CN113583310B - 一种高导热碳氢组合物及其制备的高频覆铜板和制备方法 - Google Patents

一种高导热碳氢组合物及其制备的高频覆铜板和制备方法 Download PDF

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CN113583310B
CN113583310B CN202110863695.6A CN202110863695A CN113583310B CN 113583310 B CN113583310 B CN 113583310B CN 202110863695 A CN202110863695 A CN 202110863695A CN 113583310 B CN113583310 B CN 113583310B
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向中荣
刘永成
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Wuxi Relong New Material Technology Co ltd
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Abstract

本发明提供一种高导热碳氢组合物及其制备的高频覆铜板和制备方法，高导热碳氢组合物，按重量组份计，包括复合树脂20‑50份；导热填料10‑40份；阻燃剂10‑40份；无机填料5‑30份；抗氧剂0.1‑5份；交联剂2‑10份；复合树脂为树脂为聚丁二烯聚合物，聚丁二烯‑苯乙烯共聚物，苯乙烯‑丁二烯‑苯乙烯共聚物，改性聚苯醚，丁二烯‑丙烯腈共聚物中的两种或两种以上的复合物。本发明采用高导热碳氢组合物浸渍以电子级E级玻璃纤维布制得胶片，两面覆铜压合制得高频覆铜板，此覆铜板具有低介电常数，低介质损耗，高导热系数，吸水率极低，铜箔玻璃强度高，综合性能稳定，能充分满足5G高频通信领域的对材料的性能要求。

