CN113498255A - 高频电路用表面处理铜箔及高频电路用表面处理铜箔的制造方法 - Google Patents
高频电路用表面处理铜箔及高频电路用表面处理铜箔的制造方法 Download PDFInfo
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- CN113498255A CN113498255A CN202110242800.4A CN202110242800A CN113498255A CN 113498255 A CN113498255 A CN 113498255A CN 202110242800 A CN202110242800 A CN 202110242800A CN 113498255 A CN113498255 A CN 113498255A
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- copper foil
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000011889 copper foil Substances 0.000 title claims abstract description 61
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011651 chromium Substances 0.000 claims abstract description 22
- 239000011701 zinc Substances 0.000 claims abstract description 22
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 20
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 20
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 19
- 239000011733 molybdenum Substances 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 11
- 150000004706 metal oxides Chemical group 0.000 claims abstract description 11
- 238000007747 plating Methods 0.000 claims description 30
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 19
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 13
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 abstract description 12
- 238000005096 rolling process Methods 0.000 abstract description 7
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 9
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000006087 Silane Coupling Agent Substances 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 229920001955 polyphenylene ether Polymers 0.000 description 2
- 229910002059 quaternary alloy Inorganic materials 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 229910002703 Al K Inorganic materials 0.000 description 1
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005246 galvanizing Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 239000011686 zinc sulphate Substances 0.000 description 1
