CN1993501A - 复合铜箔及其制造方法 - Google Patents

复合铜箔及其制造方法 Download PDF

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CN1993501A
CN1993501A CNA2005800257753A CN200580025775A CN1993501A CN 1993501 A CN1993501 A CN 1993501A CN A2005800257753 A CNA2005800257753 A CN A2005800257753A CN 200580025775 A CN200580025775 A CN 200580025775A CN 1993501 A CN1993501 A CN 1993501A
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copper foil
resin
molybdenum
metal oxide
mainly
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CN1993501B (zh
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佐藤佑志
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NIPPON ELECTROLYTIC CO Ltd
Nippon Denkai Co Ltd
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Abstract

本发明涉及由支撑体金属层、剥离层和薄铜层这样的三层构成的复合铜箔，其中，所述剥离层的一个表面主要由钨合金或钼合金构成，另一个表面主要由含有钨的金属氧化物或含有钼的金属氧化物构成。该复合铜箔在高温下进行加热加工时，不会发生支撑体金属层所不希望的膨胀、剥离、脱落等现象，并且在加热加工后容易从薄铜层上剥离掉支撑体金属层。

Description

复合铜箔及其制造方法
技术领域
本发明涉及印刷电路板的制造中使用的复合铜箔，尤其涉及支撑体金属层与薄铜层之间的剥离强度的稳定性优异的复合铜箔。
背景技术
在超高密度印刷电路板制造工序中使用由支撑体金属层、剥离层和薄铜层构成的带有支撑体的铜箔。使薄铜层面向树脂基材，将带有支撑体的铜箔和树脂基材层压成形，然后剥离支撑体金属层，对薄铜层进行蚀刻加工，形成电路。与使用无支撑体金属层的普通铜箔的情况相比，由于能够将薄铜层的厚度减小，所以有利于形成微细电路。
作为剥离层，通常使用的是含有苯并三唑类有机化合物或铬氧化物等无机化合物的层，但在高温下铜向剥离层内扩散，因而难以从薄铜层剥离掉支撑体金属层。为此，有人提出了在支撑体金属层或薄铜层中的任一方的、面向剥离层的表面上形成防止铜扩散的层的技术方案(例如参见专利文献1)。
通过防止铜的扩散，可以抑制高温下的剥离强度提高，但是，随着层的结构变得复杂，由于热膨胀系数的差别或晶体结构的变化等而引起界面破坏，导致支撑体金属层从薄铜层上自行剥离，从而引起薄铜层表面被高温空气氧化而劣化、切断加工时发生损伤等，对作业性和镀铜叠层板的品质带来不良影响。
专利文献1：特开2002-292788号公报
发明内容
发明要解决的技术问题
本发明的目的在于，提供支撑体金属层与薄铜箔层之间的剥离强度的稳定性提高的复合铜箔。
解决任务的技术方案
