CN111995832B - 树脂组合物、胶黏剂及柔性覆铜板 - Google Patents
树脂组合物、胶黏剂及柔性覆铜板 Download PDFInfo
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- CN111995832B CN111995832B CN202010525000.9A CN202010525000A CN111995832B CN 111995832 B CN111995832 B CN 111995832B CN 202010525000 A CN202010525000 A CN 202010525000A CN 111995832 B CN111995832 B CN 111995832B
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本发明提供了一种树脂组合物、胶黏剂及柔性覆铜板。以重量百分比计，树脂组合物包括：35～45％的环氧树脂，环氧树脂选自双环戊二烯酚醛环氧树脂、联苯型环氧树脂和萘环型环氧树脂中的任意一种或多种；1～3.5％的固化剂；25～35％的增韧剂；15～25％氟树脂；10～20％的阻燃剂；以及1～3％的固化促进剂。上述树脂组合物的各组分混合后作为胶黏剂应用于柔性覆铜板中时，可以实现对聚酰亚胺和其它低介电、低损耗薄膜的牢固粘结，进而可以在聚酰亚胺膜上设置其他与铜箔热膨胀系数差异较小的低介电、低损耗薄膜，使得铜箔之上的介电层厚度得以提高，从而使所形成的柔性覆铜板满足5G高频、高速的无线传输要求。
Description
技术领域
本发明涉及柔性线路板技术领域，具体而言，涉及一种树脂组合物、胶黏剂及柔性覆铜板。
背景技术
近年来，随着终端应用产品的功能整合愈来愈强，反应速度必须愈来愈快，软板高频/高速化的趋势越来越重要。因为高介电常数(Dk)会使信号传递速度变慢，高介电损失(Df)会使信号部分转化为热能损耗在基板材料中，因此降低材料Dk/Df已成为柔性基板材料之趋势，各种低Dk/Df的新技术和新材料也不断涌现出来。
针对这些材料要求，作为柔性印刷电路板(FPC)的基材膜，已经提出具有低介电特性的液晶聚合物(LCP)、间规聚苯乙烯、聚苯硫醚等基材膜，以替代以前的聚酰亚胺、聚对苯二甲酸乙二酯膜等。最常见的是LCP，因其具有高频传输所需的低介电常数及低介电损失，在智能手机天线板的使用已逐渐浮出水面。然而，LCP的加工必须使用高温设备及条件，这与现行FPC的传统制程明显不同，因此采用LCP作为基材膜时，不仅要更换设备，也同时影响到生产速度。而传统聚酰亚胺覆铜基板无需更换FPC生产设备，生产制程符合现今软板制作。因此，降低介电常数以及损耗成为聚酰亚胺覆铜基板开发的首要目标。
聚酰亚胺覆铜基板的生产制作，主要是在聚酰亚胺酸涂布于铜箔上，再经去溶剂和加热处理形成聚酰亚胺覆铜基板。然而，在覆铜板生产过程中，因聚酰亚胺与铜箔之间的热膨胀系数差异，容易造成涂覆聚酰亚胺后，经过烘烤程序，造成覆铜板卷取，形成生产制作障碍，尤其是薄铜厚聚酰亚胺的叠构组合，比如现有制作工艺可达到的规格为1/3Oz铜箔(12μm)涂覆1.5mil(大约38μm)聚酰亚胺层。然而，为了符合5G高频/高速无线传输应用需求，柔性印刷电路板须符合线路设计的阻抗匹配(100ohm)，聚酰亚胺的厚度需要往更厚的厚度设计，才更能满足设计需求。