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- H05K9/00—Screening of apparatus or components against electric or magnetic fields
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Abstract
本发明涉及高频电路用表面处理铜箔及高频电路用表面处理铜箔的制造方法。本发明是一种表面处理铜箔，其与高频电路的绝缘基板有优异的粘着性，特别是即使在施加高温轧压加工的热负载下，也能够制造一种抑制起泡产生的覆铜层叠体。更具体而言，本发明是一种高频电路用表面处理铜箔，具有形成于厚度35μm以下的铜箔的耐热处理层，其中，该耐热处理层为包含铬、钼、锌以及镍的四级金属氧化物以及其化合物的膜。
Description
技术领域
本发明关于一种高频电路用的表面处理铜箔，更具体而言，关于一种表面处理铜箔，其与高频电路的绝缘基板有优异的粘着性，并且在高频区域有优异的传输特性。
背景技术
近年来，随着智能型手机以及行动PC以及SNS(也就是，社群网络服务以及影片网站)等信息终端的普及，日益增强对于高速处理大量数据的要求。有鉴于此，对于典型上包括手机的行动通讯装置以及包括使用网络处理资料的电脑的电子装置而言，为了进行大容量信息传输处理的高频率信号受到着目。如今，正迅速发展使用GHz量级的信号的开发，因此需要能够应对如此高速信号的高频电路用印刷线路板。
在构装高频电路用印刷线路板时，考量了高频信号的介电损失，将粘附有铜箔的覆铜层叠体用作绝缘基板。列举几个高频电路用绝缘基板，例如使用热固性聚苯乙醚、改性苯乙醚等树脂。如此具有绝缘材料并结合有铜箔的覆铜层叠体需非常高温的轧压加工，因此，已知在高温轧压时会产生起泡(也就是，溶胀)。此时，为了抑制起泡的发生，基于提高绝缘基板以及铜箔间的密合性的目的，提案有各种表面处理铜箔(例如，专利文献1以及2)。
[现有技术文献]
[专利文献]
[专利文献1]JP 2017-122274 A
[专利文献2]JP 5764700 B
[专利文献3]JP 6294862 B。
如今正积极开发高频电路用绝缘基板，从现在开始，每当开发出新的绝缘基板时，便需要可充分地满足对绝缘基板的粘着性的表面处理铜箔。
发明内容
[发明欲解决的课题]
本发明的目的是提供一种表面处理铜箔，其对高频电路的绝缘基板具有优异的粘着性，尤其是能够制造一种覆铜层叠体，即便施加高温轧压加工的热负载也能其抑制起泡的发生。
[解决课题的手段]
本发明是一种高频电路用表面处理铜箔，是具有形成于厚度35μm以下的铜箔的耐热处理层，其中，该耐热处理层为包括铬、钼、锌以及镍的四级金属氧化物以及其复合物的膜。
本发明的耐热处理层，以金属计，具有镀覆重量为0.1至18mg/m2的铬、10至45mg/m2的钼、30至70mg/m2的锌、以及10至30mg/m2的镍。
本发明的表面处理铜箔的制造方法是：采用四级金属膜用的镀覆浴，以金属计，包括0.2至6.0g/L的铬、1.0至9.0g/L的钼、1.0至8.0g/L的锌以及1.0至7.0g/L的镍；在pH为3至4以及电流密度为0.5至5.0A/dm2的条件下，将厚度35μm以下的铜箔进行表面处理。
[发明效果]
本发明的表面处理铜箔对高频电路用绝缘基板具有优异的粘着性，因而当铜箔被高温轧压加工，特别是在1小时承受290℃的热负载时，可以制造抑制起泡发生受的覆铜层叠体。然后，本发明的表面处理铜箔可通过使用含有特定浓度的铬、钼、锌以及镍的四级金属膜用镀覆浴形成耐热处理层而实现，该耐热处理层为包含四级金属氧化物以及其化合物的膜，据此，可有效率地制造。
附图说明
图1是显示评估起泡发生用的比对照片，以及
图2是显示对本实施例的表面处理铜箔实施XPS分析的结果的作图图表。
具体实施方式
以下，详细地说明本发明。本发明中，于具有厚度35μm以下的铜箔表面形成耐热处理层，该耐热处理层为包含铬、钼、锌以及镍的四级金属氧化物以及其化合物的膜。此时，即便将表面处理铜箔接粘在需要被高温轧压加工的高频电路用绝缘基板，而形成覆铜层叠体，并且在290℃进行1小时的热处理，也不会产生任何起泡或凸起。
本发明的表面处理铜箔中，构成耐热处理层的四级金属膜的镀覆重量，以金属计，较优选为0.1至18mg/m2的铬、10至45mg/m2的钼、30至70mg/m2的锌、以及10至30mg/m2的镍。若镀覆重量小于各元素的下限，则容易发生起泡或凸起，若各镀覆重量超过各元素的上限，则高频特性恶化。
