢硅油(含氢量为1.3％)，高速搅拌均匀后称取0.001份己炔醇，搅拌30min后加入0.01份铂-甲基苯基乙烯基络合物，继续搅拌30min后加入30份白色颜料金红石型二氧化钛，室温下搅拌1h，乳化20min，得白色加成型硅树脂胶液。
除了使用该树脂胶液外，与实施例1同样进行，获得预浸料和厚度为1.0mm的双面覆铜层压板。
对比例2
称取R/Si＝1.1(摩尔比)，Ph/(Me+Ph)＝0(摩尔比)的甲基硅树脂100份，溶于100份甲苯溶剂中，待溶解完全后，用精准取液器量取0.003份的辛酸锌催化剂和0.5份硅烷偶联剂γ-缩水甘油醚氧丙基三甲氧基硅烷(美国，道康宁制造)，投入到硅树脂溶液中，搅拌均匀后，添加2.5份白色颜料金红石型二氧化钛，室温下搅拌1h，乳化20min，得白色硅树脂胶液。
除了使用该树脂胶液外，与实施例1同样进行，获得预浸料和厚度为1.0mm的双面覆铜层压板。
对比例3
称取R/Si＝1.6(摩尔比)，Ph/(Me+Ph)＝0.8(摩尔比)的甲基苯基硅树脂100份，溶于100份甲苯溶剂中，待溶解完全后，用精准取液器量取0.1份的环烷酸铝催化剂和1.8份W-903(德国，BYK公司制造)，投入到硅树脂溶液中，搅拌均匀后，添加65份白色颜料锐钛矿型二氧化钛和10份二氧化硅填料，室温下搅拌1h，乳化20min，得白色硅树脂胶液。
除了使用该树脂胶液外，与实施例1同样进行，获得预浸料和厚度为1.0mm的双面覆铜层压板。
对比例4
称取R/Si＝1.8(摩尔比)，Ph/(Me+Ph)＝0.8(摩尔比)的甲基苯基硅树脂100份，溶于100份甲苯溶剂中，待溶解完全后，用精准取液器量取0.1份的环烷酸铝催化剂和1.8份W-903(德国，BYK公司制造)，投入到硅树脂溶液中，搅拌均匀后，添加25份白色颜料锐钛矿型二氧化钛和10份二氧化硅填料，室温下搅拌1h，乳化20min，得白色硅树脂胶液。
除了使用该树脂胶液外，与实施例1同样进行，获得预浸料和厚度为1.0mm的双面覆铜层压板。
效果确认测试
(1)耐热变色性
将实施例1～5及对比例1～4中得到的覆铜箔白色层压板用切割锯将双面覆铜层压板切割为大小100×100mm后进行蚀刻处理，得各有机硅白色层压板，并在200℃下进行长时间烘烤实验，进行反射率对比，数据请见下表。
(2)耐热稳定性
将实施例1～5及对比例1～4的覆铜板层压板进行蚀刻处理，得到各层压板，使用热重分析(TGA)测量层压板基材热分解温度，其分解2％的温度Td(2％)请见下表。
测试设备：NETZSCHTG209F3
测试条件：室温至700℃，升温速率可控制在10℃±0.1℃/min，氮气流速为0.9ml/s。
(3)剥离强度测试
测试方法：使用IPC-TM-6502.4.8方法进行测试，测试数据请见下表。
物性分析：从上表的数据可以看出，实施例1～5常温下具有很好光的反射率，且在高温下长期烘烤仍然能保持很好的光反射率，同时其在高温下稳定性也较好，剥离强度较高，完全能符合LED白色层压板的需求。而对比例1与实施例2相比，树脂为甲基乙烯基硅树脂，为加成型固化方式，覆铜板高温反射率、耐高温性和剥离强度都较差；对比例2与实施例1相比，由于白色填料含量较少，其常温反射率和高温反射率较差；对比例3与实施例3相比，由于白色填料超过范围，导致与铜箔的剥离强度降低，无法正常使用；对比例4与实施例3相比，R/Si非常高，导致板材偏软，并且固化不完全，其耐热性较差。
申请人声明，本发明通过上述实施例来说明本发明的详细方法，但本发明并不局限于上述详细方法，即不意味着本发明必须依赖上述详细方法才能实施。所属技术领域的技术人员应该明了，对本发明的任何改进，对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等，均落在本发明的保护范围和公开范围之内。

Claims (9)

1.一种有机硅树脂组合物，其特征在于，所述有机硅树脂组合物，包括：
2.如权利要求1所述的有机硅树脂组合物，其特征在于，所述缩合型硅树脂为甲基硅树脂、甲基苯基硅树脂或苯基硅树脂中的任意一种或者至少两种的混合物。
3.如权利要求1或2所述的有机硅树脂组合物，其特征在于，所述缩合型硅树脂为R/Si＝1.0～1.7(摩尔比)和Ph/(Me+Ph)＝0～1.0(摩尔比)的甲基硅树脂、甲基苯基硅树脂或苯基硅树脂中的任意一种或者至少两种的混合物，其中Ph代表苯基基团，Me代表甲基基团，R代表有机官能团-CH3、-Ph、-OCH3、-OCH2CH3、-H或-OH；
优选地，所述缩合型硅树脂为R/Si＝1.2～1.7(摩尔比)且Ph/(Me+Ph)＝0.2-0.6(摩尔比)的甲基苯基硅树脂。
4.如权利要求1-3之一所述的有机硅树脂组合物，其特征在于，所述白色填料为氧化铝、二氧化钛、氢氧化铝、二氧化硅或氧化锌中的任意一种或者至少两种的混合物，优选二氧化钛。
5.如权利要求1-4之一所述的有机硅树脂组合物，其特征在于，所述催化剂是环烷酸锌、环烷酸锡、环烷酸钴、环烷酸铁、环烷酸铈、羧酸锌、羧酸锡、羧酸钴、羧酸铁、羧酸铈、全氟磺酸、氯化磷腈、胺类、辛酸锌、异辛酸锌、季铵碱、钛酸酯或胍类化合物等中的任意一种或者至少两种的组合；
优选地，所述助剂为偶联剂或/和分散剂，所述偶联剂为硅烷偶联剂或/和钛酸酯偶联剂。
6.一种树脂胶液，其特征在于，其是将如权利要求1-5之一所述的有机硅树脂组合物溶解或分散在溶剂中得到。
7.一种白色预浸料，其特征在于，其包括增强材料及通过含浸干燥后附着在增强材料上的如权利要求1-5之一所述的硅树脂组合物。
8.一种白色层压板，其特征在于，所述白色层压板含有至少一张如权利要求7所述的白色预浸料。
9.一种白色覆铜箔层压板，其特征在于，所述白色覆铜箔层压板包括至少一张叠合的如权利要求7所述的白色预浸料及压覆在叠合后的预浸料的一侧或两侧的铜箔。
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