CN107848260B - 带树脂的铜箔、覆铜层叠板和印刷电路板 - Google Patents

带树脂的铜箔、覆铜层叠板和印刷电路板 Download PDF

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Publication number
CN107848260B
CN107848260B CN201680043034.6A CN201680043034A CN107848260B CN 107848260 B CN107848260 B CN 107848260B CN 201680043034 A CN201680043034 A CN 201680043034A CN 107848260 B CN107848260 B CN 107848260B
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resin
copper foil
resin layer
layer
copper
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CN107848260A (zh
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米田祥浩
松岛敏文
细井俊宏
桑子富士夫
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Mitsui Mining and Smelting Co Ltd
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Mitsui Mining and Smelting Co Ltd
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Abstract

本发明提供树脂层具有适于高频用途的优异的介电特性、且形成覆铜层叠板或印刷电路板时能发挥优异的层间密合性和耐热性的带树脂的铜箔。本发明的带树脂的铜箔在铜箔的至少单面上具备树脂层。而且，树脂层包含：含有环氧树脂、聚酰亚胺树脂和芳香族聚酰胺树脂的树脂混合物；和，咪唑系固化催化剂。

Description

带树脂的铜箔、覆铜层叠板和印刷电路板
技术领域
本发明涉及带树脂的铜箔、覆铜层叠板和印刷电路板。
背景技术
作为覆铜层叠板、印刷电路板的制造中使用的铜箔，已知有在单面具备树脂层的带树脂的铜箔用以提高与预浸料等树脂基材的密合性。需要说明的是，预浸料是指，合成树脂板、玻璃板、玻璃织布、玻璃无纺布、纸等基材中浸渗有合成树脂的复合材料的总称。
例如，专利文献1(日本专利第5118469号公报)中公开了一种带树脂层的铜箔，其在铜箔的单面具备含填料颗粒树脂层，记载了，含填料颗粒树脂层包含芳香族聚酰胺树脂聚合物、环氧树脂和固化促进剂，且为用作为氨基系硅烷偶联剂的苯基氨基硅烷进行过处理的含有填料颗粒的半固化树脂层。
另外，专利文献2(日本专利第3949676号公报)中公开一种带极薄粘接剂层的铜箔，其在未实施粗糙化处理的铜箔的单面具备用于与树脂基材良好地粘结并确保密合性的极薄底漆树脂层，记载了，极薄底漆树脂层是使用包含20～80重量份的环氧树脂(包括固化剂)、20～80重量份的芳香族聚酰胺树脂聚合物、和根据需要添加的固化促进剂的树脂混合物而形成的。该极薄底漆树脂层作为用于与树脂基材良好地粘结并确保密合性的极薄粘接剂层发挥功能。
进而，专利文献3(国际公开第2013/105650号)中公开了一种带粘接剂层的铜箔，其在铜箔的单面具备粘接剂层，记载了，粘接剂层是由包含聚苯醚化合物100质量份和5质量份以上且65质量份以下的苯乙烯丁二烯嵌段共聚物的树脂组合物形成的层。
另外，印刷电路板被广泛用于移动用电子设备等电子设备。特别是，伴随着近年来的移动用电子设备等的高功能化，为了大量信息的高速处理，推进信号的高频化，寻求适于高频用途的印刷电路板。对于这样的高频用印刷电路板，为了可以不降低品质地使高频信号输送，期望降低传输损耗。印刷电路板具备加工为布线图案的铜箔和绝缘树脂基材，传输损耗主要由源自铜箔的导体损耗和源自绝缘树脂基材的电介质损耗构成。
现有技术文献
专利文献
专利文献1：日本专利第5118469号公报
专利文献2：日本专利第3949676号公报
专利文献3：国际公开第2013/105650号
发明内容
