CN112793254A - 一种碳氢树脂与氧化硅纤维网格布复合材料及制备方法 - Google Patents

一种碳氢树脂与氧化硅纤维网格布复合材料及制备方法 Download PDF

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CN112793254A
CN112793254A CN202110115523.0A CN202110115523A CN112793254A CN 112793254 A CN112793254 A CN 112793254A CN 202110115523 A CN202110115523 A CN 202110115523A CN 112793254 A CN112793254 A CN 112793254A
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hydrocarbon resin
mesh cloth
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林东
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Shandong Ruili Taiyang New Material Technology Co ltd
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Abstract

本发明公开了一种碳氢树脂与氧化硅纤维网格布复合材料及制备方法，所述方法通过将碳氢树脂加热软化后，与二氧化硅球混合，浸渍于二氧化硅纤维网格布，制备无机有机双纳米杂化材料。本发明方法利用碳氢树脂的热塑性，与二氧化硅球完成杂化复合，成本低、工艺简单，所制备的符合材料兼备较高的机械强度和塑性，且拥有低介电常数和较小的介电损耗，为高速高频线路板的生产提供了优质的制作材料。

Description

一种碳氢树脂与氧化硅纤维网格布复合材料及制备方法
技术领域
本发明涉及杂化复合材料合成技术领域，具体提供一种碳氢树脂与氧化硅纤维网格布复合材料及制备方法。
背景技术
有机无机纳米杂化材料是在微观尺寸上有机和无机相互结合得到的一种材料，是二十世纪八十年代开始兴起的一种新型材料，对无机和有机材料在宏观尺寸上进行复合，以改进单一材料的不足。而这种微观层面上的复合材料具有传统的有机和无机材料，以及传统的宏观尺寸复合物所没有的独特性能。有机无机杂化材料的合成方面，目前主流有溶胶凝胶法、插层复合技术、无机离子的表面改性、电化学合成法、组装法等。
碳氢树脂是指一种全碳氢组分的树脂，即其分子结构中仅含有C、H两种元素，且分子结构中不含极性基团，因而具有优异的介电性能。是近年来新兴的一种高频高速覆铜板用基体树脂，但其玻璃化转变温度低、耐热性差。长期以来本领域的技术人员对介电性能很好的碳氢树脂进行了研究。
专利WO97/38564采用非极性的苯乙烯与丁二烯和二乙烯基苯的四聚物添加硅铝酸镁填料，以玻璃纤维布作为增强材料制成的电路基板，虽然介电性能优异，但是基板的耐热性很差，玻璃化转变温度只有100℃左右，很难满足PCB制作过程无铅化制程的高温(240℃以上)要求。
美国专利US571609采用分子量小于5000的低分子量的1，2-聚丁二烯树脂或聚异丁二烯，和高分子量的丁二烯与苯乙烯的共聚物配合，并加入大量的硅微粉作为填料，以玻璃纤维布作为增强材料制作的电路基板，虽然介电性能优异，但是因为在该专利中采用了高分子量的成分来改善半固化片粘手状况，使得制作半固化片的过程的工艺性能变差，而且因为整个树脂体系的树脂分子中的刚性结构苯环的比例很少，交联以后的链段大都由刚性很低的亚甲基组成，因此制作成的板材刚性不好，弯曲强度很低。
中国专利CN101544841B使用分子量11000以下乙烯基含量60％以上的碳氢树脂作为主体，采用烯丙基改性的酚醛树脂改进半固化片发粘的特性，剥离强度有一定提升，但是体系固化后的耐热性低，覆铜箔层压板在PCB加工过程中出现分层失效的风险较高。
附图说明
图1为本发明带粒径实心硅球板材扫描电镜图。
发明内容
本发明的技术任务是针对上述存在的问题，提供一种碳氢树脂与氧化硅纤维网格布复合材料制备方法。
一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，所述方法通过将碳氢树脂加热软化后，与二氧化硅球混合，浸渍于二氧化硅纤维网格布，制备无机有机双纳米杂化材料。
在高聚物加入少量层状无机物并实现插层复合后，可使纳米复合体系的机械性能大大提高，耐热性也显著增强，且通过对粘土含量、界面作用、分散状态的优化有可能使材料的力学性能得到更大幅度的提高，得到性能更好的结构材料。
二氧化硅球为纳米球型二氧化硅，具有颗粒尺寸小、形状为真球型、比表面积大、紫外线、可见光及红外线反射能力强等特点,与有机高分子材料的相容性好，利用纳米球型SiO2来制造复合材料，大大提高了材料的致密性、韧性和光洁度。
其特征在于所述碳氢树脂和二氧化硅球的混合质量比例为：55-70比10-45。
所述方法的实现过程包括步骤如下：
1)将碳氢树脂加热软化；
2)将加热软化后的碳氢树脂与二氧化硅球混合；
3)将混合后的材料浸渍于二氧化硅纤维网格布，压制并冷却，制备成平板结构。
通过与二氧化硅纤维网格布的复合，达到了增强其机械强度，降低其介电系数与损耗的作用。
所述步骤1)中的加热温度为70-80oC。
所述步骤3)中的平板结构厚度为0.5-2mm。
所述的二氧化硅球的直径为1-15μm。
所述碳氢树脂采用水浴方式加热。
所述二氧化硅纤维网格布为1层或多层堆叠。
所述方法的实现过程还包括：通过将二氧化硅纤维网格布平铺于平板模板之上，将软化的碳氢树脂均匀浸渍于网格布，压延成型。
一种碳氢树脂与氧化硅纤维网格布复合材料，所述复合材料通过上述任一方法制备。
与现有技术相比，本发明一种新型碳氢树脂与氧化硅杂化复合材料及制备方法具有以下突出的有益效果：
本发明方法利用碳氢树脂的热塑性，与二氧化硅球和二氧化硅网格布完成杂化复合，成本低、工艺简单，所制备的符合材料兼备较高的机械强度和塑性，且拥有低介电常数和较小的介电损耗，为高速高频线路板的生产提供了优质的制作材料。
具体实施方式
下面将结合实施例，对本发明作进一步详细说明。
实施例1
一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，步骤如下：
(1)碳氢树脂与二氧化硅球杂化复合
将10克碳氢树脂粉水浴加热至80℃，搅拌直至完全软化；
向碳氢树脂中加入1.75克5-10微米直径的二氧化硅球，水浴加热搅拌至完全混合均匀。
(2)浸渍二氧化硅纤维网格布
将一层二氧化硅纤维网格布平铺于平板摸具上，将软化后的碳氢树脂和二氧化硅球混合物浸润二氧化硅纤维网格布，直至碳氢树脂完全包裹并浸润网格布；
(3)干压法制备成膜
将软化的碳氢树脂和二氧化硅球混合物浸润后的二氧化硅纤维网格布，采用单轴干压法制备成1mm厚平板，冷却硬化，获得低介电损耗可用于PCD板基材的碳氢树脂和氧化硅杂化复合的材料，如图1所示。
实施例2
(1)碳氢树脂与二氧化硅球杂化复合
将14克碳氢树脂粉水浴加热至70℃，搅拌直至完全软化；
向碳氢树脂中加入3克1-5微米直径的二氧化硅球，水浴加热搅拌至完全混合均匀。
(2)浸渍二氧化硅纤维网格布
将2层二氧化硅纤维网格布堆叠平铺于平板摸具上，将软化后的碳氢树脂和二氧化硅球混合物浸润二氧化硅纤维网格布，直至碳氢树脂完全包裹并浸润网格布；
(3)干压法制备成膜
将软化的碳氢树脂和二氧化硅球混合物使用单轴干压法制备成2mm厚平板，冷却硬化，获得低介电损耗可用于PCD板基材的碳氢树脂和氧化硅杂化复合的材料。
实施例3
(1)碳氢树脂与二氧化硅球杂化复合
将11克碳氢树脂粉水浴加热至75℃，搅拌直至完全软化；
向碳氢树脂中加入2克10-15微米直径的二氧化硅球，水浴加热搅拌至完全混合均匀。
(2)浸渍二氧化硅纤维网格布
将4层二氧化硅纤维网格布堆叠平铺于平板摸具上，将软化后的碳氢树脂和二氧化硅球混合物浸润二氧化硅纤维网格布，直至碳氢树脂完全包裹并浸润网格布；
(3)压延法制备成膜
将软化的碳氢树脂和二氧化硅球混合物使用单轴压延法制备成0.5mm厚平板，冷却硬化，获得低介电损耗可用于PCD板基材的碳氢树脂和氧化硅杂化复合的材料。
以上所述仅为本申请的较佳实施例，并不用以限制本申请，凡在本申请的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本申请的保护范围之内。