公开号为CN104691066A的中国专利申请公开了一种低介电常数的多层聚酰亚胺膜制作方法，该制作方法公开了一种三层聚酰亚胺膜，其中第一层以至少两种的芳香族二胺类和至少两种之芳香族四羧酸二酐类聚合而成，并额外添加四氟乙烯；第二层和第三层系以至少两种的芳香族二胺类和至少两种之芳香四羧酸二酐类聚合而成，并额外添加有机硅化合物，以增加聚醯亚胺膜与金属层的接着力。然而，此技术所制造的聚酰亚胺膜具有孔洞结构，使其机械强度下降，而不利于高频基板发展。
授权公告号为TW I591100B的中国台湾专利公开一种低介电常数聚酰亚胺覆铜基板制造方法，此专利公开了含氟高分子分散液溶于溶剂以及芳香族二胺中，再加入芳香族二酐进行聚合得到聚硫胺酸溶液，再以传统涂布方式进行涂布，除溶剂以及后续亚胺化程序，得到具有低介电/低损耗的聚酰亚胺覆铜基板。虽然此法可生产低介电/低损耗之聚酰亚胺覆铜基板，但因聚酰亚胺与铜箔的热膨胀系数差异，制作1/3 Oz(12μm)铜箔涂布38μm聚酰亚胺的覆铜板已是极限，对于涂覆层更厚的聚酰亚胺涂布需求是有相当难度。
为了符合5G高频/高速无线传输软板阻抗匹配需求，单面板覆铜基板介电层增厚至50μm是必须的，且此基板材料特性必须保有优异之机械特性、耐热性、电性等，但是目前的覆铜板基板介电层增加至50μm时，容易与铜箔剥离。
发明内容
本发明的主要目的在于提供一种树脂组合物、胶黏剂及柔性覆铜板，以解决现有技术中聚酰亚胺覆铜板难以满足5G的高频/高速无线传输要求的问题。
为了实现上述目的，根据本发明的一个方面，提供了一种树脂组合物，以重量百分比计，树脂组合物包括：35～45％的环氧树脂，环氧树脂选自双环戊二烯酚醛环氧树脂、联苯型环氧树脂和萘环型环氧树脂中的任意一种或多种；1～3.5％的固化剂；25～35％的增韧剂；15～25％氟树脂；10～20％的阻燃剂；以及1～3％的固化促进剂。
进一步地，上述环氧树脂的环氧当量为160～2000g/eq，优选环氧树脂的摩尔体积≥200mL/mol，分子极化率≤85C·m2/V，优选环氧树脂选自一种或多种双环戊二烯酚醛环氧树脂的混合物，更优选为DIC公司的HP-7200系列的双环戊二烯酚醛环氧树脂和圣东实业的SEV-3408系列的双环戊二烯酚醛环氧树脂的混合物，进一步优选HP-7200系列的双环戊二烯酚醛环氧树脂和SEV-3408系列的双环戊二烯酚醛环氧树脂的重量比为3～5:4。
进一步地，上述氟树脂为树脂粉末，优选树脂粉末的平均粒径在10μm以下，优选为0.1～10μm，更优选为0.1～7μm，进一步优选为0.1～5μm，优选氟树脂为聚四氟乙烯、三氟氯乙烯、全氟烷氧基聚合物、氟化乙烯-丙烯共聚物、聚全氟亚乙烯基聚合物组成的组中的任意一种或多种。
进一步地，上述固化剂选自多胺基类固化剂、酞酐类固化剂、酯类固化剂组成的组中的任意一种或多种的组合，优选多胺基类固化剂为二乙撑基三胺、二胺基二苯基甲烷、3,3-二胺基二苯基砜，4,4-二胺基二苯基砜和双腈胺，酯类固化剂为胜东实业的SHC-4314M65、SHC-5620TM65和SAP-641。
进一步地，上述增韧剂选自聚酰亚胺树脂、聚酯树脂、丁腈橡胶、苯乙烯-丁二烯橡胶、苯乙烯-丁二烯-苯乙烯嵌段共聚物中的任意一种。
