CN106751711A - 氟取代乙烯基聚合物树脂组合物、半固化片及层压板 - Google Patents

氟取代乙烯基聚合物树脂组合物、半固化片及层压板 Download PDF

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CN106751711A
CN106751711A CN201710036777.7A CN201710036777A CN106751711A CN 106751711 A CN106751711 A CN 106751711A CN 201710036777 A CN201710036777 A CN 201710036777A CN 106751711 A CN106751711 A CN 106751711A
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resin
substituted ethylene
based polyalcohol
ethylene based
fluorine substituted
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CN106751711B (zh
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钟健人
王琢
邹水平
钱晋
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Ventec Electronics Suzhou Co Ltd
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Ventec Electronics Suzhou Co Ltd
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Abstract

本发明公开了氟取代乙烯基聚合物树脂组合物及由其制得的半固化片及层压板，氟取代乙烯基聚合物树脂组合物包含氟取代乙烯基聚合物树脂和官能团化高分子聚合物，其中，所述的氟取代乙烯基聚合物树脂由下式表示，且其粒径最大不超过100微米，取代基R1，R2，R3，R4至少有一种是氟原子，重复单元数n不小于100。本发明中组合物的制备调制方法简单，组合物可应用于电子装备，大大提高了信号传输速度，降低信号损失；半固化片含胶量均匀、表面平整、性能稳定；层压板制作工艺简单，具有优异的机械、耐热性和介电性能。

Description

氟取代乙烯基聚合物树脂组合物、半固化片及层压板
技术领域
本发明涉及电子产品材料领域，具体涉及一种氟取代乙烯基聚合物树脂组合物、半固化片及层压板。
背景技术
随着无线网络、卫星通讯的日益发展,信息产品走向高速与高频化,通信产品走向容量大速度快的无线传输之语音、视像和数据规范化。因而电子产品趋向轻薄短小，并适合高频传输，电路板的配线走向高密度化，高多层化。
为了维持传输速率及保持传输讯号的完整性，电路板的基板材料必须兼具较低的介电常数(dielectricconstant，Dk)及介电损耗(又称损失因子，dissipation factor，Df)。介电常数、介电损耗越小，信号损失越小。
当前使用聚苯醚、氰酸酯胶液或改性环氧胶液制得的半固化片，胶含量为50-60％制得的基板，Dk值都不低于3.2，无法满足高频板的信号传输要求。另中国专利CN201210144675.4、201310476142.0公开了将聚四氟乙烯粉与聚苯醚粉混合，经球磨后在模具中285℃压合形成介质材料层，玻璃纤维布放入PTFE树脂内烧结成半固化片，然后将铜箔、金属基板、模具压合形成的介质材料层、半固化片按照顺序叠放后压合形成基板的方法。此技术公开的方法工艺复杂，成本高，且制得的基板厚度均匀性难控制，外观不平滑，难以制作高多层PCB板。美国专利2539329中提到了用205℃对PTFE玻纤布漆片进行预处理，碾压后再浸渍的方法来改善PTFE涂层过厚产生的“泥裂”现象，这种方法存在原涂层再浸胶时易脱落，且低于250℃以下难以进行层压的难题。
发明内容
