CN116334949A - 一种低介电损耗无纺布及其制备及其应用 - Google Patents

一种低介电损耗无纺布及其制备及其应用 Download PDF

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Publication number
CN116334949A
CN116334949A CN202111598907.9A CN202111598907A CN116334949A CN 116334949 A CN116334949 A CN 116334949A CN 202111598907 A CN202111598907 A CN 202111598907A CN 116334949 A CN116334949 A CN 116334949A
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CN
China
Prior art keywords
emulsion
dielectric loss
low dielectric
fluorine
nonwoven fabric
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CN202111598907.9A
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English (en)
Inventor
梁伟
柴颂刚
刘潜发
郝良鹏
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Shengyi Technology Co Ltd
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Shengyi Technology Co Ltd
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Priority to CN202111598907.9A priority Critical patent/CN116334949A/zh
Priority to US17/980,053 priority patent/US20230202126A1/en
Priority to JP2022191883A priority patent/JP2023095793A/ja
Publication of CN116334949A publication Critical patent/CN116334949A/zh
Pending legal-status Critical Current

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    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/36—Inorganic fibres or flakes
    • D21H13/38—Inorganic fibres or flakes siliceous
    • D21H13/40—Inorganic fibres or flakes siliceous vitreous, e.g. mineral wool, glass fibres
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Abstract

本发明提供一种低介电损耗无纺布及其制备及其应用，所述低介电损耗无纺布由无机纤维和粘结剂组成，所述的粘结剂为含氟树脂乳液、聚烯烃乳液、聚苯醚树脂或氰酸酯树脂中的任意一种或至少两种的组合。本发明的无纺布介电性能好，增强效果明显，能满足高频通信领域对覆铜板材料的各项性能要求。

Description

一种低介电损耗无纺布及其制备及其应用
技术领域
本发明属于层压板技术领域，涉及一种低介电损耗无纺布及其制备及应用。
背景技术