因此，将带树脂层的铜箔用于高频用途时，期望抑制源自树脂层的电介质损耗。为此，要求树脂层的优异的介电特性、特别是介质损耗角正切低。然而，对比文件1和2中公开的带树脂层的铜箔虽然可以实现与预浸料等树脂基材的密合性的提高，但是介质损耗角正切高，因此，介电特性差，因而不适于高频用途。
本发明人等此次获得如下见解：在铜箔的至少单面上具备树脂层的带树脂的铜箔中，通过采用包含环氧树脂、聚酰亚胺树脂和芳香族聚酰胺树脂以及咪唑系固化催化剂的树脂层，树脂层具有适于高频用途的优异的介电特性，并且形成覆铜层叠板或印刷电路板时，可以发挥优异的层间密合性和耐热性。
因此，本发明的目的在于，提供：树脂层具有适于高频用途的优异的介电特性，并且形成覆铜层叠板或印刷电路板时，可以发挥优异的层间密合性和耐热性的带树脂的铜箔。
根据本发明的一方式，提供一种带树脂的铜箔，其为在铜箔的至少单面上具备树脂层的带树脂的铜箔，前述树脂层包含：含有环氧树脂、聚酰亚胺树脂和芳香族聚酰胺树脂的树脂混合物；和，咪唑系固化催化剂。
根据本发明的另一方式，提供一种覆铜层叠板，其具备上述方式的带树脂的铜箔，且前述树脂层已被固化。
根据本发明的另一方式，提供一种印刷电路板，其具备上述方式的带树脂的铜箔，且前述树脂层已被固化。
附图说明
图1为示出用于例1～19中的介电特性评价的样品的制作步骤的图。
图2为示出用于例1～19中的耐热性评价和铜箔密合性的评价的样品的制作步骤的图。
具体实施方式
带树脂的铜箔
本发明的带树脂的铜箔为在铜箔的至少单面上具备树脂层的带树脂的铜箔。带树脂的铜箔的树脂层包含树脂混合物；和，咪唑系固化催化剂。该树脂混合物含有环氧树脂、聚酰亚胺树脂和芳香族聚酰胺树脂。如此，通过采用包含环氧树脂、聚酰亚胺树脂和芳香族聚酰胺树脂以及咪唑系固化催化剂的树脂层，树脂层具有适于高频用途的优异的介电特性(低的介质损耗角正切)，并且形成覆铜层叠板或印刷电路板时，可以发挥优异的层间密合性和耐热性。用于制造覆铜层叠板或印刷电路板时，可以防止电路剥离等不良情况，这样的铜箔和树脂层间的优异的密合性和耐热性可以实现制品成品率的提高。另外，低的介质损耗角正切有利于降低电介质损耗，其结果，可以实现高频用途中的传输损耗的降低。因此，本发明的带树脂的铜箔可以优选作为网络设备中的高频数字通信用的印刷电路板用的绝缘层和导体层应用。作为这样的网络设备的例子，可以举出(i)基站内服务器、路由器等、(ii)企业内网络、(iii)高速移动通信的骨干系统等。
具体而言，对于本发明的带树脂的铜箔，在树脂层已固化的状态下，树脂层在频率1GHz下优选具有低于0.020的介质损耗角正切，更优选低于0.015、进一步优选低于0.008。需要说明的是，该介质损耗角正切典型地为0.001以上、更典型地具有0.002以上的值。另外，对于本发明的带树脂的铜箔，在树脂层已固化的状态下，依据JIS C6481-1996测定的、树脂层与铜箔间的剥离强度优选0.20kgf/cm以上、更优选0.40kgf/cm以上、进一步优选0.60kgf/cm以上。需要说明的是，该剥离强度典型地为1.4kgf/cm以下，更典型地具有1.2kgf/cm以下的值。
树脂层包含树脂混合物和咪唑系固化催化剂。而且，树脂混合物含有环氧树脂、聚酰亚胺树脂和芳香族聚酰胺树脂。
环氧树脂只要分子内具有2个以上的环氧基、且可以用于电气和电子材料用途就没有特别限定。作为环氧树脂的例子，可以举出双酚A型环氧树脂、双酚F型环氧树脂、双酚S型环氧树脂、苯酚酚醛清漆型环氧树脂、联苯酚醛清漆型环氧树脂、甲酚酚醛清漆型环氧树脂、脂环式环氧树脂、缩水甘油胺型环氧树脂、萘型环氧树脂、蒽型环氧树脂、二环戊二烯型环氧树脂、和它们的任意的组合。从保持固化物的耐热性的方面出发，优选芳香族环氧树脂或多官能环氧树脂，更优选为苯酚酚醛清漆型环氧树脂、萘型环氧树脂、甲酚酚醛清漆型环氧树脂或联苯酚醛清漆型环氧树脂。
聚酰亚胺树脂有利于介电特性的提高(特别是介质损耗角正切的降低)。树脂混合物中的聚酰亚胺树脂的优选含量相对于环氧树脂100重量份为160～340重量份、更优选为200～300重量份、进一步优选为220～280重量份。为这样的含量时，可以确保良好的耐热性并且可以体现优异的介电特性。聚酰亚胺树脂只要可以得到期望的介电特性、密合性和耐热性就没有特别限定，从可以形成与环氧树脂良好地相容的清漆和涂膜的方面出发，优选可溶于有机溶剂的聚酰亚胺树脂(以下，称为有机溶剂可溶性聚酰亚胺)。使聚酰亚胺树脂可溶的该有机溶剂的溶解度参数(SP值)优选7.0～17.0，作为这样的有机溶剂的优选例，可以举出甲乙酮、甲苯、二甲苯、N-甲基吡咯烷酮、二甲基乙酰胺、二甲基甲酰胺，环戊酮、环己酮、环己烷、甲基环己烷、乙二醇、乙二醇二甲基醚、乙二醇乙酸酯、和它们的任意的组合。从保持固化后的耐热性的方面出发，特别优选使用分子末端具有至少一个能与环氧基反应的官能团的物质。具体而言，对于聚酰亚胺树脂，作为其末端乃至侧链的官能团，优选具有选自由羧基、磺酸基、巯基和酚性羟基组成的组中的至少1种官能团。通过具有这样的官能团，聚酰亚胺树脂的有机溶剂可溶性和与环氧树脂的相容性提高。另外，热处理时与环氧树脂的聚合反应得到促进，进而聚酰亚胺树脂彼此的聚合反应得到促进，由此耐热性进一步高，且可以得到介质损耗角正切低的固化物。其中，更优选使用具有羧基作为末端或侧链的官能团的聚酰亚胺树脂。