本发明的目的在于克服现有技术存在的以上问题，提供一种氟取代乙烯基聚合物树脂组合物、半固化片及层压板，本发明中组合物的制备调制方法简单，组合物可应用于电子装备，大大提高了信号传输速度，降低信号损失；半固化片含胶量均匀、表面平整、性能稳定；层压板制作工艺简单，具有优异的机械、耐热性和介电性能。
为实现上述技术目的，达到上述技术效果，本发明通过以下技术方案实现：
一种氟取代乙烯基聚合物树脂组合物，包含氟取代乙烯基聚合物树脂和官能团化的高分子聚合物，所述氟取代乙烯基聚合物树脂的结构式如下：
其中，取代基R1，R2，R3，R4至少有一种是氟原子，n不小于100，
所述氟取代乙烯基聚合物树脂的粒径不超过100μm。
进一步包括，所述官能团化的高分子聚合物包括以下中的一种或几种：环氧树脂、氰酸酯树脂、聚苯醚树脂、聚丁二烯、聚异戊二烯、环氧树脂改性物、氰酸酯树脂改性物、聚苯醚树脂改性物、聚丁二烯改性物、聚异戊二烯改性物。
进一步包括，氟取代乙烯基聚合物树脂组合物是由聚氟乙烯、聚四氟乙烯、聚偏氟乙烯、聚三氟乙烯中一种或二种及其多种而成的混合物。
进一步包括，所述氟取代乙烯基聚合物树脂所占的固体质量百分比为1-70％。
进一步包括，还包含至少一种有机或无机填料，填料固体质量百分比不超过80％。
进一步包括，所述有机或无机填料经过偶联剂表面处理或者未经偶联剂表面处理。
进一步包括，还包含至少一种交联剂。
进一步包括，所述交联剂包括以下中的一种或几种：胺类、酸酐类、酚醛类、活性酯、过氧化物。
进一步包括，还包含一种阻燃剂。
进一步包括，还包含溶剂，所述溶剂包括以下中的一种或几种：丙酮、丁酮、环己酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、苯、甲苯、二甲苯、水。
进一步包括，所述树脂组合物的玻璃态转化温度大于170℃。
进一步包括，所述树脂组合物的裂解温度大于350℃。
进一步包括，所述树脂组合物在288℃下，超过30min发生分层。
进一步包括，所述树脂组合物的介电常数为2.4-2.8。
进一步包括，所述树脂组合物的介电损耗因子为0.001-0.01。
一种半固化片，将氟取代乙烯基聚合物树脂和官能团化高分子聚合物浸润到基材中，经特别固化形成半固化片，所述氟取代乙烯基聚合物树脂的结构式如下：
其中，取代基R1，R2，R3，R4至少有一种是氟原子或官能团，n不小于100，所述氟取代乙烯基聚合物树脂的粒径不超过100μm。
进一步包括，所述基材为玻璃纤维，玻璃纤维布，玻璃纤维织物，所述官能团化高分子聚合物包括以下中的一种或几种：环氧树脂、氰酸酯树脂、聚苯醚树脂、聚丁二烯、聚异戊二烯、环氧树脂改性物、氰酸酯树脂改性物、聚苯醚树脂改性物、聚丁二烯改性物、聚异戊二烯改性物。
进一步包括，所述树脂组合物的介电常数为2.4-2.8。
一种层压板，将氟取代乙烯基聚合物树脂和官能团化高分子聚合物浸润到基材中，经特别固化形成半固化片，所述半固化片与铜箔热压形成层压板，所述氟取代乙烯基聚合物树脂的结构式如下：
其中，取代基R1，R2，R3，R4至少有一种是氟原子或官能团，n不小于100，所述氟取代乙烯基聚合物树脂的粒径不超过100μm。
进一步包括，所述官能团化高分子聚合物包括以下中的一种或几种：环氧树脂、氰酸酯树脂、聚苯醚树脂、聚丁二烯、聚异戊二烯、环氧树脂改性物、氰酸酯树脂改性物、聚苯醚树脂改性物、聚丁二烯改性物、聚异戊二烯改性物，所述树脂组合物的介电常数为2.4-2.8。
本发明的有益效果是:
本发明以氟取代乙烯基聚合物树脂组合物为主体胶液，调制简单易行，该组合物可应用于电子装备，大大提高了信号传输速度，降低信号损失。由该氟取代乙烯基聚合物树脂组合物浸渍玻璃布制得半固化片，含胶量均匀，且胶含量在50％-60％之间的半固化片制得的层压板，介电常数Dk可做到3.0以下。此外由此氟取代乙烯基聚合物树脂组合物制作的层压板，具有较高的玻璃态转变温度，高耐剥离机械性能，且具有优异的介电性能，满足服务器及基站、天线、雷达等通讯领域之高可靠性和极低Loss损耗材料要求。