进一步地，上述阻燃剂选自磷系阻燃剂和含金属化合物阻燃剂，优选含金属化合物阻燃剂为金属氧化物或金属氢氧化物，优选金属氧化物的平均粒径为1～5μm。
进一步地，上述固化促进剂选自路易斯碱系固化促进剂和路易斯酸系固化促进剂中的任意一种或多种，路易斯碱系固化促进剂为咪唑和三氟化硼胺复合物、2-甲基咪唑、2-苯基咪唑、2-乙基-4-甲基咪唑与4-二甲基胺基吡啶，路易斯酸系固化促进剂为有机金属盐类化合物，优选为锰、铁、钴、镍、铜、锌的有机盐。
根据本发明的另一方面，提供了一种胶黏剂，将溶剂与上述任一种的树脂组合物混合制备而成，胶黏剂的固含量为35～60％。
根据本发明的又一方面，提供了一种柔性覆铜板，柔性覆铜板包括铜基板和设置在铜基板上的介电层，该介电层包括：聚酰亚胺膜，设置在铜基板的表面上；粘结层，采用上述的胶黏剂制备而成；低介电/低损耗膜，通过粘结层与聚酰亚胺膜粘结，低介电/低损耗膜与铜基板的热膨胀系数差值的绝对值为A，聚酰亚胺与铜基板的热膨胀系数差值的绝对值为B，其中A小于B。
进一步地，上述介电层的厚度大于50μm，优选聚酰亚胺膜的厚度为20～30μm，优选低介电/低损耗薄膜为聚醚醚酮膜。
应用本发明的技术方案，采用双环戊二烯酚醛环氧树脂、联苯型环氧树脂和萘环型环氧树脂中的任意一种或多种作为树脂组合物的环氧树脂，上述各树脂具有低介电、低损耗性能，同时本申请的组合物中采用的氟树脂同样具有低介电低损耗性能，因此可以满足5G高频、高速无线传输对于介电性能和损耗水平的要求。上述树脂组合物的各组分混合后作为胶黏剂应用于柔性覆铜板中时，可以实现对聚酰亚胺和其它低介电、低损耗薄膜的牢固粘结，进而可以在聚酰亚胺膜上设置其他与铜箔热膨胀系数差异较小的低介电、低损耗薄膜，使得铜箔之上的介电层厚度得以提高，从而使所形成的柔性覆铜板满足5G高频、高速的无线传输要求。
具体实施方式
需要说明的是，在不冲突的情况下，本申请中的实施例及实施例中的特征可以相互组合。下面将结合实施例来详细说明本发明。
如本申请背景技术所分析的，现有技术的聚酰亚胺覆铜基板的聚酰亚胺膜厚度仅能达到38μm，如果继续增加厚度将会导致聚酰亚胺膜从铜基板上的剥离，进而难以满足5G高频/高速无线传输的要求，为了解决该问题，本身请提供了一种树脂组合物、胶黏剂及柔性覆铜板。
在本申请一种典型的实施方式中，提供了一种树脂组合物，以重量百分比计，该树脂组合物包括35～45％的环氧树脂、1～3.5％的固化剂、25～35％的增韧剂、1～3.5％的固化剂、25～35％的增韧剂、15～25％的氟树脂、10～20％的阻燃剂以及1～3％的固化促进剂，环氧树脂选自双环戊二烯酚醛环氧树脂、联苯型环氧树脂和萘环型环氧树脂中的任意一种或多种。
本申请采用双环戊二烯酚醛环氧树脂、联苯型环氧树脂和萘环型环氧树脂中的任意一种或多种作为树脂组合物的环氧树脂，上述各树脂具有低介电、低损耗性能，同时本申请的组合物中采用的氟树脂同样具有低介电低损耗性能，因此可以满足5G高频、高速无线传输对于介电性能和损耗水平的要求。上述树脂组合物的各组分混合后作为胶黏剂应用于柔性覆铜板中时，可以实现对聚酰亚胺和其它低介电、低损耗薄膜的牢固粘结，进而可以在聚酰亚胺膜上设置其他与铜箔热膨胀系数差异较小的低介电、低损耗薄膜，使得铜箔之上的介电层厚度得以提高，从而使所形成的柔性覆铜板满足5G高频、高速的无线传输要求。