作为优选的有机溶剂可溶性聚酰亚胺，可以举出使四羧酸二酐与二胺化合物进行酰亚胺化反应而得到物质。作为四羧酸二酐的例子，可以举出2,2-双(3,4-二羧基苯基)丙烷二酐、2,2-双(2,3-二羧基苯基)丙烷二酐、双(3,4-二羧基苯基)砜二酐、双(3,4-二羧基苯基)醚二酐、2,2-双(3,4-二羧基苯基)六氟丙烷二酐、2,2-双[4-(3,4-二羧基苯基)苯基]丙烷二酐、均苯四酸二酐、3,3’,4,4’-联苯四羧酸二酐、2,3,3’,4’-联苯四羧酸二酐、2,2’,3,3’-联苯四羧酸二酐、3,3’,4,4’-二苯甲酮四羧酸二酐、2,2’,3,3’-二苯甲酮四羧酸二酐、1,1-双(3,4-二羧基苯基)乙烷二酐、1,1-双(2,3-二羧基苯基)乙烷二酐、双(3,4-二羧基苯基)甲烷二酐、双(2,3-二羧基苯基)甲烷二酐、1,2,5,6-萘四羧酸二酐、2,3,6,7-萘四羧酸二酐、2,3,5,6-吡啶四羧酸二酐、3,4,9,10-苝四羧酸二酐等、或在它们的芳香族环上具有烷基、卤素原子的取代基的化合物、和它们的任意的组合等。其中，从提高树脂组合物的耐热性的方面出发，优选以2,2-双(3,4-二羧基苯基)六氟丙烷二酐、2,2-双[4-(3,4-二羧基苯基)苯基]丙烷二酐、2,3,3’,4’-联苯四羧酸二酐、或2,2’,3,3’-联苯四羧酸二酐为主的聚酰亚胺树脂。
另一方面，作为二胺的例子，可以举出3,4’-二氨基二苯基硫醚、4,4’-二氨基二苯基硫醚、3,4’-二氨基二苯基醚、4,4’-二氨基二苯基醚、3,4’-二氨基二苯基砜、4,4’-二氨基二苯基砜、双[4-(4-氨基苯氧基)苯基]砜、双[4-(3-氨基苯氧基)苯基]砜、双(4-氨基苯氧基)联苯、双[4-(4-氨基苯氧基)苯基]醚、1,4-双(4-氨基苯氧基)苯、1,3-双(4-氨基苯氧基)苯、2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷、2,2-双[4-(4-氨基苯氧基)苯基]丙烷、1,3-双(氨基甲基)环己烷和它们的任意的组合。
特别是，以聚酰亚胺树脂单独的形态计，在频率1GHz下，介电常数能取2.0～5.0、介质损耗角正切能取0.001～0.008的范围的聚酰亚胺树脂优选供于本发明的树脂组合物，更优选为介电常数能取2.0～3.0、介质损耗角正切能取0.001～0.005的范围的聚酰亚胺树脂。
另外，从充分地保持固化物的耐热性的观点出发，以聚酰亚胺树脂单独的形态计的软化点优选为70℃以上、更优选为90℃以上、进一步优选为120℃以上。软化点的测定可以通过JIS K 7196：2012而测定。此处“以聚酰亚胺树脂单独的形态计”是指，使溶剂从溶解有聚酰亚胺树脂的清漆蒸发干固直至溶剂含量成为0.1重量％以下而得到的固化物。另外，从进一步保持固化物的耐热性且保持对有机溶剂的溶解性能的方面出发，以聚酰亚胺树脂单独的形态计的玻璃化转变点优选为130℃以上、更优选为150～190℃。该玻璃化转变点可以通过动态粘弹性测定而确定。
芳香族聚酰胺树脂有利于树脂层的耐热性的提高。树脂混合物中的芳香族聚酰胺树脂的优选含量相对于环氧树脂100重量份为50～200重量份、更优选为80～150重量份、进一步优选为90～120重量份。为这样的含量时，可以确保良好的介电特性，并且可以体现优异的耐热性。芳香族聚酰胺树脂是指，通过芳香族二胺与二羧酸的缩聚而合成的物质。作为上述缩聚中使用的芳香族二胺的例子，可以举出3,4’-二氨基二苯基醚、4,4’-二氨基二苯基醚、4,4’-二氨基二苯基甲烷、3,3’-二氨基二苯基砜、间二甲苯二胺、3,3’-氧二苯胺等、和它们的任意的组合。另外，作为上述缩聚中使用的二羧酸的例子，可以举出草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸、富马酸、和它们的任意的组合。为了对芳香族聚酰胺树脂赋予耐热性，二羧酸优选为芳香族二羧酸，作为芳香族二羧酸的例子，可以举出邻苯二甲酸、间苯二甲酸、对苯二甲酸、富马酸、和它们的任意的组合。特别优选分子内含有酚性羟基的芳香族聚酰胺树脂。另外，对于该芳香族聚酰胺树脂，可以在不有损耐热性的范围内，在分子内适宜具有对芳香族聚酰胺树脂赋予挠性的化学键作为柔软链，也可以以与聚酰胺树脂的交联性聚合物合金的形式在以部分聚集状态存在。作为具有对芳香族聚酰胺树脂赋予挠性的化学键作为柔软链的化合物的例子，例如可以举出丁二烯、乙烯-丙烯共聚物、苯乙烯-丁二烯共聚物、羧酸丁二烯共聚物、丙烯腈-丁二烯共聚物、聚氨酯、聚氯丁二烯、硅氧烷等。