覆铜板广泛应用在手机、电脑、自动售货机、通信基站、卫星以及可穿戴设备、无人驾驶汽车、无人机和智能机器人等领域，是电子通讯和信息行业的关键基础材料之一。以聚四氟乙烯(PTFE)为代表的含氟树脂拥有其他聚合物树脂无法比拟的低介电常数、低介电损耗、高热稳定性和化学稳定性等多种优异性能，是一种理想的覆铜板基体材料。含氟树脂的高分子链柔性较大，通常需要引入无机材料以提高含氟树脂基覆铜板的机械强度，例如CN101857708A中公开了采用氟树脂混合物浸渍玻纤布烘烤后获得PTFE漆布，但由于玻璃布采用经纬编织，制备的PTFE覆铜板不均匀，覆铜板不同位置的介电常数、CTE、介电损耗不同，造成不同位置信号传输延时不同。
随着高频覆铜板基材各向同性的要求越来越强，需要开发一种各向同性的增强材料，使PTFE复合材料具有卓越的Dk一致性，极低的介质损耗，同时比不含增强材料的PTFE膜相比具备更好的机械强度。目前，没有极低介电损耗的各向同性的增强材料。
传统无纺布具备增强及各向同性的特点，但一般都采用环氧类粘结剂、丙烯酸酯类粘结剂、三聚氰胺类粘结剂或者聚乙烯醇类粘结剂，这些粘结剂的介电损耗大。环氧类粘结剂、丙烯酸酯类粘结剂、三聚氰胺类粘结剂或者聚乙烯醇类粘结剂的介电损耗大，远远大于高频主流产品使用的碳氢树脂、聚苯醚树脂或PTFE树脂的介电损耗，如果将传统的无纺布使用在高频产品中会失去碳氢树脂、聚苯醚树脂或PTFE树脂的介电优势，因此，本领域技术人员都是利用玻璃纤维布的增强及低介电损耗的特点，去考虑如何克服玻璃纤维布的经纬编织带来的各向异性，例如用玻璃布开纤的方式、对玻璃布进行预处理浸渍树脂等方式减少经纬编织带来的缺陷。
发明内容
针对现有技术的不足，本发明的目的在于提供一种低介电损耗无纺布及其制备及应用。本发明的无纺布介电性能好，增强效果明显，能满足高频通信领域对覆铜板材料的各项性能要求。
为达此目的，本发明采用以下技术方案：
一方面，本发明提供一种低介电损耗无纺布，所述低介电损耗无纺布由无机纤维和粘结剂组成，所述的粘结剂为含氟树脂乳液、聚烯烃乳液、聚苯醚树脂或氰酸酯树脂中的任意一种或至少两种的组合。
在本发明中，通过使用所述粘结剂，使得无纺布具有低的介电损耗，均匀性好，厚度一致，纤维各向分布一致，拉伸强度高，可在浸渍低介电损耗树脂时添加较多的介电填料，制备低介电损耗高频覆铜箔板。
在本发明中，所述低介电损耗无纺布是指无纺布的介电损耗小于0.0015(10GHz)。
优选地，所述低介电损耗无纺布中无机纤维的重量百分比为60-95％(例如60％、62％、65％、68％、70％、73％、75％、78％、80％、83％、85％、88％、90％、93％或95％)，粘结剂的重量百分比为5％-40％(例如5％、8％、10％、15％、18％、20％、23％、25％、28％、30％、33％、35％、38％或40％)。
所述的粘结剂为含氟树脂乳液、聚烯烃乳液、聚苯醚树脂或氰酸酯树脂中的任意一种或至少两种的组合。这些含氟树脂乳液、聚烯烃乳液、聚苯醚树脂或氰酸酯树脂可以根据需要添加溶剂去溶解稀释到合适的粘度，来获得粘结剂。
从低介电性能角度考虑，优选地，所述粘结剂为含氟树脂乳液。
优选地，所述含氟树脂乳液选自聚全氟乙丙烯乳液、聚偏氟乙烯乳液、四氟乙烯-全氟烷基乙烯基醚共聚物乳液、乙烯-四氟乙烯共聚物乳液、聚三氟氯乙烯乳液或乙烯-三氟氯乙烯共聚物乳液中的任意一种或至少两种的组合。
优选地，所述含氟树脂乳液中固含量为30-70％，例如30％、35％、38％、40％、45％、50％、55％、60％、65％或70％。
优选地，所述含氟树脂乳液中含氟树脂粒径0.10μm～0.40μm。
本文中含氟树脂乳液粒径采用激光衍射法测试，测试仪器马尔文激光粒度仪，型号MS3000。本文中介电常数和介电损耗采用SPDR(splite post dielectric resonator)法进行测试，频率为10GHz。
优选地，所述聚烯烃乳液选自不饱和聚丁二烯树脂乳液、苯乙烯-丁二烯-苯乙烯三嵌段共聚物(SBS)乳液、氢化苯乙烯-丁二烯-苯乙烯三嵌段共聚物(SEBS)乳液或丁苯树脂乳液中的任意一种或至少两种组合。聚烯烃乳液的固含量为30-70％，例如30％、35％、38％、40％、45％、50％、55％、60％、65％或70％。
优选地，所述无机纤维选自E玻璃纤维、NE玻璃纤维、L玻璃纤维、石英纤维的任意一种或至少两种的组合。
优选地，所述无机纤维平均直径小于10微米，例如9微米、8微米、7微米、6微米、5微米、4微米、3微米、2微米或1微米等，优选1-5微米。