具体地，传统环氧树脂其Dk约在3.3～3.6之间，Df约在0.023～0.035之间。本申请所选用的环氧树脂的Dk大约在3.0～3.1之间，Df在0.008～0.01之间。然而，为了让整体配方材料达到Dk≤3.0、Df≤0.007，单靠上述Low Dk/Df环氧树脂是不足的。氟树脂具有极佳之Low Dk/Df电性表现，将氟树脂以类似添加剂的方式加入配方系统，来达到更低Dk/Df之目标。但由于氟树脂极性偏低，一般高极性的环氧树脂与其混合容易造成相分离现象，本申请的Low Dk/Df环氧树脂采用低极性的苯环或萘环结构，因此容易与低极性的氟树脂兼容，来达到进行较佳的氟树脂分散，以获得更佳的电性表现。
上述双环戊二烯酚醛环氧树脂的通式为：
联苯型环氧树脂的通式为：
萘环型环氧树脂的通式为：
优选，上述环氧树脂的环氧当量为160～2000g/eq。上述环氧树脂固化前分子较小，因为铜箔其表面结构为粗糙的结构，固化之前的较小分子环氧树脂可以容易填入凹凸粗糙的铜箔表面；当温度提高固化剂产生作用时，较小分子的环氧树脂开始进行固化，并穿插于大分子量的氟树脂高分子结构中，因此紧密得与铜箔的表面粘结，形成如同钩锚效应来达到高粘结性能。
用于本申请的环氧树脂处理满足上述低介电和低损耗的要求外，为了进一步提高其低介电和低损耗性能，并提高其与氟树脂的兼容性，优选上述环氧树脂的摩尔体积≥200mL/mol，分子极化率≤85C·m2/V，优选环氧树脂选自一种或多种双环戊二烯酚醛环氧树脂的混合物，更优选为DIC公司的HP-7200系列的双环戊二烯酚醛环氧树脂和圣东实业的SEV-3408系列的双环戊二烯酚醛环氧树脂的混合物，进一步优选HP-7200系列的双环戊二烯酚醛环氧树脂和SEV-3408系列的双环戊二烯酚醛环氧树脂的重量比为3～5:4。
本申请的氟树脂可以采用现有技术中常用的氟树脂，为了提高氟树脂介电性能的发挥，优选上述氟树脂为树脂粉末。另外，为了使氟树脂与其它组分更充分地接触反应，优选树脂粉末的平均粒径在10μm以下，优选为0.1～10μm，更优选为0.1～7μm，进一步优选为0.1～5μm，优选氟树脂为聚四氟乙烯(PTFE)、三氟氯乙烯(CTFE)、全氟烷氧基聚合物(PFA)、氟化乙烯-丙烯共聚物(FEP)、聚全氟亚乙烯基聚合物(PVDF)组成的组中的任意一种或多种。
用于本申请的固化剂选用对上述环氧树脂和氟树脂具有促进固化作用的固化剂，优选上述固化剂选自多胺基类固化剂、酞酐类固化剂、酯类固化剂组成的组中的任意一种或多种的组合，优选多胺基类固化剂为二乙撑基三胺、二胺基二苯基甲烷、3,3-二胺基二苯基砜，4,4-二胺基二苯基砜和双腈胺，酯类固化剂为胜东实业的SHC-4314M65、SHC-5620TM65和SAP-641，上述酞酐类固化剂可以为酞酐、四氢酞酐或二者的组合。为了使本申请的树脂组合物在不同温度下具有不同的热固化程度，可以选用具有不同作用温度的固化剂，比如同时使用二胺基二苯基砜和双腈胺。
本申请使用增韧剂的主要目的是提供组合物在高温固化后具有高挠曲性，优选上述增韧剂选自可溶性聚酰亚胺树脂、聚酯树脂、丁腈橡胶、苯乙烯-丁二烯橡胶(SBR)、苯乙烯-丁二烯-苯乙烯嵌段共聚物(SBS)中的任意一种。进一步优选如下的各增韧剂：可溶性聚酰亚胺树脂(荒川化学，PIAD；日本宇部，P260；晋一化工，PI-220)、聚酯树脂(TOYOBO,BX-39SS)、端乙烯基丁腈橡胶(美国CVC特种化学品有限公司，VTBN1300X33LC)以及SBS橡胶(科胜高性能聚合物公司，D1192ET)。