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，本发明的具体实施方式由以下实施例详细给出。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例中的氟取代乙烯基聚合物树脂组合物包含氟取代乙烯基聚合物树脂和官能团化高分子聚合物，其中氟取代乙烯基聚合物树脂具有如下结构式(1)，其最大粒径可选用小于100微米的，也可选用粒径小于90微米的，或小于80微米的，或小于70微米的，或小于60微米的，或小于50微米的。
取代基R1，R2，R3，R4至少有一种是氟原子或官能团，这些取代基不一定要相同，可以有不同的化学结构，但至少需含有一种氟原子。
在其它一些实施例中，氟取代乙烯基聚合物树脂组合物是由聚氟乙烯、聚四氟乙烯、聚偏氟乙烯、聚三氟乙烯中一种或二种及其多种而成的混合物。
优先选择聚氟乙烯，因为聚氟乙烯结构不完全对称，极性增强，更利于树脂的兼容性及分散。
在实施例中，重复单元数n可以是大于100，或大于150，或大于200，或大于250，或大于300，或大于350，或大于400，或大于450，或大于500。优先选用大于100，因为分子量小更利于在树脂中更好的分散及流动；
氟取代乙烯基聚合物树脂组合物的固体质量百分比可以是1％-70％，或1％-60％，或1％-50％，或1％-40％，或10％-70％，或10％-60％，或10％-50％，或10％-40％，或10％-30％，或10％-20％，或20％-70％，或20％-60％，或20％-50％，或20％-40％，或20％-30％，或30％-70％，或30％-60％，或30％-50％，或30％-40％。优先选用1％-50％，综合性能最佳。
在实施例中，官能团化高分子聚合物是环氧树脂、氰酸酯树脂、聚苯醚树脂、聚丁二烯、聚异戊二烯及前述高分子改性物中的一种或几种，优先选用聚苯醚树脂，通过聚苯醚树脂与氟取代乙烯基聚合物树脂相互作用，改善了氟取代乙烯基聚合物树脂电性能、机械性能低，加工难的问题，同时还可具有优异的低介电常数和低介电损耗因子。
在实施例中，氟取代乙烯基聚合物树脂组合物进一步还含有填料，填料可以是有机或无机成分。
填料的固体质量百分比不超过80％，在一些实施例中，填料的固体质量百分比可以少于70％，或少于60％，或少于50％，或少于40％，或少于30％，在其它的实例里，填料可以是具有或没有经偶联剂处理的。
上述氟取代乙烯基聚合物树脂组合物还含有至少一种交联剂，交联剂可以是胺类、酸酐类、酚醛类、活性酯、过氧化物中的一种或几种。
氟取代乙烯基聚合物树脂组合物还含有阻燃剂和溶剂，溶剂选自于丙酮、丁酮、环己酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、苯、甲苯、二甲苯、水中的一种或几种。
实施例1-4、对比例1-2
在实施例1-4和对比例1-2中，各组分如表1中所示。
表1 实施例1-4和对比例1-2组分表
实施例1-4、对比1-2中制备的组合物胶液的性能如表2中所示。
表2 性能表
如表2中所示，实施例1提供的氟取代乙烯基聚合物树脂组合物，玻璃态转化温度为175℃,热分解温度为350℃，在288℃条件下发生分层的时间大于30分钟，耐剥离强度为6.2lb/in,在10GHz条件下Dk、Df分别是2.5和0.005。
相同地，实施例3提供的氟取代乙烯基聚合物树脂组合物，玻璃态转化温度为176℃,热分解温度为352℃，在288℃条件下发生分层的时间大于30分钟，耐剥离强度为6lb/in,在10GHz条件下Dk、Df分别是2.5和0.005。
对比例1提供的氟取代乙烯基聚合物树脂组合物，玻璃态转化温度为140℃,热分解温度为340℃，在288℃条件下发生分层的时间大约为5分钟，耐剥离强度为3lb/in,在10GHz条件下Dk、Df分别是2.1和0.0005。介电性能优异，但耐热性、机械性能较差。
在本发明的实施例中，可以发现该树脂组合物玻璃态转化温度大于140℃，有的大于150℃，或大于160℃，或大于170℃，或大于172℃，或大于173℃，或大于174℃，或大于175℃，或大于176℃，或大于177℃。热裂解温度大于340℃，或大于350℃，或大于355℃，或大于360℃，或大于361℃，或大于362℃。在288℃条件下发生分层的时间大于5分钟，或大于10分钟，或大于20分钟，或大于30分钟。