本发明是由支撑体金属层、在支撑体金属层上的剥离层以及在剥离层上的薄铜层这样的三层构成的复合铜箔，其最主要的特征在于，剥离层的一个表面主要由钨合金或钼合金构成，另一个表面主要由含有钨的金属氧化物或含有钼的金属氧化物构成。例如，剥离层的主要由钨合金或钼合金构成的表面的氧/金属比，以原子数比计优选为0.01～0.99，更优选为0.10～0.60；主要由含有钨的金属氧化物或含有钼的金属氧化物构成的表面的氧/金属比，以原子数比计优选为1.0～9.0，更优选为1.5～4.0。
主要由含有钨的金属氧化物或含有钼的金属氧化物构成的表面，以可剥离的强度将薄铜层和支撑体金属层结合，另一方面，主要由钨合金或钼合金构成的表面，防止铜原子在薄铜层和支撑体金属层之间相互热扩散到剥离层内，增大薄铜层与支撑体金属层的结合力而导致无法剥离。优选的是，剥离层内不存在明显的界面，是连续地变化，即其组成呈梯度变化。这样，热膨胀系数的差异或晶体结构的变化所引起的应力减小，不会发生自行剥离的现象。作为这样的剥离层，例如可以举出下面所述的剥离层：由钨合金和含有钨的金属氧化物构成，钨合金的含有率，从主要由钨合金构成的表面向主要由含有钨的金属氧化物构成的表面连续地减少，而含有钨的金属氧化物的含有率，从主要由含有钨的金属氧化物构成的表面向主要由钨合金构成的表面连续地减少。作为另外一例子，可以举出下面所述的剥离层：由钼合金和含有钼的金属氧化物构成，钼合金的含有率从主要由钼合金构成的表面向主要由含有钼的金属氧化物构成的表面连续地减少，而含有钼的金属氧化物的含有率从主要由含有钼的金属氧化物构成的表面向主要由钼合金构成的表面连续地减少。具有这种剥离层的复合铜箔，例如可以采用本发明的方法按以下所述制造，即，在支撑体金属层上通过电镀依次形成剥离层和薄铜层的复合铜箔的制造方法中，作为用于形成剥离层的电解液，使用含有下列物质的电解液：钨酸化合物或钼酸化合物、含有铁族元素的化合物、以及柠檬酸。
发明的效果
本发明的复合铜箔，在高温下剥离强度提高较小，并且不会发生支撑体金属层从薄铜层上自行剥离，对作业性和镀铜叠层板的品质带来不良影响等问题，因此有利于制造高密度印刷电路板。
具体实施方式
在本发明中使用的支撑体金属层的材质、厚度没有特别限制，但是从生产成本和制造工艺、机械性能及化学性能的角度考虑，优先选择厚度8μm～35μm的铜箔。关于表面粗糙度，当需要薄铜层与树脂基材之间的粘接强度时，支撑体金属层的表面粗糙度大一些为好，另一方面，当需要形成微细电路时，希望表面粗糙度小一些。另外，当薄铜层较薄时，也是表面粗糙度小一些为好。
在形成剥离层之前，最好是通过适当的前处理净化支撑体金属层的表面。除了通常的酸洗处理以外，也可以进行碱脱脂或电解清洗。
本发明的剥离层，可以使用含有下列物质的电解液：钨酸化合物或钼酸化合物、含铁族元素的化合物以及柠檬酸，以支撑体金属层作为阴极进行电镀而形成。作为铁族元素，优选使用镍。出于调整阻抗值的目的，也可以在电解液中添加硫酸钠等无机盐。钨酸化合物或钼酸化合物的添加量，换算成各金属，通常为0.1～10g/l，优选0.5～2g/l。至于含有铁族元素的化合物，换算成金属，通常为0.6～60g/l，优选3～12g/l。柠檬酸的浓度，相对于除了钠离子以外的金属种类，换算成摩尔数，即相对于钨酸化合物和含有铁族元素的化合物的合计摩尔数，或相对于钼酸化合物和含有铁族元素的化合物的合计摩尔数，通常为0.2～5倍，优选0.5～2倍。作为钨酸化合物，例如可以使用钨酸钠二水合物等钨酸盐或其水合物。作为钼酸化合物，例如可以使用钼酸钠二水合物等钼酸盐或其水合物。作为含有铁族元素的化合物，例如可以使用硫酸镍六水合物等镍盐或其水合物。作为柠檬酸源，例如可以使用柠檬酸钠二水合物等柠檬酸盐或其水合物。