阻燃剂用于在组合物应用与线路板时起到阻燃作用，现有技术中线路板中常用的阻燃剂均可考虑应用于本申请中，优选上述阻燃剂选自磷系阻燃剂和含金属化合物阻燃剂，优选含金属化合物阻燃剂为金属氧化物或金属氢氧化物，优选金属氧化物的平均粒径为1～5μm。上述金属氧化物可以为三氧化锑，金属氢氧化物可以为氢氧化铝或氢氧化镁，上述磷系阻燃剂可以选用双酚联苯磷酸盐、聚磷酸铵、对苯二酚-双-(联苯基磷酸盐)、亚磷酸钾、亚磷酸钠、二乙基磷酸铝中的任意一种或多种的组合。
为了降低固化温度，使用固化促进剂，为了对环氧树脂的固化发挥更好的促进作用，优选上述固化促进剂选自路易斯碱系固化促进剂和路易斯酸系固化促进剂中的任意一种或多种，路易斯碱系固化促进剂为咪唑和三氟化硼胺复合物、2-甲基咪唑、2-苯基咪唑、2-乙基-4-甲基咪唑与4-二甲基胺基吡啶，路易斯酸系固化促进剂为有机金属盐类化合物，优选为锰、铁、钴、镍、铜、锌的有机盐。
在本申请另一种典型的实施方式中，提供了一种胶黏剂，将溶剂与上述任一种的树脂组合物混合制备而成，胶黏剂的固含量为35～60％。
本申请的树脂组合物的双环戊二烯酚醛环氧树脂、联苯型环氧树脂和萘环型环氧树脂中、氟树脂具有低介电、低损耗性能，因此可以满足5G高频、高速无线传输对于介电性能和损耗水平的要求。上述树脂组合物的各组分混合后作为胶黏剂应用于柔性覆铜板中时，可以实现对聚酰亚胺和其它低介电、低损耗薄膜的牢固粘结，进而可以在聚酰亚胺膜上设置其他与铜箔热膨胀系数差异较小的低介电、低损耗薄膜，使得铜箔之上的介电层厚度得以提高，从而使所形成的柔性覆铜板满足5G高频、高速的无线传输要求。
上述胶黏剂使用的溶剂可包括但不限于丁酮、丙酮、甲苯、二甲苯、二甲基甲酰胺、丙二醇甲基醚或上述的任意组合。
在本申请又一种典型的实施方式中，提供了一种柔性覆铜板，该柔性覆铜板包括铜基板和设置在铜基板上的介电层，该介电层包括聚酰亚胺膜、粘结层和低介电/低损耗膜，聚酰亚胺膜设置在铜基板的表面上；粘结层采用上述的胶黏剂制备而成；低介电/低损耗膜通过粘结层与聚酰亚胺膜粘结，低介电/低损耗膜与铜基板的热膨胀系数差值的绝对值为A，聚酰亚胺与铜基板的热膨胀系数差值的绝对值为B，其中A小于B。
上述树脂组合物的各组分混合后作为胶黏剂应用于柔性覆铜板中时，可以在聚酰亚胺膜上设置其他与铜箔热膨胀系数差异较小的低介电、低损耗薄膜，使得铜箔之上的介电层厚度得以提高，从而使所形成的柔性覆铜板满足5G高频、高速的无线传输要求。
为了进一步提高柔性覆铜板的无线传输性能，优选上述介电层的厚度大于50μm，优选聚酰亚胺膜的厚度为20～30μm，优选低介电/低损耗膜为聚醚醚酮膜。比如优选为低介电/低损耗膜聚醚醚酮膜(KURABO，EX-PEEK,Dk≈3.2；Df≈0.002)、低介电/低损耗聚酰亚胺膜(达迈，LKA,Dk≈2.8；Df≈0.005，此为商业化聚酰亚胺膜，其CTE＝18.25，与铜箔(大约17)接近，因此热膨胀系数非常接近，涨缩影响较小)。
以下将结合实施例和对比例，进一步说明本申请的有益效果。
胶黏剂的制备过程：