优选地，所述无机纤维平均长度为1-100毫米，例如100毫米、90毫米、80毫米、70毫米、60毫米、50毫米、40毫米、30毫米、20毫米、10毫米、5毫米。本发明中无机填料的平均直径、平均长度都采用扫描电镜观察测试获得。
优选地，所述低介电损耗无纺布单重为20-200克/平方米，例如20克/平方米、25克/平方米、30克/平方米、35克/平方米、40克/平方米、50克/平方米、60克/平方米、80克/平方米、100克/平方米、120克/平方米、150克/平方米、180克/平方米或200克/平方米，优选20-100克/平方米。
另一方面，本发明提供了如上所述低介电损耗无纺布的制备方法，将无机纤维与粘结剂混合，浸渍，经过抄纸成型，烘干得到所述低介电损耗无纺布。
优选地，所述浸渍的时间为40～50min，例如40min、43min、45min、48min或50min。
优选地，所述烘干的温度为120～150℃，例如120℃、125℃、130℃、135℃、140℃、145℃或150℃。
当粘结剂选自含氟树脂乳液时，烘干后要增加烧结步骤，使含氟树脂熔融成膜。
优选地，所述烧结的温度为220℃-370℃，例如220℃、230℃、250℃、270℃、290℃、300℃、320℃、340℃、360℃或370℃，烧结的时间为28～30min。
另一方面，本发明提供一种预浸料，所述预浸料包括如上所述的低介电损耗无纺布和通过浸渍附着在其上的树脂组合物。
优选地，所述树脂组合物为含氟树脂乳液；
优选地，所述含氟树脂乳液选自聚全氟乙丙烯乳液、聚偏氟乙烯乳液、四氟乙烯-全氟烷基乙烯基醚共聚物乳液、乙烯-四氟乙烯共聚物乳液、聚三氟氯乙烯乳液或乙烯-三氟氯乙烯共聚物乳液中的任意一种或至少两种的组合。
另一方面，本发明提供一种覆铜板，所述覆铜板包括铜箔，以及如上所述的预浸料。
另一方面，本发明提供一种印制电路板，所述印制电路板包括铜箔，以及如上所述的预浸料。
相对于现有技术，本发明具有以下有益效果：
本发明的无纺布介电损耗低，均匀性好，厚度一致，纤维各向分布一致，拉伸强度高，可在浸渍低介电损耗树脂时添加较多的介电填料，制备低介电损耗以及高剥离强度的高频覆铜板。
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。本领域技术人员应该明了，所述实施例仅仅是帮助理解本发明，不应视为对本发明的具体限制。
以下实施例和比较例中使用的原料如下：
FEP树脂乳液，粒径0.20μm，固含量50wt％，日本大金公司生产，牌号：ND-110。
PFA树脂乳液，粒径0.20μm，固含量55wt％，日本大金公司生产，牌号：AD-2CR。
PTFE树脂乳液，粒径0.25μm，固含量55wt％，日本大金公司生产，牌号：D210C。
聚烯烃乳液，粒径0.1μm，固含量45wt％，北京燕山石化样品。
聚苯醚粘结剂：称取100份乙烯基改性聚苯醚(三菱瓦斯OPE-2ST)溶解于甲苯溶剂，经搅拌均匀后制得聚苯醚粘结剂。
低热膨胀系数树脂A：取上述PTFE树脂乳液450g，进行高速搅拌混合2h，得到均一的树脂组合物。
热固性树脂A：将30重量份乙丙橡胶(数均分子量80000g/mol，美国狮子化学公司)、40重量份聚丁二烯(分子量3200g/mol，日本曹达株式会社)、2重量份过氧化苯甲酰(上海康朗生物科技有限公司)溶于50重量份二甲苯中，混合均匀，得到均一的树脂组合物。
热固性树脂B：将70重量份的甲基丙烯酸封端聚苯醚树脂MMA-PPE(SA9000，SABIC公司)和70重量份作为溶剂的甲苯溶剂混合，溶解完全得到官能化聚苯醚树脂溶液，然后加入30重量份的苯乙烯-丁二烯共聚物R100(Sartomer公司)作为交联固化剂，加入3重量份的过氧化异丙苯DCP作为引发剂，15重量份的溴阻燃剂乙基-双(四溴苯邻二甲酰亚胺)BT-93W(雅宝公司：溴含量67.2％)，将上述混合物在甲苯中混合，并搅拌溶解以得到均一的树脂组合物。
平均直径5μm的E玻璃纤维，中国巨石股份有限公司
平均直径5μm的NE玻璃纤维，中国巨石股份有限公司
平均直径1μm和5μm的石英纤维，中国神玖
平均直径8μm的E玻璃纤维，中国巨石股份有限公司
无纺布，由环氧粘结剂和平均直径13μm的E玻璃纤维制备，陕西华特
无纺布，由丙烯酸酯粘结剂和平均直径13μm的E玻璃纤维制备，陕西华特无纺布，由三聚氰胺粘结剂和平均直径13μm的E玻璃纤维制备，陕西华特。
实施例1