Claims (10)

1.一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于，所述方法通过将碳氢树脂加热软化后，与二氧化硅球混合，浸渍于二氧化硅纤维网格布，制备无机有机双纳米杂化材料。
2.根据权利要求1所述的一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于所述碳氢树脂和二氧化硅球的混合质量比例为：55-70比10-15。
3.根据权利要求2所述的一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于，所述方法的实现过程包括步骤如下：
1)将碳氢树脂加热软化；
2)将加热软化后的碳氢树脂与二氧化硅球混合；
3)将混合后的材料浸渍于二氧化硅纤维网格布，压制并冷却，制备成平板结构。
4.根据权利要求3所述的一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于，所述步骤1)中的加热温度为70-80℃。
5.根据权利要求3所述的一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于，所述步骤3)中的平板结构厚度为0.5-2mm。
6.根据权利要求3所述的一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于，所述的二氧化硅球的直径为1-15μm。
7.根据权利要求3所述的一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于，所述碳氢树脂采用水浴方式加热。
8.根据权利要求7所述的一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于，所述二氧化硅纤维网格布为1层或多层堆叠。
9.根据权利要求8所述的一种碳氢树脂与氧化硅纤维网格布复合材料制备方法，其特征在于，所述方法的实现过程还包括：通过将二氧化硅纤维网格布平铺于平板模板之上，将软化的碳氢树脂均匀浸渍于网格布，压延成型。
10.一种碳氢树脂与氧化硅纤维网格布复合材料，其特征在于，所述复合材料通过上述任一权利要求所述的方法制备。
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CN102070854A (zh) * 2010-12-18 2011-05-25 广东生益科技股份有限公司 复合材料、用其制作的高频电路基板及其制作方法
CN108382047A (zh) * 2018-04-01 2018-08-10 苏州欣天新精密机械有限公司 一种覆铜板的热熔制备方法
CN110561857A (zh) * 2019-08-21 2019-12-13 瑞声科技（南京）有限公司 覆铜层压板、印刷电路板及印刷电路板的制造方法
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CN102070854A (zh) * 2010-12-18 2011-05-25 广东生益科技股份有限公司 复合材料、用其制作的高频电路基板及其制作方法
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