在本发明的实施例中，该树脂组合物，在10GHZ条件下，介电常数范围为2.4-2.8,或2.4-2.7,或2.4-2.6,或2.4-2.5。介电损耗因子为0.001-0.01,或0.002-0.009，或0.003-0.008，或0.004-0.007,或0.005-0.006。
实施例5
使用上述氟取代乙烯基聚合物树脂组合物浸润到基材中并使浸润后的基材半固化或特别固化而制得半固化片。
该氟取代乙烯基聚合物树脂组合物具有上述提到的结构式(1)，其粒径为上述所述的可选用小于100微米的，也可选用粒径小于90微米的，或小于80微米的，或小于70微米的，或小于60微米的，或小于50微米的。
该氟取代乙烯基聚合物树脂组合物的取代基R1，R2，R3，R4至少有一种是氟原子，在其它一些实施例中，氟取代乙烯基聚合物树脂组合物是由聚氟乙烯、聚四氟乙烯、聚偏氟乙烯、聚三氟乙烯中一种或二种及其多种而成的混合物。
该氟取代乙烯基聚合物树脂组合物的重复单元数n可以是大于100，或大于150，或大于200，或大于250，或大于300，或大于350，或大于400，或大于450，或大于500。
基材为玻璃纤维，玻璃纤维布，玻璃纤维织物。该氟取代乙烯基聚合物树脂组合物中的官能团化高分子聚合物可选自于环氧树脂、氰酸酯树脂、聚苯醚树脂、聚丁二烯、聚异戊二烯及前述高分子改性物中的一种或几种。
上述半固化片，在10GHz条件下，介电常数为2.4～2.8,或2.4～2.7,或2.4～2.6,或2.4～2.5。
实施例6
使用上述氟取代乙烯基聚合物树脂组合物浸润到基材中半固化或特别固化而制得的半固化片，与铜箔压合，制得层压板。该层压板所使用的氟取代乙烯基聚合物树脂组合物，结构如式(1)，其最大粒径可选用小于100微米的，也可选用粒径小于90微米的，或小于80微米的，或小于70微米的，或小于60微米的，或小于50微米的。
该氟取代乙烯基聚合物树脂组合物取代基R1，R2，R3，R4至少有一种是氟原子，在其它一些实施例中，氟取代乙烯基聚合物树脂组合物是由聚氟乙烯、聚四氟乙烯、聚偏氟乙烯、聚三氟乙烯中一种或二种及其多种而成的混合物。
该氟取代乙烯基聚合物树脂组合物的重复单元数n可以是大于100，或大于150，或大于200，或大于250，或大于300，或大于350，或大于400，或大于450，或大于500。
该半固化片，在10GHz条件下，介电常数为2.4～2.8,或2.4～2.7,或2.4～2.6,或2.4～2.5。
上述实施例中的氟取代乙烯基聚合物树脂组合物，调制简单，该组合物可应用于电子装备，大大提高了信号传输速度，降低信号损失。
由该氟取代乙烯基聚合物树脂组合物浸渍基材制得的半固化片，不需要在模具中烧结形成，和普通FR-4半固化片的制作过程一样，且该半固化片含胶量均匀、表面平整、性能稳定。基材可以是玻璃纤维，玻璃纤维布或布的混合物。和普通FR-4半固化片的制作过程一样，且该半固化片含胶量均匀、表面平整、性能稳定。
半固化片与铜箔压合，制得层压板，该层压板制作工艺简单，具有优异的机械、耐热性和介电性能。该层压板满足下游PCB线路特性及尺寸的多种设计要求，给PCB更多的设计自由性。通过减小PCB内层之间的厚度，有效控制PCB板总厚度，给制造更薄高多层PCB板带来了机遇。在一些实施例中，我们可以证明具有氟取代乙烯基聚合物树脂组合物的层压板，具有高玻璃态转变温度，优异的耐剥离机械性能以及改善的介电性能。简单地说，该层压板可满足服务器、基站、天线、汽车等通讯领域产品之高可靠性和极低Loss损耗的材料要求。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (20)

1.一种氟取代乙烯基聚合物树脂组合物，其特征在于，包含氟取代乙烯基聚合物树脂和官能团化的高分子聚合物，所述氟取代乙烯基聚合物树脂的结构式如下：
其中，取代基R1，R2，R3，R4至少有一种是氟原子或基团，n不小于100，所述氟取代乙烯基聚合物树脂的粒径不超过100μm。
2.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述官能团化的高分子聚合物包括以下中的一种或几种：环氧树脂、氰酸酯树脂、聚苯醚树脂、聚丁二烯、聚异戊二烯、环氧树脂改性物、氰酸酯树脂改性物、聚苯醚树脂改性物、聚丁二烯改性物、聚异戊二烯改性物。