在本实施例中提供一种低介电损耗无纺布，所述低介电损耗无纺布由玻璃纤维和粘结剂组成，所述粘结剂为FEP乳液。
具体制备方法包括以下步骤：
将92重量份E玻璃纤维(平均直径5微米)与8重量份FEP粘结剂浸渍45min，经过抄纸成型，再使用150℃烘箱干燥后，再于高温烘箱300℃环境下烧结30min，取出冷却后制得单重为20克/平方米的无纺布A。
实施例2
将85重量份NE玻璃纤维(平均直径5微米)与15重量份FEP粘结剂浸渍45min，经过抄纸成型，再使用150℃烘箱干燥后，再于高温烘箱300℃环境下烧结30min，取出冷却后制得单重为75克/平方米的无纺布B。
实施例3
将70重量份石英纤维(平均直径1μm和5μm，重量比为1:4)与30重量份FEP粘结剂浸渍45min，经过抄纸成型，再使用140℃烘箱干燥后，再于高温烘箱220℃环境下烧结28min，取出冷却后制得单重为75克/平方米的无纺布C。
实施例4
将85重量份E玻璃纤维(平均直径8微米)与15重量份FEP粘结剂浸渍45min，经过抄纸成型，再使用140℃烘箱干燥后，再于高温烘箱350℃环境下烧结28min，取出冷却后制得单重为75克/平方米的无纺布D。
实施例5
将85重量份E玻璃纤维(平均直径8微米)与15重量份聚烯烃粘结剂粘结剂浸渍45min，经过抄纸成型，再于烘箱120℃环境下干燥，取出冷却后制得单重为120克/平方米的无纺布E。
实施例6
将85重量份E玻璃纤维(平均直径8微米)与15重量份乙烯基改性聚苯醚(三菱瓦斯OPE-2ST)粘结剂浸渍45min，经过抄纸成型，再于烘箱200℃环境下干燥，取出冷却后制得单重为120克/平方米的无纺布F。
如上实施例的无纺布的主要材料和参数总结于如下表1中：
表1
Figure BDA0003432383220000071
Figure BDA0003432383220000081
实施例7
在本实施例中提供一种PTFE覆铜板，制备方法具体包括以下步骤：
步骤(1)：将低热膨胀系数树脂A胶液用上胶机浸胶在实施例1中的无纺布A上，得到上胶树脂含量为90％的预浸料H。
步骤(2)：将步骤(1)得到的预浸料H置于100℃的真空烘箱中，烘烤1h，去除分水，在260℃下烘烤1h去除助剂，在350℃下烘烤10min后得到厚度0.25mm的粘结片。
步骤(3)：将单张粘结片的上下两面覆盖1OZ厚的铜箔进行层压，施加压力400PSI，最高温度和保留时间为380℃/60min，即得到PTFE覆铜板。
实施例8
与实施例7中区别仅在于，步骤(1)无纺布A改为无纺布B，得到预浸料I；
实施例9
与实施例7中区别仅在于，步骤(1)无纺布A改为无纺布C，得到预浸料J。
实施例10
与实施例7中区别仅在于，步骤(1)无纺布A改为无纺布D，得到预浸料K。
实施例11
在本实施例中提供一种高频电路基板，制备方法具体包括以下步骤：
步骤(1)：将热固性树脂A胶液用上胶机浸胶在实施例5中的无纺布E上，得到上胶树脂含量为90％的预浸料M。
步骤(2)：将步骤(1)预浸料M置于100℃的烘箱中，烘烤1h，去除溶剂，得到粘结片。
步骤(3)：在单张粘结片的树脂层的上下两面覆盖1OZ厚的铜箔进行叠配，放进压机进行固化制得高频电路基板，所述固化的温度为200℃，固化90min，所述固化的压力为50kg/cm2。
实施例12
在本实施例中提供一种高频电路基板，制备方法具体包括以下步骤：
步骤(1)：将热固性树脂B胶液用上胶机浸胶在实施例6中的无纺布F上，得到上胶树脂含量为90％的预浸料N。
步骤(2)：将步骤(1)预浸料N在100℃烘箱中干燥，除去甲苯溶剂，制得粘结片。
步骤(3)：在单张粘结片的树脂层上下两面配以1OZ厚度的铜箔，在压机中真空层压固化90min，固化压力为50kg/cm2，固化温度为200℃，制得高频电路基板。
比较例1
与实施例7中区别仅在于，步骤(1)无纺布A改为环氧粘结剂的无纺布，其余完全相同。
比较例2
与实施例7中区别仅在于，步骤(1)无纺布A改为丙烯酸酯粘结剂的无纺布，其余完全相同。
比较例3
与实施例7中区别仅在于，步骤(1)无纺布A改为三聚氰胺粘结剂的无纺布，其余完全相同。
比较例4
与实施例11中区别仅在于，步骤(1)无纺布E改为环氧粘结剂的无纺布，其余完全相同。
比较例5
与实施例12中区别仅在于，步骤(1)无纺布F改为环氧粘结剂的无纺布，其余完全相同。
比较例6