Description

一种高导热碳氢组合物及其制备的高频覆铜板和制备方法
技术领域
本发明属于高频通讯材料技术领域，具体涉及一种高导热碳氢组合物及其制备的高频覆铜板和制备方法。
背景技术
在5G高速发展的当下，对于覆铜板要求信息处理高速化，信号传输高频化，对覆铜板性能要求越来越高。传统环氧覆铜板由于其介电常数较高，介质损耗亦较高，已不能满足高频、高速通讯领域的要求。改性聚苯醚基覆铜板，由于其较低的介电常数和介质损耗已在高速信号传输领域广发应用，但是其高熔性缺点导致后期PCB加工中孔隙等缺陷，且基板吸水率较高，热膨胀系数高，无法应用到低吸水率及低热膨胀系数的通讯天线领域等。
聚四氟乙烯基高频覆铜板具有最优异的介电性能，且聚四氟乙烯介温漂、频漂较小等优点，目前已广泛应用于雷达，天线，滤波器等。然而由于其加工温度高大于360℃，且加工工艺难度较大，后期PCB加工孔金属化和电镀都是比较难的，且尺寸涨缩明显，进一步限制其应用。
聚碳氢基高频覆铜板具有低介电常数，低介质损耗，低热膨胀系数及较低吸水率等性能被广泛用作高频电子通讯材料。随着信号传输高频化、高速化发展，PCB的热管理也受到越来越多的重视，从而在一些应用场合对于PCB核心元器件覆铜板的导热系数就有着明确的要求，导热系数越高，元器件散热快，使得PCB温升相对较小。由于碳氢基聚合物或共聚物本身的导热非常差在0.01-0.03之间，因而通过填料选择改性，使得碳氢覆铜板具有较高的导热系数是覆铜板研究者常使用方法之一。常用导热填料包括氧化铝、氮化硼、氮化硅等，而高频材料对介电性能和吸水率等高要求的限制下，对于各种导热填料的选择搭配等要求也较高。
因而，研发出低介电常数、低介质损耗、优异的耐热性能、高导热系数等性能稳定的碳氢基高频覆铜板有着重要意义。
发明内容
本发明针对上述缺陷，提供一种由高导热碳氢组合物的组分，以及采用上述组合物制备得到的低介电常数、低介质损耗、优异耐热性能、高导热系数等性能稳定的碳氢基高频覆铜板和制备方法。
本发明提供如下技术方案：一种高导热碳氢组合物，按重量组份计，包括以下成分：
Figure BDA0003186753800000021
进一步地，所述复合树脂为聚丁二烯聚合物、聚丁二烯-苯乙烯共聚物、苯乙烯-丁二烯-苯乙烯共聚物、改性聚苯醚和丁二烯-丙烯腈共聚物中的两种或两种以上的复合物。
进一步地，所述聚丁二烯聚合物的分子量为1000-10000，所述聚丁二烯-苯乙烯共聚物的分子量为10000-50000，所述苯乙烯-丁二烯-苯乙烯共聚物的分子量为20000-100000，所述改性聚苯醚的分子量为2000-20000，所述丁二烯-丙烯腈共聚物的分子量为10000-50000。
进一步地，所述导热填料为三氧化二铝、碳化硅、氮化硅和氮化硼中一种或几种形成的混合物。
进一步地，所述阻燃剂为磷系阻燃剂、氮系阻燃剂、溴系阻燃剂、铝系阻燃剂、镁系阻燃剂、有机硅类阻燃剂和硼系阻燃剂中一种或几种形成的混合物。
进一步地，所述无机填料为硅微粉、气相二氧化硅、二氧化锡、硅灰石、氧化铝和钛白粉中一种或几种形成的混合物。
进一步地，所述抗氧剂为四[β-丙酸]季戊四醇酯、亚磷酸三(2,4-二叔丁基苯基)酯、4,4'-硫代双(6-叔丁基-3-甲基苯酚)、2,4-二(正辛基硫亚甲基)-6-甲基苯酚、1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯、2，6-二叔丁基对甲酚、甘醇双-3-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯、双(2,4-二叔丁基苯酚)季戊四醇二亚磷酸酯和2,2'-甲撑双(4-甲基-6-叔丁基苯酚)中的一种或几种形成的共混物。
进一步地，所述交联剂为二乙烯基苯、三烯丙基异氰尿酸脂、二烯丙基双酚A、2,5-二甲基-2，5二叔丁基过氧化己烷、二叔丁基过氧化物、过氧化苯甲酰和过氧化氢二异丙苯中一种或至少两种的混合物。
本发明还提供采用上述的高导热碳氢组合物制备高频覆铜板的方法，包括以下步骤：
1)将所述高导热碳氢组合物二甲苯为溶剂，以500-1500r/min转速搅拌分散制得分散良好的悬浮液，且胶液粘度在柴氏四号杯的30-60秒；
2)使用1080电子级玻璃纤维布浸渍分散好的悬浮液，通过调整制得65-80％胶含量的胶片，在110-140℃烘箱中烘烤10-20分钟得到制备好的胶片，待压合；
3)取上述制备好的胶片6张，两面附铜箔，在200℃，3Mpa条件下压合80-150分钟，得到最终产品-高导热碳氢高频覆铜板。
本发明还提供根据上述制备方法制备得到的高频覆铜板。
本发明的有益效果为：
采用本发明提供的高导热碳氢组合物制备的碳氢基高频覆铜板具有低介电常数、低介质损耗、优异的耐热性能、高导热系数的优异特性，其性能稳定，采用本发明提供的高导热碳氢组合物的二甲苯分散液浸渍以电子级E级玻璃纤维布制得胶片，两面覆铜压合制得高频覆铜板，此覆铜板具有低介电常数，低介质损耗，高导热系数，吸水率极低，铜箔玻璃强度高，综合性能稳定，能充分满足5G高频通信领域的对材料的性能要求。
具体实施方式
下面将结合本发明实施例，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做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1-3
下述实施例1-3制备方法如下：首先将复合树脂、导热填料、阻燃剂、无机填料、抗氧剂、交联剂依次加入二甲苯中，转速500-2000r/min充分混合均匀，调整胶液粘度在30-60s(柴氏四号杯)，制得胶液固含量约65-80％待用。将电子级1080玻璃布浸渍于已制备好的胶液，在110-140℃烘箱中烘烤30min脱除二甲苯制得半固化片。取6片胶片两面覆以1OZ(35μm)铜，经过热压机，温度在180-230℃保温80-150min热压制成双面板，具体实施例1-3的配方见表1：
表1
Figure BDA0003186753800000041
Figure BDA0003186753800000051
对比例1-3
对比例1-3与实施例1-3的区别在于采用如表2的配方。
表2
对比例1 对比例2 对比例3
苯乙烯-丁二烯-苯乙烯共聚物 15 10 20
聚丁二烯 15 20 10
改性聚苯醚 3 0 3
丁二烯-丙烯腈共聚物 0 3 0
二氧化硅 16 21 25
十溴二苯乙烷 15 0 10
膨胀型阻燃剂 0 30 15
氧化铝 30 0 0
氮化硼 0 10 0
氮化硅 0 0 10
4,4'-硫代双(6-叔丁基-3-甲基苯酚) 1 1 1
二乙烯基苯 2 1 1
三烯丙基异氰酸酯TAIC 0 1 2
过氧化二异丙苯 3 3 3
实施例1-3和对比例1-3的制备的覆铜板的各项性能如下：
Figure BDA0003186753800000052
Figure BDA0003186753800000061
如对比例1，导热材料仅使用三氧化二铝为导热填料，导热系数仅为0.56w/mk,小于目标值0.7w/mk。如对比例2，导热填料为氮化硼且添加量为10份，导热系数可达到0.70w/mk，但是吸水率很高至0.2％，且抗剥强度低3.35lb/inch。如对比例3，导热填料为氮化硅且添加量为10份，导热系数可达到0.69w/mk，但是吸水率较高至0.1％，抗剥为3.92lb/inch相对较小。
如实施例1-3中，由于氧化铝导热系数相对较低且介电常数较高，氮化硼吸水率较大且抗剥较小，氮化硅较氮化硼类似，具有自润滑性，故采取两种或两种以上复配，使得各导热填料的缺陷影响降至最低，同时尽可能发挥导热填料的优势性能，制得导热系数较高，抗剥强度较高，吸水率较低高可靠，高稳定的碳氢复合物。添加交联助剂及不同交联剂复配进一步增加了机械性能及耐热性等，制得介电性能优异，耐热性能好，材料均匀的碳氢高频覆铜板。
本发明工艺易于实现，成本较低，且易于批量化，此性能稳定的碳氢高导热覆铜板可充分满足5G通讯应用要求。
以上各实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
此外，本领域的技术人员能够理解，尽管在此的一些实施例包括其它实施例中所包括的某些特征而不是其它特征，但是不同实施例的特征的组合意味着处于本发明的范围之内并且形成不同的实施例。例如，在上面的权利要求书中，所要求保护的实施例的任意之一都可以以任意的组合方式来使用。公开于该背景技术部分的信息仅仅旨在加深对本发明的总体背景技术的理解，而不应当被视为承认或以任何形式暗示该信息构成已为本领域技术人员所公知的现有技术。