首先，氟系树脂(比如各种氟树脂:全氟烷氧基聚合物(EA-2000,ASAHI Glass):D50＝2～3μm；聚四氟乙烯(YA-4,Admatechs):D50＝1.5～3μm；聚全氟亚乙烯基聚合物(2801-00，阿克玛)：D50＝3～5μm)需先溶于溶剂中，以高速搅拌(4000～5000rpm)进行搅拌1小时，即可得到氟系树脂分散液。另外，将固化剂、阻燃剂和固化促进剂溶于溶剂中，进行搅拌混合，混合时间大约1.5小时，接着添加低介电/低损耗环氧树脂，再添加增轫剂，最后再加入已分散好的氟系树脂分散液，进行搅拌混合3小时，即可得胶黏剂，配制好的胶黏剂粘度控制在800～1200cps，最终固形份大约50％左右。
按照上述流程制备各实施例和比较例的胶黏剂，各实施例和比较例的胶黏剂组成见表1-1和1-2。
表1-1
表1-2
HP-7200:低介电/低损耗双环戊二烯酚醛环氧树脂，日本DIC公司；
SEV-3408:低介电/低损耗双环戊二烯酚醛环氧树脂，胜东实业制；
HP-5000:低介电/低损耗双环戊二烯酚醛环氧树脂，日本DIC公司；
EBA-65:低介电/低损耗萘环型环氧树脂，上海华谊树脂有限公司；
4,4-DDS:4,4-二胺基二苯基砜，Atul公司制，商品名为AlulSulpho 44DDS；
DICY:二乙撑基三胺，勤裕企业制；
SHC-4314M65:酯类固化剂，胜东实业制；
PIAD：可溶性聚酰亚胺，荒川化学制；
P-260:可溶性聚酰亚胺，宇部化学制；
PI-22:可溶性聚酰亚胺，晋一化工制；
BX-39SS:聚酯，日本东洋纺制；
Hycar-1042:丙烯腈-丁二烯橡胶，南帝化工制；
EA-2000:全氟烷氧基聚合物，日本ASAHI GLASS制；
YA-4:聚四氟乙烯，日本Admatechs制
2801-00:聚全氟亚乙烯基聚合物，阿克玛制
OP-935:二乙基磷酸铝，克莱恩化学公司制；
H-42M:氢氧化铝，昭和化工制；
BF3MEA:三氟化硼-单乙基铵络合物，东信化学制；
C11Z:2-甲基咪唑，四国化成制。
覆铜板制作
本发明覆铜板制作使用的MPI为芳香族二胺(对二苯胺、二胺基二苯醚、二苯胺甲烷以及双三氟甲基联苯二胺所组成的至少两者)先溶于N-甲基吡咯烷酮(NMP)，再加入芳香族四羧酸二酐(可选联苯四羧酸二酸酐、均苯四羧酸二酐、二苯醚四羧酸二酐等)进行聚合反应形成聚酰胺酸。接着以涂布方式将聚酰胺酸涂布于1/3Oz(12μm)的铜箔上，经过去溶剂，高温亚胺化形成MPI覆铜基板，此MPI厚度约为25μm，MPI的Dk约2.80(@10GHz)，Df约为0.006(@10GHz)。为了增加整体厚度，选用具有低介电/低损耗的薄膜来增厚，优选为聚醚醚酮膜(KURABO，EX-PEEK,Dk≈3.2；Df≈0.002)、低介电/低损耗聚酰亚胺膜(达迈，LKA,Dk≈2.8；Df≈0.005，LKA膜CTE＝18.25，与铜箔接近，改善涨缩问题)。
将低介电/低损耗的胶体先涂布于LKA膜上，涂膜厚度约10μm，经过滚轮加温将此膜与MPI覆铜基板的MPI膜进行贴合达到增厚的效果，最后再以150℃、2小时固化，此低介电/低损耗的胶体即可紧密与MPI及LKA结合，在铜基板上形成单一介电层，达到增厚效果。
【评价方式】
介电常数(Dk)和介电损耗(Df)的测量：