电解液的溶剂一般是水。电解液温度通常为5～70℃，优选为10～50℃。电流密度通常为0.2～10A/dm2，优选为0.5～5A/dm2。另外，pH通常为2～8，优选为4～7的范围。按上述条件进行电镀时，首先，主要析出金属，随着电镀的进行，主要析出氧化物。以氧化物为主体的表面发挥剥离功能，另一方面，以金属为主体的表面则抑制因铜原子热扩散引起的层结构一体化的现象。剥离层的厚度和组成，通过电解液的组成和电解条件来控制。通常，剥离层的厚度为0.005～0.5μm。
剥离层可以一次形成，也可以反复进行多次电镀来形成。可以用一个槽进行几次电镀，也可以用几个槽进行电镀。当多次进行剥离层的形成时，剥离强度将更加稳定。
对于薄铜层的形成没有特别的限制，但使用以焦磷酸铜为主体的电解液时，可以形成致密的铜镀层，因此针孔会减少。另外，当使用以硫酸铜为主体的电解液时，可以进行快速电镀，可以高效率地形成薄铜层。通过组合使用这两种电镀方法，可以高效率地形成具有期望厚度并且针孔少的薄铜层。薄铜层的厚度可以根据用途任意设定。为了形成微细电路，通常优选为0.1～10μm，但也可以更厚。用该方法制造本发明的复合铜箔时，由于与薄铜层相接的剥离层的表面以氧化物为主体，因此剥离强度小，剥离层将残留在支撑体金属层一侧。
对于薄铜层的表面，可以用公知的方法进行粗糙化处理，以提高与树脂基材的粘接性，另外，也可以采用铬酸盐处理等公知的方法进行防锈处理。此外，还可以根据需要，用硅烷偶联剂等进行粘接增强处理，以提高与树脂基材的粘接性。
在采用上述本发明的制造方法制造的复合铜箔中，钨合金是含有钨和铁族元素的合金，钼合金是含有钼和铁族元素的合金，含有钨的金属氧化物包含钨的氧化物和铁族元素的氧化物，含有钼的金属氧化物包含钼的氧化物和铁族元素的氧化物。
将本发明的复合铜箔和树脂基材层压成形，层压成形时使复合铜箔的薄铜层一侧面向树脂基材，形成镀铜膜叠层板，可以用于制造印刷电路板。另外，也可以在本发明的复合铜箔的薄铜层上涂布树脂基材溶液，进行加热，制成镀铜膜树脂薄膜，用于制造印刷电路板。在制造印刷电路板时，可以从镀铜膜叠层板或镀铜膜树脂薄膜上剥离支撑体金属层和剥离层，然后对薄铜层进行蚀刻加工形成电路，得到印刷电路板。作为树脂基材，例如可以使用至少含有聚酰亚胺系树脂、环氧系树脂、马来酰亚胺系树脂、三嗪系树脂、聚苯醚系树脂、聚丁二烯系树脂中的一种的树脂基材。作为聚酰亚胺系树脂，例如可以举出聚酰亚胺、聚酰胺酰亚胺、或它们的前体，例如聚酰胺酸等。制造镀铜膜叠层板时，通常是将这些树脂中的至少一种浸渍到玻璃布等而成的预浸料用作为树脂基材。在制造镀铜膜树脂薄膜时，通常使用含有上述树脂中的至少一种的树脂基材溶液。
实施例
支撑体金属层使用厚度18μm的电解铜箔。在硫酸中对该铜箔的表面进行阴极处理，净化其表面。接着，以该净化后的铜箔作为阴极(阳极：Ti基体氧化铟涂层电极)，按照表1记载的条件(电解液的pH：6.0，液温：30℃)在光泽面上形成剥离层1。其中，在形成剥离层1时，实施例2是按照表1记载的条件对铜箔进行20秒阴极处理后，停止电流，  间隔10秒钟后按照相同条件再次进行20秒阴极处理。
形成剥离层1后，依次使用焦磷酸铜电镀液和硫酸铜电镀液，形成3.9μm的薄铜层。形成薄铜层时的电镀条件如下。
(1)焦磷酸铜电镀
电解液组成：焦磷酸铜80g/l、焦磷酸钙320g/l、氨水2ml/l
pH：8.5
电流密度：2.0A/dm2
时间：20秒
温度：40℃
(2)硫酸铜电镀
电解液组成：硫酸铜200g/l，硫酸100g/l。
电流密度：3.5A/dm2
时间：300秒
温度：40℃