与实施例7中区别仅在于，步骤(1)无纺布A中的粘结剂过量，比例是50％，其余完全相同。
对实施例7-12以及比较例1-6的覆铜板或者高频电路基板进行性能评价，方法如下：
1、Dk和Df：采用SPDR(splite post dielectric resonator)法进行测试，测试条件为A态，频率为10GHz。
2、剥离强度：GB/T 4722-20177.2方法。
测试结果如表2和表3所示。
表2
Figure BDA0003432383220000101
Figure BDA0003432383220000111
表3
Figure BDA0003432383220000112
从表2和表3可以看出：
实施例7-10可以看出采用低损耗粘结剂制备的无纺布与PTFE混合制备成覆铜板后，其介电损耗(Dk(10GHz)低于2.26，Df(10GHz)低于0.0013)和剥离强度(1.3N/mm以上)明显优于比较例1-3采用的普通无纺布所制成的覆铜板性能。
实施例11与对比例4可以采用低损耗粘结剂制备的无纺布与碳氢体系制备成覆铜板后，其介电损耗和剥离强度明显优于比较例4采用的普通无纺布所制成的覆铜板性能。
实施例12与对比例5可以看出采用低损耗粘结剂制备的无纺布与聚苯醚体系制备成覆铜板后，其介电损耗和剥离强度明显优于比较例5采用的普通无纺布所制成的覆铜板性能。
对比例6采用的低损耗粘结剂过量，导致板材介电损耗过高。
申请人声明，本发明通过上述实施例来说明本发明的低介电损耗无纺布及其制备及其应用，但本发明并不局限于上述实施例，即不意味着本发明必须依赖上述实施例才能实施。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 (10)

1.一种低介电损耗无纺布，其特征在于，所述低介电损耗无纺布由无机纤维和粘结剂组成，所述的粘结剂为含氟树脂乳液、聚烯烃乳液、聚苯醚树脂或氰酸酯树脂中的任意一种或至少两种的组合。
2.根据权利要求1所述的低介电损耗无纺布，其特征在于，所述低介电损耗无纺布中无机纤维的重量百分比为60-95％，粘结剂的重量百分比为5％-40％。
3.根据权利要求1或2所述的低介电损耗无纺布，其特征在于，所述粘结剂为含氟树脂乳液；
优选地，所述含氟树脂乳液选自聚全氟乙丙烯乳液、聚偏氟乙烯乳液、四氟乙烯-全氟烷基乙烯基醚共聚物乳液、乙烯-四氟乙烯共聚物乳液、聚三氟氯乙烯乳液或乙烯-三氟氯乙烯共聚物乳液中的任意一种或至少两种的组合；
优选地，所述含氟树脂乳液固含量为30-70％；
优选地，所述含氟树脂乳液中含氟树脂粒径0.10μm～0.40μm。
4.根据权利要求1-3中任一项所述的低介电损耗无纺布，其特征在于，所述聚烯烃乳液选自不饱和聚丁二烯树脂乳液、苯乙烯-丁二烯-苯乙烯三嵌段共聚物乳液、氢化苯乙烯-丁二烯-苯乙烯三嵌段共聚物乳液或丁苯树脂乳液中的任意一种或至少两种组合；
优选地，所述聚烯烃乳液中固含量为30-70％。
5.根据权利要求1-4中任一项所述的低介电损耗无纺布，其特征在于，所述无机纤维选自E玻璃纤维、NE玻璃纤维、L玻璃纤维、石英纤维的任意一种或至少两种的组合；
优选地，所述无机纤维平均直径小于10微米，优选1-5微米；
优选地，所述无机纤维平均长度为1-100毫米，优选1-10毫米。
6.根据权利要求1-5中任一项所述的低介电损耗无纺布，其特征在于，所述低介电损耗无纺布单重为20-200克/平方米，优选20-100克/平方米。
7.一种如上权利要求1-6中任一项所述的低介电损耗无纺布的制备方法，其特征在于，所述制备方法包括以下步骤：将无机纤维与粘结剂混合，浸渍，经过抄纸成型，烘干得到所述低介电损耗无纺布。
8.一种预浸料，其特征在于，所述预浸料包括如权利要求1-6中任一项所述的低介电损耗无纺布和通过浸渍附着在其上的树脂组合物；
优选地，所述树脂组合物为含氟树脂乳液；
优选地，所述含氟树脂乳液选自聚全氟乙丙烯乳液、聚偏氟乙烯乳液、四氟乙烯-全氟烷基乙烯基醚共聚物乳液、乙烯-四氟乙烯共聚物乳液、聚三氟氯乙烯乳液或乙烯-三氟氯乙烯共聚物乳液中的任意一种或至少两种的组合。
9.一种覆铜板，其特征在于，所述覆铜板包括铜箔，以及如权利要求8所述的预浸料。
10.一种印制电路板，其特征在于，所述印制电路板包括铜箔，以及如权利要求8所述的预浸料。
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