以实施例和比较例中得到的树脂组合物胶体增厚的介电层于150℃干燥30min，在25℃及50％RH的条件下使用谐振器(安捷伦E5071BENA)通过分离介质谐振器(SPDR)方法测量各介电层的介电常数和介电损耗。
锡焊耐热性的比较：
参照IPC-TM650.2.6.8标准。将5厘米×5厘米的增厚覆铜基板浸入温度288℃的锡炉浸泡达30秒，取出试片后，观察表面是否起泡、变色、浮起和剥离等现象，以下述基准评估外观的变化。
○：无脱层且无变色
×：脱层且变色
抗张强度：
将由实施例及比较例得到的树脂组合物胶体增厚的复合介电层裁切成尺寸为152.4厘米×12.7厘米的测试品。接着，将这些测试品以万能拉力机，进行抗张强度的测量。
耐燃性：
本发明此处所称的耐燃性是以UL-94V0的规定进行。具体而言，对本发明增厚的介电层进行2次各为10秒的燃烧测试，若火焰在30秒内熄灭且无燃烧物落下，代表耐燃性佳。反之，则耐燃性不佳，具体评价标准如下：
○：火焰在30秒内熄灭，且无燃烧物落下，耐燃性佳
×：火焰未在30秒内熄灭，或有燃烧物落下，耐燃性不佳
上述各实施例和比较例的测试结果见表2。
表2
根据表2的数据可以发现，本申请的树脂组合物形成的胶黏剂可以成功进行介电层增厚的粘结，介电层厚度可超过2mil(50μm)。根据实施例及比较例的对比可以明显发现，低介电/低损耗环氧树脂、增轫剂、含氟树脂以及耐燃剂若未如本发明专利所呈现的使用量范围，其特性就有不同程度的差异，可见此低介电/低损耗树脂组合物胶体于柔性覆铜板中的重要性。
例如比较例1，添加的环氧树脂不足，漂锡耐热性不佳，并降低抗张强度；另外使用的增轫剂为丙烯腈-丁二烯橡胶，此橡胶本身介电及损耗比实施例所使用的可溶性聚酰亚胺、聚酯树脂高出许多，即影响整体复合材料的介电及损耗特性。比较例2添加的含氟树脂不足，整体材料介电/损耗也偏高；同时耐燃剂不足，耐燃特性亦无法通过UL-94VTM-0。比较例3，添加环氧树脂重量份不足，漂锡耐热性不佳，另外增轫剂重量增加，整体抗张强度大幅下降。
从以上的描述中，可以看出，本发明上述的实施例实现了如下技术效果：
本申请采用双环戊二烯酚醛环氧树脂、联苯型环氧树脂和萘环型环氧树脂中的任意一种或多种作为树脂组合物的环氧树脂，上述各树脂具有低介电、低损耗性能，同时本申请的组合物中采用的氟树脂同样具有低介电低损耗性能，因此可以满足5G高频、高速无线传输对于介电性能和损耗水平的要求。上述树脂组合物的各组分混合后作为胶黏剂应用于柔性覆铜板中时，可以实现对聚酰亚胺和其它低介电、低损耗薄膜的牢固粘结，进而可以在聚酰亚胺膜上设置其他与铜箔热膨胀系数差异较小的低介电、低损耗薄膜，使得铜箔之上的介电层厚度得以提高，从而使所形成的柔性覆铜板满足5G高频、高速的无线传输要求。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (18)
1.一种树脂组合物，其特征在于，以重量百分比计，所述树脂组合物包括：
35~45%的环氧树脂；
1~3.5%的固化剂；
25~35%的增韧剂；
15~25%氟树脂；
10~20%的阻燃剂；以及
1~3%的固化促进剂；
所述环氧树脂为HP-7200系列的双环戊二烯酚醛环氧树脂和SEV-3408系列的双环戊二烯酚醛环氧树脂的重量比为3~5:4组成的混合物，或者所述环氧树脂为HP-5000系列的双环戊二烯酚醛环氧树脂与EBA-65系列的萘环型环氧树脂以重量比为25:15或20:20组成的混合物，或者所述环氧树脂为HP-7200系列的双环戊二烯酚醛环氧树脂和EBA-65系列的萘环型环氧树脂以重量比为20:20组成的混合物；