对于咪唑系固化催化剂，与环氧树脂的固化反应后不以离子的形式游离而作为环氧树脂的一部分组入分子结构中，因此，可以使树脂层的介电特性、绝缘可靠性优异。咪唑系固化催化剂的含量只要考虑树脂层的组成等各条件并适宜确定引起期望的固化的量就没有特别限定。作为咪唑固化催化剂的例子，可以举出2-十一烷基咪唑、2-十七烷基咪唑、2-乙基-4-甲基咪唑、2-苯基-4-甲基咪唑、1-氰基乙基-2-十一烷基咪唑、1-氰基乙基-2-乙基-4-甲基咪唑、2-乙基-4-甲基咪唑、1-氰基乙基-2-苯基咪唑、2-苯基-4,5-二羟基甲基咪唑、2-苯基-4-甲基-5-羟基甲基咪唑、2-甲基咪唑、和它们的任意的组合。作为咪唑系固化催化剂的优选例，可以举出2-甲基咪唑、2-乙基-4-甲基咪唑、2-苯基-4-甲基咪唑、2-苯基-4-甲基-5-羟基甲基咪唑，其中，从树脂层的半固化(B阶)状态下的化学稳定性的方面出发，可以举出具有苯基的咪唑系固化催化剂即2-苯基-4-甲基咪唑、2-苯基-4-甲基-5-羟基甲基咪唑作为更优选例。其中，可以特别优选举出2-苯基-4-甲基-5-羟基甲基咪唑。
根据期望，树脂层可以还包含无机填料。通过添加无机填料，可以使树脂层的介质损耗角正切理想地降低。无机填料可以适宜使用能用于树脂组合物的公知的物质，没有特别限定。作为优选的无机填料的例子，可以举出二氧化硅、氧化铝、滑石等的颗粒，从降低介质损耗角正切的观点出发，特别优选为二氧化硅颗粒。无机填料的粒径没有特别限定，从保持树脂层的表面平滑性和混合清漆时抑制聚集的方面出发，通过平均粒径激光衍射散射式粒度分布测定而测定的平均粒径D50优选0.01～2.0μm、更优选为0.01～1.0μm、进一步优选为0.01～0.5μm。树脂层中的无机填料的含量相对于环氧树脂、聚酰亚胺树脂和芳香族聚酰胺树脂(即树脂固体成分)的总量100重量份，优选为10～100重量份、更优选为10～70重量份、进一步优选为30～70重量份、特别优选为30～50重量份。为这样的含量时，介质损耗角正切优异，并且可以避免剥离强度的降低。
含有无机填料时，优选使用实施了特定的表面处理的填料颗粒。由此，可以使树脂层与铜箔的密合性更良好，可以使该带树脂层的铜箔与预浸料更牢固地密合。其结果，可以进一步提高剥离强度，可以抑制分层的发生。特别优选填料颗粒用硅烷偶联剂进行表面处理。作为硅烷偶联剂，可以使用氨基官能性硅烷偶联剂、丙烯酸官能性硅烷偶联剂、甲基丙烯酸官能性硅烷偶联剂、环氧官能性硅烷偶联剂、烯烃官能性硅烷偶联剂、巯基官能性硅烷偶联剂、乙烯基官能性硅烷偶联剂等各种硅烷偶联剂。上述中，更优选氨基官能性硅烷偶联剂、丙烯酸官能性硅烷偶联剂、甲基丙烯酸官能性硅烷偶联剂、乙烯基官能性硅烷偶联剂等。如此，通过对填料颗粒实施上述表面处理，与溶剂的湿润性提高，可以使填料颗粒良好地分散于树脂溶液中。其结果，可以得到层内均匀地分散有填料颗粒的树脂层。另外，通过对填料颗粒实施上述表面处理，可以使填料颗粒与上述树脂组合物的相容性良好，也可以使填料颗粒与树脂组合物的密合性良好。作为氨基官能性硅烷偶联剂的例子，可以举出N-2-(氨基乙基)-3-氨基丙基甲基二甲氧基硅烷、N-2-(氨基乙基)-3-氨基丙基三甲氧基硅烷、3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、3-三乙氧基甲硅烷基-N-(1,3-二甲基-丁叉基)丙基胺、N-苯基-3-氨基丙基三甲氧基硅烷等。作为甲基丙烯酸官能性硅烷偶联剂和丙烯酸官能性硅烷偶联剂的例子，可以举出3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二乙氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷3-丙烯酰氧基丙基三甲氧基硅烷等。作为乙烯基官能性硅烷偶联剂的例子，可以举出乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基苯基三乙氧基硅烷等。另外，也可以使用甲基三甲氧基硅烷、二甲基二甲氧基硅烷、苯基三甲氧基硅烷、甲基三乙氧基硅烷、二甲基二乙氧基硅烷、苯基三乙氧基硅烷等烷氧基硅烷。使用这些硅烷偶联剂的表面处理的方法没有特别限定，可以适宜使用适当的方法而进行。