3.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，氟取代乙烯基聚合物树脂组合物是由聚氟乙烯、聚四氟乙烯、聚偏氟乙烯、聚三氟乙烯中一种或二种及其多种而成的混合物。
4.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述氟取代乙烯基聚合物树脂所占的固体质量百分比为1-70％。
5.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，还包含至少一种有机或无机填料，填料固体质量百分比不超过80％。
6.根据权利要求5所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述有机或无机填料经过偶联剂表面处理或者未经偶联剂表面处理。
7.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，还包含至少一种交联剂。
8.根据权利要求7所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述交联剂包括以下中的一种或几种：胺类、酸酐类、酚醛类、活性酯、过氧化物。
9.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，还包含一种阻燃剂。
10.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，还包含溶剂，所述溶剂包括以下中的一种或几种：丙酮、丁酮、环己酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、苯、甲苯、二甲苯、水。
11.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述树脂组合物的玻璃态转化温度大于170℃。
12.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述树脂组合物的裂解温度大于350℃。
13.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述树脂组合物在288℃下，超过30min发生分层。
14.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述树脂组合物的介电常数为2.4-2.8。
15.根据权利要求1所述的氟取代乙烯基聚合物树脂组合物，其特征在于，所述树脂组合物的介电损耗因子为0.001-0.01。
16.一种半固化片，其特征在于，将权利要求1～15所述的氟取代乙烯基聚合物树脂和官能团化高分子聚合物组合物浸润到基材中，经固化条件制备成半固化片，所述氟取代乙烯基聚合物树脂的结构式如下：
其中，取代基R1，R2，R3，R4至少有一种是氟原子，n不小于100，所述氟取代乙烯基聚合物树脂的粒径不超过100μm。
17.根据权利要求16所述的半固化片，其特征在于，所述基材为玻璃纤维，玻璃纤维布，玻璃纤维织物，所述官能团化高分子聚合物包括以下中的一种或几种：环氧树脂、氰酸酯树脂、聚苯醚树脂、聚丁二烯、聚异戊二烯、环氧树脂改性物、氰酸酯树脂改性物、聚苯醚树脂改性物、聚丁二烯改性物、聚异戊二烯改性物。
18.根据权利要求16所述的半固化片，其特征在于，所述树脂组合物的介电常数为2.4-2.8。
19.一种层压板，其特征在于，将氟取代乙烯基聚合物树脂和官能团化高分子聚合物浸润到基材中，经特别固化形成半固化片，所述半固化片与铜箔热压形成层压板，所述氟取代乙烯基聚合物树脂的结构式如下：
其中，取代基R1，R2，R3，R4至少有一种是氟原子，n不小于100，所述氟取代乙烯基聚合物树脂的粒径不超过100μm。
20.根据权利要求19所述的层压板，其特征在于，所述官能团化高分子聚合物包括以下中的一种或几种：环氧树脂、氰酸酯树脂、聚苯醚树脂、聚丁二烯、聚异戊二烯、环氧树脂改性物、氰酸酯树脂改性物、聚苯醚树脂改性物、聚丁二烯改性物、聚异戊二烯改性物，所述树脂组合物的介电常数为2.4-2.8。
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