所述氟树脂为聚四氟乙烯、三氟氯乙烯、全氟烷氧基聚合物、氟化乙烯-丙烯共聚物、聚全氟亚乙烯基聚合物组成的组中的任意一种或多种，
所述增韧剂选自聚酰亚胺树脂、聚酯树脂、丁腈橡胶、苯乙烯-丁二烯橡胶、苯乙烯-丁二烯-苯乙烯嵌段共聚物中的任意一种。
2.根据权利要求1所述的树脂组合物，其特征在于，所述氟树脂为树脂粉末。
3.根据权利要求2所述的树脂组合物，其特征在于，所述树脂粉末的平均粒径在10μm以下。
4.根据权利要求3所述的树脂组合物，其特征在于，所述树脂粉末的平均粒径为0.1~10μm。
5.根据权利要求3所述的树脂组合物，其特征在于，所述树脂粉末的平均粒径为0.1~ 7μm。
6.根据权利要求3所述的树脂组合物，其特征在于，所述树脂粉末的平均粒径为0.1 ~5μm。
7.根据权利要求1所述的树脂组合物，其特征在于，所述固化剂选自多胺基类固化剂、酞酐类固化剂、酯类固化剂组成的组中的任意一种或多种的组合。
8.根据权利要求7所述的树脂组合物，其特征在于，所述多胺基类固化剂为二乙撑基三胺、二胺基二苯基甲烷、3,3-二胺基二苯基砜，4,4-二胺基二苯基砜和双腈胺，所述酯类固化剂为胜东实业的SHC-4314M65、SHC-5620TM65和SAP-641。
9.根据权利要求1所述的树脂组合物，其特征在于，所述阻燃剂选自磷系阻燃剂和含金属化合物阻燃剂。
10.根据权利要求9所述的树脂组合物，其特征在于，所述含金属化合物阻燃剂为金属氧化物或金属氢氧化物。
11.根据权利要求10所述的树脂组合物，其特征在于，所述金属氧化物的平均粒径为1~5μm。
12.根据权利要求1所述的树脂组合物，其特征在于，所述固化促进剂选自路易斯碱系固化促进剂和路易斯酸系固化促进剂中的任意一种或多种，所述路易斯碱系固化促进剂为咪唑和三氟化硼胺复合物、2-甲基咪唑、2-苯基咪唑、2-乙基-4-甲基咪唑与4-二甲基胺基吡啶，所述路易斯酸系固化促进剂为有机金属盐类化合物。
13.根据权利要求12所述的树脂组合物，其特征在于，所述路易斯酸系固化促进剂为锰、铁、钴、镍、铜、锌的有机盐。
14.一种胶黏剂，将溶剂与权利要求1至13中任一项所述的树脂组合物混合制备而成，所述胶黏剂的固含量为35~60%。
15.一种柔性覆铜板，所述柔性覆铜板包括铜基板和设置在所述铜基板上的介电层，其特征在于，所述介电层包括：
聚酰亚胺膜，设置在所述铜基板的表面上；
粘结层，采用权利要求14所述的胶黏剂制备而成；
低介电/低损耗膜，通过所述粘结层与所述聚酰亚胺膜粘结，所述低介电/低损耗膜与所述铜基板的热膨胀系数差值的绝对值为A，所述聚酰亚胺与所述铜基板的热膨胀系数差值的绝对值为B，其中A小于B。
16.根据权利要求15所述的柔性覆铜板，其特征在于，所述介电层的厚度大于50μm。
17.根据权利要求15所述的柔性覆铜板，其特征在于，所述聚酰亚胺膜的厚度为20~30μm。
18.根据权利要求15所述的柔性覆铜板，其特征在于，所述低介电/低损耗薄膜为聚醚醚酮膜。
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