树脂层的厚度没有特别限定，优选为0.1～100μm、更优选为0.5～70μm、进一步优选为1.0～50μm。为这些范围内的厚度时，通过涂布树脂组合物而容易形成树脂层，并且在与铜箔之间容易确保充分的密合性。
树脂层可以由其本身构成覆铜层叠板、印刷电路板中的绝缘层。另外，树脂层也可以作为用于与覆铜层叠板、印刷电路板中的预浸料粘结的底漆层形成于铜箔表面。上述情况下，带树脂的铜箔的树脂层作为底漆层可以提高预浸料与铜箔的密合性。因此，本发明的带树脂的铜箔可以在树脂层上具备预浸料。需要说明的是，对于该树脂层，可以将上述树脂组合物固化而得到，或将上述树脂组合物以为半固化(B阶)状态的树脂组合物层形式提供，也可以在作为后续工序的热加压中供于粘接固化。该热加压可以采用如下真空热加压法：预先达到真空后，在温度150～300℃、温度保持时间30～300分钟、压力10～60kgf/cm2的范围的条件下进行固化。
铜箔可以为经过电解制箔或压延制箔直接得到的金属箔(所谓生箔)，也可以为对至少任一面实施了表面处理的表面处理箔的形态。表面处理可以是为了在金属箔的表面提高乃至赋予任意性质(例如防锈性、耐湿性、耐化学药品性、耐酸性、耐热性、和与基板的密合性)而进行的各种表面处理。表面处理可以在金属箔的至少单面进行，也可以在金属箔的两面进行。作为对铜箔进行的表面处理的例子，可以举出防锈处理、硅烷处理、粗糙化处理、阻隔形成处理等。
铜箔的树脂层侧的表面中的、依据JIS B0601-2001测定的微观不平度十点高度Rzjis优选为2.0μm以下、更优选为1.5μm以下，进一步优选为1.0μm以下。为这样的范围内时，可以理想地降低高频用途中的传输损耗。即，可以使越高频越显著体现的由于铜箔的表皮效果而增大的源自铜箔的导体损耗降低，可以实现传输损耗的进一步降低。铜箔的树脂层侧的表面中的微观不平度十点高度Rzjis的下限值没有特别限定，从提高与树脂层的密合性的观点出发，Rzjis优选为0.005μm以上、更优选为0.01μm以上、进一步优选为0.05μm以上。
在保持上述微观不平度十点高度Rzjis的数值范围的范围内，在可以使与树脂层的耐热密合性显著提高的方面，优选在铜箔的树脂层侧的表面形成颗粒状突起。在可以使印刷电路板的高频传输损耗降低的方面，构成该颗粒状突起的金属优选为铜。对于颗粒状突起，在确保与树脂层的密合性作为物理性锚固效果、且可以较高地保持将铜箔作为布线层形成时的高频输送特性的方面，平均粒径优选为10～300nm、进一步优选为50～200nm。另外，从上述观点出发，颗粒状突起优选以40～280个/μm2的面密度存在，更优选为80～250个/μm2。这些颗粒状突起可以通过利用扫描型电子显微镜、以5000～50000倍进行表面观察来识别各颗粒。平均粒径可以根据针对任意20个颗粒的颗粒轮廓的面积圆当量直径的平均值而算出。作为颗粒状突起的形成方法的例子，可以举出电解处理、喷丸处理、和氧化还原处理，从颗粒的均匀形成的观点出发，优选电解处理，更优选为铜电解处理。例如作为电解处理液，通过使用铜浓度10～20g/L、游离硫酸浓度15～100g/L、9-苯基吖啶浓度100～200mg/L、和氯浓度20～100mg/L的水溶液进行电解镀，从而可以优选形成颗粒状突起。
铜箔的厚度没有特别限定，优选为0.1～100μm、更优选为0.15～40μm、进一步优选为0.2～30μm。为这些范围内的厚度时，可以采用印刷电路板的布线形成的一般图案形成方法、即、MSAP(改性·半添加)法、SAP(半添加)法、消减法等工艺。但铜箔的厚度例如成为10μm以下的情况下等，对于本发明的带树脂的铜箔，为了提高操作性，可以在具备剥离层和载体的带载体的铜箔的铜箔表面形成树脂层。
覆铜层叠板