接着，按照公知的方法进行相当于厚度1μm的微细粗糙化处理，然后进行铬酸盐处理和硅烷偶联剂处理，制成复合铜箔A～D。其中，为了进行比较，依次形成剥离层2和剥离层3来代替剥离层1，除此之外与复合铜箔A～D同样操作，制成复合铜箔E。
从复合铜箔A～E上剥离薄铜层，一面用氩离子对支撑体金属层上的剥离层的表面在深度方向上进行腐蚀，一面进行XPS分析。结果一并示于表中。其中，氧原子与金属原子之比是将铜金属除外后计算出的。复合铜箔A～D都是在腐蚀初期检测出较多的氧，随着腐蚀的进行，氧逐渐减少。由此可知，在腐蚀初期观察到的面、即与薄铜层相接触一侧的表面上，钼和钨主要是以氧化物存在，而在与支撑体金属层相接触的面上是以金属存在。
从未加热状态的复合铜箔A～E上剥离薄铜层，按照JIS C6481测定支撑体金属层与薄铜层之间的剥离强度，结果示于表1中。在玻璃布基材环氧树脂预浸料(相当于FR-5)上，使薄铜层面向基材来叠层复合铜箔A～E，在260℃下以30kN/m2压制60分钟，形成镀铜膜叠层板。另外，在复合铜箔A～E上涂布市售的聚酰胺酸溶液，在120℃下干燥100分钟，接着在200℃下干燥20分钟，然后，在450℃下加热10分钟进行酰亚胺化处理，制成镀铜膜聚酰亚胺树脂薄膜。按照JIS C6481测定支撑体金属层与薄铜层之间的剥离强度，结果示于表1中。在表1中，“260℃/60分钟”表示上述镀铜膜叠层板制造中压制时的加热条件，“450℃/10分钟”表示上述镀铜膜聚酰亚胺树脂薄膜制造中酰亚胺化处理时的加热条件。
使用复合铜箔E的镀铜聚酰亚胺树脂薄膜，支撑体金属层自行剥离，薄铜层的表面氧化变色。另一方面，使用复合铜箔A～D的镀铜聚酰亚胺树脂薄膜，具有20～280kN/m的剥离强度，剥离后的薄铜层表面呈现通常的金属光泽和金属铜特有的色相。
表1
项目   实施例1   实施例2   实施例3   实施例4   比较例1
  铜箔A   铜箔B   铜箔C   铜箔D   铜箔E
剥离层1 镀液组成(g/l)   NiSO4·6H2O   30   30   30   30   -
  Na2MoO4·2H2O   3   3   3   -   -
  Na2WO4·2H2O   -   -   -   3   -
  Na3C6H5O7·2H2O   30   30   30   30   -
  Na2SO4   30   30   30   30   -
       电流密度(A/dm2)   3   3   3   3   -
       电解时间(秒)   40   20+20   20   20   -
剥离层2 镀液组成(g/l)   NiSO4·6H2O   -   -   -   -   300
  H3BO3   -   -   -   -   40
  H3PO3   -   -   -   -   0.5
  MgSO4·6H2O   -   -   -   -   80
  糖精钠   -   -   -   -   2
       电流密度(A/dm2)   -   -   -   -   5.4
       电解时间(秒)   -   -   -   -   20
剥离层3 镀液组成(g/l)   Na2MoO4·2H2O   2
  Na2Cr2O7·2H2O   -   -   -   -   2
       电流密度(A/dm2)   -   -   -   -   5.4
       电解时间(秒)   -   -   -   -   20
剥离强度(N/m)   未加热   20   20   20   10   20