Claims (3)

1.一种高导热碳氢组合物，其特征在于，按重量组份计，由以下成分组成：
复合树脂            33份；
导热填料            10份；
阻燃剂              30份；
无机填料            21份；
抗氧剂              1份；
交联剂              5份；
所述复合树脂组成为10份苯乙烯-丁二烯-苯乙烯共聚物、20份聚丁二烯聚合物、以及3份丁二烯-丙烯腈共聚物；
所述导热填料的组成为5份氮化硅及5份氮化硼；
所述阻燃剂为膨胀阻燃剂；
所述无机填料为气相二氧化硅；
所述抗氧剂为4,4'-硫代双(6-叔丁基-3-甲基苯酚）；
所述交联剂的组成为1份过氧化氢二异丙苯、1份三烯丙基异氰尿酸脂、以及3份二乙烯基苯。
2.采用权利要求1所述的高导热碳氢组合物制备高频覆铜板的方法，其特征在于，包括以下步骤：
1）首先将复合树脂、导热填料、阻燃剂、无机填料、抗氧剂、交联剂依次加入二甲苯中，转速500-2000r/min充分混合均匀，调整胶液粘度在柴氏四号杯的30-60s，制得胶液固含量65-80%待用；
2）将电子级1080玻璃布浸渍于已制备好的胶液，在110-140℃烘箱中烘烤30min脱除二甲苯制得半固化片；
3）取6片胶片两面覆以35μm、1OZ的铜，经过热压机，温度在180-230℃保温80-150min热压制成双面板。
3.根据权利要求2所述的制备方法制备得到的高频覆铜板。
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