本发明的带树脂的铜箔优选用于制作印刷电路板用覆铜层叠板。即，根据本发明的优选方式，提供具备上述带树脂的铜箔的覆铜层叠板、或使用上述带树脂的铜箔而得到的覆铜层叠板。上述情况下，上述带树脂的铜箔的树脂层已固化。该覆铜层叠板具备：本发明的带树脂的铜箔；和，与该带树脂的铜箔的树脂层密合而设置的绝缘基材层。上述情况下，树脂层可作为用于提高与绝缘基材层的密合性的底漆层发挥功能。带树脂的铜箔可以设置于绝缘树脂层的单面，也可以设置于两面。绝缘树脂层包含绝缘性树脂。绝缘基材层优选玻璃纤维填充预浸料、玻璃板、陶瓷板、树脂薄膜、或它们的组合。作为用作预浸料的绝缘性树脂的优选例，可以举出环氧树脂、氰酸酯树脂、聚酰亚胺树脂、马来酰亚胺三嗪树脂(BT树脂)、聚苯醚树脂、酚醛树脂等。树脂层可以由多层构成。其中，聚苯醚树脂和聚酰亚胺树脂在提高覆铜层叠板的输送特性的意义上也优选，与本发明的带树脂的铜箔中的树脂层的密合性变得特别优异。作为用作树脂薄膜的绝缘树脂的例子，可以举出聚酰亚胺树脂、液晶聚合物等。需要说明的是，考虑了各种用于形成覆铜层叠板的方法，但典型地，由使本发明的带树脂的铜箔与绝缘基材层粘结的方法形成。此外，还考虑了如下方法：在绝缘基材层上预先涂布树脂层后，使铜箔与树脂层的表面粘结，使绝缘基材层和树脂层固化。换言之，事后具备作为带树脂的金属箔的层构成的方案也包含于本发明的一个方案中。
印刷电路板
本发明的带树脂的铜箔优选用于制作印刷电路板。即，根据本发明的优选方式，提供具备上述带树脂的铜箔的印刷电路板、或使用上述带树脂的铜箔而得到的印刷电路板。上述情况下，上述带树脂的铜箔的树脂层被固化。本方式的印刷电路板包含依次层叠有绝缘树脂层和铜层的层构成。另外，对于绝缘树脂层，关于覆铜层叠板如上述。任何情况下，印刷电路板均可以采用公知的层构成。作为关于印刷电路板的具体例，可以举出：使本发明的带树脂的铜箔粘接于预浸料的单面或两面并固化形成层叠体、在此基础上进行电路形成的单面或两面印刷电路板；或将它们多层化的多层印刷电路板等。另外，作为其他具体例，可以举出：在树脂薄膜上形成本发明的带树脂的铜箔并形成电路的柔性印刷电路板、COF、TAB载带、积层多层布线板、在半导体集成电路上交替重复带树脂的铜箔的层叠和电路形成的直接·积层·在线·晶圆(direct buildup on wafer)等。本发明的带树脂的铜箔可以特别优选作为网络设备中的高频数字通信用的印刷电路板用的绝缘层和导体层应用。作为这样的网络设备的例子，可以举出(i)基站内服务器、路由器等、(ii)企业内网络、(iii)高速移动通信的骨干系统等。
实施例
根据以下的例子对本发明进一步进行具体说明。
例1～10和14～19
制备包含树脂组合物的树脂清漆，使用该树脂清漆制造带树脂的铜箔，进行其评价。具体而言，如以下所述。
(1)树脂清漆的制备
首先，作为树脂清漆用原料成分，准备以下所示的树脂成分、咪唑系固化催化剂和无机填料。需要说明的是，无机填料仅在例6中使用。
‐环氧树脂：新日铁住金化学株式会社制、YDCN-704(甲酚酚醛清漆型、环氧当量210g/Eq)
‐聚酰亚胺树脂A：荒川化学工业株式会社制、PIAD-300(末端官能团：羧基、溶剂：环己酮、甲基环己烷和乙二醇二甲基醚的混合液、介电常数(1GHz)：2.70、介质损耗角正切(1GHz)：0.003、软化点：140℃)
‐聚酰亚胺树脂B：株式会社T&K TOKA制、PI-2的溶剂稀释物(末端官能团：羧基、主溶剂：二甲基乙酰胺、介电常数(1GHz)：3.0、介质损耗角正切(1GHz)：0.018、软化点：150℃)
‐芳香族聚酰胺树脂：日本化药株式会社制、BPAM-155(含酚性羟基的橡胶改性型、羟基当量4000g/Eq)
‐咪唑系固化催化剂：四国化成工业株式会社制、2P4MHZ
‐无机填料：球状二氧化硅、Admatechs株式会社制、SC1050-DJA(平均粒径D50＝0.3μm、表面氨基硅烷处理品)
以表1～3所示的配混比(重量比)称量上述树脂清漆用原料成分。另外，将作为有机溶剂的二甲基乙酰胺25重量份和环戊酮75重量份混合，作为混合溶剂。将称量的树脂清漆用原料成分和溶剂投入至烧瓶，以60℃搅拌，使树脂成分溶解于溶剂，将树脂清漆回收。
(2)树脂单独的形态的评价
将上述(1)中得到的树脂清漆涂覆于厚度18μm的电解铜箔的电极面(微观不平度十点高度Rzjis：0.5μm、依据JIS B0601-2001测定)，以使干燥后涂覆厚度成为50μm的厚度。使经涂覆的树脂清漆在烘箱中干燥，形成半固化(B阶)状态。如此，如图1所示那样，制作2张在铜箔12的单面具备树脂层14的带树脂的铜箔10。如图1所示那样，将2张带树脂的铜箔10以树脂层14彼此重叠方式层叠，在加压温度190℃、温度保持时间90分钟、加压压力40kgf/cm2的条件下进行真空加压，使树脂层14成为固化状态。如此固化的树脂层14的厚度为100μm。从加压后的层叠体将铜箔蚀刻并去除，得到由树脂层14单独形成的树脂薄膜。
＜介电特性评价-介质损耗角正切＞