  260℃/60分钟   20   20   20   10   20
  450℃/10分钟   90   20   160   280   自行剥离
剥离层中的氧/金属(原子数比)   腐蚀：0秒   3.6   3.3   3.3   3.4   5.8
  腐蚀：30秒   1.6   0.9   1.2   1.2   0.1
  腐蚀：60秒   0.9   0.8   0.7   0.8   0.1
  腐蚀：120秒   0.6   0.6   0.6   0.6   0.0
  腐蚀：240秒   0.5   0.5   0.5   0.5   0.0
产业上的应用可能性
本发明的复合铜箔，在高温下剥离强度提高很少，并且，不会发生支撑体金属层和薄铜层在加工过程中自行剥离，对作业性和镀铜膜叠层板的品质带来不良影响等问题，因此适于制造高密度印刷电路板。

Claims (13)

1.复合铜箔，由支撑体金属层、在支撑体金属层上的剥离层和在剥离层上的薄铜层这样的三层构成，其特征在于，剥离层的一个表面主要由钨合金或钼合金构成，另一个表面主要由含有钨的金属氧化物或含有钼的金属氧化物构成。
2.根据权利要求1所述的复合铜箔，其中，支撑体金属层是铜箔。
3.根据权利要求1所述的复合铜箔，其中，钨合金是含有钨和铁族元素的合金，钼合金是含有钼和铁族元素的合金，含有钨的金属氧化物包含钨的氧化物和铁族元素的氧化物，含有钼的金属氧化物包含钼的氧化物和铁族元素的氧化物。
4.根据权利要求3所述的复合铜箔，其中，铁族元素是镍。
5.根据权利要求1所述的复合铜箔，其中，主要由钨合金或钼合金构成的表面是与支撑体金属层相接触的表面，主要由含有钨的金属氧化物或含有钼的金属氧化物构成的表面是与薄铜层相接触的表面。
6.根据权利要求1所述的复合铜箔，其中，剥离层由钨合金和含有钨的金属氧化物构成，钨合金的含有率从主要由钨合金构成的表面向主要由含有钨的金属氧化物构成的表面连续地减少，而含有钨的金属氧化物的含有率从主要由含有钨的金属氧化物构成的表面向主要由钨合金构成的表面连续地减少。
7.根据权利要求1所述的复合铜箔，其中，剥离层由钼合金和含有钼的金属氧化物构成，钼合金的含有率从主要由钼合金构成的表面向主要由含有钼的金属氧化物构成的表面连续地减少，而含有钼的金属氧化物的含有率从主要由含有钼的金属氧化物构成的表面向主要由钼合金构成的表面连续地减少。
8.权利要求1所述的复合铜箔的制造方法，其特征在于，通过电镀在支撑体金属层上依次形成剥离层和薄铜层制成复合铜箔，其中，作为用于形成剥离层的电解液，使用含有下列物质的电解液：钨酸化合物或钼酸化合物、含有铁族元素的化合物、以及柠檬酸。
9.根据权利要求8所述的复合铜箔的制造方法，其中，支撑体金属层是铜箔，铁族元素是镍。
10.印刷电路板的制造方法，其特征在于，使用将权利要求1所述的复合铜箔和树脂基材层压成形而制成的镀铜膜叠层板，在上述层压成形时使复合铜箔的薄铜层一侧面向树脂基材。
11.根据权利要求10所述的印刷电路板的制造方法，其特征在于，树脂基材至少包含聚酰亚胺系树脂、环氧系树脂、马来酰亚胺系树脂、三嗪系树脂、聚苯醚系树脂、聚丁二烯系树脂中的一种。
12.印刷电路板的制造方法，其特征在于，使用在权利要求1所述的复合铜箔的薄铜层上涂布树脂基材溶液、进行加热而得到的镀铜膜树脂薄膜。
13.根据权利要求12所述的印刷电路板的制造方法，其特征在于，树脂基材至少包含聚酰亚胺系树脂、环氧系树脂、马来酰亚胺系树脂、三嗪系树脂、聚苯醚系树脂、聚丁二烯系树脂中的一种。
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