对于上述得到的树脂薄膜，使用网络分析仪(Keysight公司制、PNA-L N5234A)，通过空腔谐振器扰动法，测定1GHz下的介质损耗角正切。该测定依据ASTMD2520(JISC2565)而进行。按照以下基准，以4阶段对所得介质损耗角正切进行评价。
‐评价A：低于0.008(非常良好)
‐评价B：0.008以上且低于0.015(良好)
‐评价C：0.015以上且低于0.020(能允许)
‐评价D：0.020以上(差)
(3)使用树脂层作为底漆层的覆铜层叠板和印刷电路板的评价
(3-1)电解铜箔的制作
分别通过以下方法制作厚度18μm的电解铜箔A～C。
＜电解铜箔A＞
在硫酸铜溶液中，阴极使用钛制的旋转电极(表面粗糙度Ra＝0.20μm)，阳极使用DSA，在溶液温度45℃、电流密度55A/dm2下进行电解，制作原箔。该硫酸铜溶液的组成设为铜浓度80g/L、游离硫酸浓度140g/L、双(3-磺丙基)二硫醚浓度30mg/L、二烯丙基二甲基氯化铵聚合物浓度50mg/L、氯浓度40mg/L。之后，对原箔的电解液面依次进行下述(a)～(c)的表面处理。
(a)锌-镍覆膜形成
‐焦磷酸钾浓度：80g/L
‐锌浓度：0.2g/L、
‐镍浓度：2g/L
‐液温：40℃
‐电流密度：0.5A/dm2
(b)铬酸盐层形成
‐铬酸浓度：1g/L、pH11
‐溶液温度：25℃
‐电流密度：1A/dm2
(c)硅烷层形成
‐硅烷偶联剂：3-氨基丙基三甲氧基硅烷(3g/L水溶液)
‐液处理方法：喷淋处理
对于如此得到的电解铜箔A的表面处理面，微观不平度十点高度Rzjis为0.5μm(依据JIS B0601-2001测定)，无颗粒状突起。
＜电解铜箔B＞
在电解铜箔A的原箔的电解液面侧的表面上形成颗粒状突起，对其颗粒状突起面进行与电解铜箔A同样的表面处理。颗粒突起通过在硫酸铜溶液(铜浓度：13g/L、游离硫酸浓度55g/L、9-苯基吖啶浓度140mg/L、氯浓度35mg/L)中、在溶液温度30℃、电流密度50A/dm2的条件下进行电解而形成。对于该电解铜箔B的表面处理面，微观不平度十点高度Rzjis为0.5μm(依据JIS B0601-2001)，颗粒状突起的基于扫描型电子显微镜图像的平均粒径为100nm、颗粒密度为205个/μm2。
＜电解铜箔C＞
在电解铜箔A的原箔的电解液面侧的表面形成颗粒状突起后，进行与电解铜箔A同样的表面处理。颗粒突起的形成通过以下3阶段的电解处理进行。第1阶段的电解处理在硫酸铜溶液(铜浓度：10.5g/L、游离硫酸浓度：220g/L)中、以溶液温度30℃、电流密度28A/dm2的条件进行。第2阶段的电解处理在硫酸铜溶液(铜浓度：10.5g/L、游离硫酸浓度：220g/L)中、以溶液温度30℃、电流密度16A/dm2的条件进行。第3阶段的电解处理在硫酸铜溶液(铜浓度：70g/L、游离硫酸浓度：220g/L)中、以溶液温度52℃、电流密度21A/dm2的条件进行。对于如此得到的电解铜箔C的表面处理面，微观不平度十点高度Rzjis为1.8μm(依据JISB0601-2001)，颗粒状突起的基于扫描型电子显微镜图像的平均粒径为1.0μm、颗粒密度为1个/μm2。
(3-2)带树脂的铜箔的制作
将上述(1)中得到的树脂清漆涂覆于上述中得到的各电解铜箔的表面处理面，以使干燥后涂覆厚度成为3.0μm的厚度。使经涂覆的树脂清漆在烘箱中干燥形成半固化(B阶)状态，从而制作在铜箔22的单面具备树脂层24的带树脂的铜箔20。
＜耐热性评价-耐热保持时间＞
将预浸料(Panasonic株式会社制MEGTRON-6)2张层叠，得到厚度0.2mm的树脂基材26。如图2所示那样，将2张带树脂的铜箔20的树脂层24侧层叠于树脂基材26的两面，在加压温度190℃、温度保持时间120分钟、加压压力30kgf/cm2的条件下进行真空加压，使树脂层24形成固化状态，得到覆铜层叠板28。如此固化后的树脂层24的厚度为3.0μm。需要说明的是，可以说树脂层24在覆铜层叠板28的制作中作为用于与树脂基材26接合的底漆层发挥功能。对所得覆铜层叠板28进行耐热性评价用的基板制作。具体而言，将覆铜层叠板28切成6.35mm×6.35mm见方。使用热机械分析装置(TMA)，使加热至288℃的石英探针与切出的覆铜层叠板28的表面接触，测定分层(电路剥离、基材剥离)发生为止的时间(分钟)。该测定依据IPC-TM-650(No.2.4.24.1)而进行。结果如表1～3所示。
‐评价AA：120分钟以上(极度良好)
‐评价A：60分钟以上(非常良好)
‐评价B：30分钟以上且低于60分钟(良好)
‐评价C：10分钟以上且低于30分钟(能允许)
‐评价D：低于10分钟(差)
＜铜箔密合性-剥离强度＞
对上述得到的覆铜层叠板28进行剥离强度测定试验用的电路形成。具体而言，使覆铜层叠板28的两面与干膜粘结，形成抗蚀层。然后，在该两面的抗蚀层上，对宽10mm的剥离强度测定试验用的电路进行曝光显影，形成蚀刻图案。之后，以铜蚀刻液进行电路蚀刻，将抗蚀层剥离，得到电路22a。将如此形成的电路22a从树脂层24剥离，测定电路22a和树脂层24间的剥离强度(kgf/cm)。该剥离强度的测定依据JIS C 6481-1996而进行。结果如表1～3所示。
‐评价A：0.60kgf/cm以上(非常良好)
‐评价B：0.40kgf/cm以上且低于0.60kgf/cm(良好)
‐评价C：0.20kgf/cm以上且低于0.40kgf/cm(能允许)
‐评价D：低于0.20kgf/cm(差)
＜输送特性评价＞
使带树脂的铜箔20为最外层，与2张预浸料(Panasonic株式会社制MEGTRON-6、实际厚度68μm)一起层叠，制作厚度0.14mm的两面覆铜层叠板28。之后，对铜箔进行图案蚀刻，从而制作微带电路。选定电路的特性阻抗成为50Ω的图案，测定50GHz下的传输损耗S21(db/cm)。结果如表3所示。
‐评价A：-0.55db/cm以上(良好)
‐评价B：-0.70db/cm以上(能允许)
例11(比较)
使用酚醛树脂(明和化成株式会社制、MEH-7500)代替聚酰亚胺树脂，除此之外，与例10同样地进行树脂清漆的制备和各种评价。结果如表2所示。
例12(比较)
将聚酰亚胺树脂的配混比减少至40重量份(相对于环氧树脂100重量份)，和不添加芳香族聚酰胺树脂，除此之外，与例1同样地进行树脂清漆的制备和各种评价。结果如表2所示。
例13(比较)
不添加聚酰亚胺树脂、和将芳香族聚酰胺树脂的配混比减少至50重量份(相对于环氧树脂100重量份)，除此之外，与例1同样地进行树脂清漆的制备和各种评价。结果如表2所示。
[表1]
Figure BDA0001554831250000181
[表2]
Figure BDA0001554831250000191
[表3]
表3
Figure BDA0001554831250000201

Claims (12)

1.一种带树脂的铜箔，其为在铜箔的至少单面具备树脂层的带树脂的铜箔，所述树脂层包含：
含有环氧树脂、聚酰亚胺树脂和芳香族聚酰胺树脂的树脂混合物；和，
咪唑系固化催化剂，
所述树脂混合物相对于100重量份的所述环氧树脂包含160～340重量份的所述聚酰亚胺树脂、且包含50～200重量份的所述芳香族聚酰胺树脂，
其中，在树脂层已固化的状态下，树脂层在频率1GHz下具有低于0.008的介质损耗角正切。
2.根据权利要求1所述的带树脂的铜箔，其中，所述树脂混合物相对于100重量份的所述环氧树脂包含200～300重量份的所述聚酰亚胺树脂、且包含80～150重量份的所述芳香族聚酰胺树脂。
3.根据权利要求1所述的带树脂的铜箔，其中，所述树脂层还包含无机填料。
4.根据权利要求1所述的带树脂的铜箔，其中，所述聚酰亚胺树脂以聚酰亚胺树脂单独的形态计、在频率1GHz下的介电常数为2.0～3.0、介质损耗角正切为0.001～0.005。
5.根据权利要求3所述的带树脂的铜箔，其中，所述树脂层包含相对于所述环氧树脂、所述聚酰亚胺树脂和所述芳香族聚酰胺树脂的总量100重量份为10～100重量份的所述无机填料。
6.根据权利要求3所述的带树脂的铜箔，其中，所述无机填料为二氧化硅颗粒。
7.根据权利要求1所述的带树脂的铜箔，其中，所述铜箔的树脂层侧的表面的、依据JISB0601-2001测定的微观不平度十点高度Rzjis为2.0μm以下。
8.根据权利要求1所述的带树脂的铜箔，其中，在所述铜箔的树脂层侧的表面具备平均粒径10～300nm的颗粒状突起。
9.根据权利要求1所述的带树脂的铜箔，其中，在所述铜箔的树脂层侧的表面以40～280个/μm2的方式存在有颗粒状突起。
10.根据权利要求1所述的带树脂的铜箔，其中，在所述树脂层固化的状态下，依据JISC6481-1996测定的、所述树脂层和所述铜箔间的剥离强度为0.40kgf/cm以上。
11.一种覆铜层叠板，其具备权利要求1～10中任一项所述的带树脂的铜箔而形成，且所述树脂层已被固化。
12.一种印刷电路板，其具备权利要求1～10中任一项所述的带树脂的铜箔而形成，且所述树脂层已被固化。
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