本耐热处理层是由铬、钼、锌以及镍的四级金属氧化物以及其化合物的膜所形成。该四种金属的混合氧化物提高了耐热处理层本身的熔点。进一步，制造四级金属氧化物以及其化合物时，膜容易且强烈地贴合于铬酸盐处理层以及硅烷偶合处理层。
本发明的表面处理铜箔可使用未处理的电解铜箔。使用厚度35μm以下的铜箔。通常，表面粗糙度较优选为Rzjis 1.0μm以下，拉伸强度较优选为300至400N/mm2。
在本发明的表面处理铜箔中，较优选为预先储存铜微粒，进行铜密封镀覆以将铜微粒固定于铜箔表面，并在未处理的电解铜箔的表面，也就是，贴合至绝缘基板的贴合表面形成粗化层。然后，较优选为形成本发明的耐热处理层，其为在粗化层的表面的包含铬、钼、锌以及镍以及其化合物的四级金属氧化物的膜。
形成本发明的表面处理铜箔的耐热处理层时，较优选为使用以金属计，含有0.2至6.0g/L铬、1.0至9.0g/L钼、1.0至8.0g/L锌、以及1.0至7.0g/L镍的四级合金的镀覆用镀覆浴。
镀覆四级合金用镀覆浴，例如，可合理地在镀覆浴中置入CrO3形式的铬、Na2MoO4 .2H2O形式的钼、ZnSO4 .7H2O形式的锌、以及NiSO4 .6H2O形式的镍。进一步，为了增加镀覆浴的导电度，较优选为添加硫酸钠。镀覆浴中化物的含量较优选为30至50ppm。较优选为使用氢氧化钠以及硫酸的稀释溶液作为pH调整剂。较优选为使用氢氧化钠以及硫酸的稀释溶液作为pH调整剂。
镀覆四级合金用镀覆浴的镀覆条件较优选为pH3至4，且电流密度为0.5至5.0A/dm2。
在本发明的表面处理铜箔中，较优选为形成由铬、钼、锌以及镍的四级金属的膜形成的耐热处理层，将膜在空气中放置10至50秒使其氧化，接着，基于防腐蚀的目的，形成铬酸盐处理层。以金属计，铬酸盐处理层中的镀覆重量的铬较优选为3至5mg/m2。
在本发明的表面处理铜箔中，为了改善形成印刷线路板时的抗吸湿劣化，较优选为形成硅烷偶联剂处理层。适合的硅烷偶联剂包括环氧基系、胺系、甲基丙烯酸系、乙烯系、巯基系、以及丙烯酸系，更优选为环氧系、胺系、以及乙烯系。
[实施例]
以下说明实施例。本实施例中使用的铜箔为使用具有厚度为18μm的电解铜箔，该电解铜箔使用钛电解滚筒、阴极以及不可溶阳极、既定浓度的硫酸铜电解液以及既定的电解条件制造的电解铜箔。电解铜箔的M表面侧的表面粗糙度为1.0μm Rzjis，S表面侧的为1.0μm Rzjis。术语M表面为在电解滚筒的非滚筒表面侧的表面，而S表面为在电解滚筒的滚筒表面侧的表面。须注意的是，该电解铜箔也使用于下述比较例。
以下述条件在电解铜箔的M表面形成粗化层。
铜微粒处理：
铜密封镀覆：
形成粗化层后，使用下述条件形成耐热处理层(其为铬、钼、锌及镍的四级金属氧化物、以及其化合物的膜)。对该耐热处理层施以下述四级金属膜镀覆，在空气中置放30秒而形成。
四级金属膜的镀覆条件：
镀覆浴组成
形成耐热处理层后，检测耐热处理层中各金属的镀覆重量并列示如下。
镀覆重量：
形成耐热处理层后，使用下述条件形成铬酸盐处理层。
铬酸盐处理条件：
形成铬酸盐处理层后，使用下述条件形成硅烷偶联剂处理层，并制造出本实施例的表面处理铜箔。
市面贩卖胺系硅烷偶联剂
干燥条件85℃×10秒
比较例
制备依次在电解铜箔的M表面形成有粗化层、锌镀覆层、铬酸盐处理层、以及硅烷偶联剂处理层的表面处理铜箔作为比较例。除了镀锌层以外的处理条件与上述实施例相同。镀锌层以下述条件处理。
镀锌条件：
镀覆浴组成
ZnSO4·7H2O Zn 0.8g/L(以金属计)
电流密度 2A/dm2
镀覆时间 2秒
检测该比较例中的表面处理铜箔各元素的镀覆重量，并列示如下。
镀覆重量：
Zn 20mg/m2
Cr 4mg/m2
<起泡发生评估>
使用两种高频电路用预浸物评估实施例以及比较例的表面处理铜箔在高温热处理的起泡发生。使用Panasonic制MEGTRON 6作为预浸物A，以及使用韩国斗山(Doosan)电子材料公司制DS-7409-DV作为预浸物B。
这些预浸物的轧压条件：
将上述轧压条件下取得的覆铜层叠体加工成5cm×5cm的大小，接着在烘箱进行1小时、290℃的热处理。为了参考的目的，图1显示起泡发生评估用的比对照片(预浸物A)。图1中，左侧是没有起泡的实施例，右侧是发生起泡的比较例。
实施例的表面处理铜箔中，在两种预浸物没有观察到起泡发生。另一方面，比较例的表面处理铜箔中，在两种预浸物观察到起泡的发生。由该结果可知，使用将表面处理铜箔与高频电路用的预浸物结合成的覆铜层叠体，该表面处理铜箔是在铜箔的表面上形成有由铬、钼、锌和镍的四级金属氧化物及其化合物所组成的耐热处理层的表面处理铜箔，即使对该覆铜层叠体施加1小时、290℃高温度热负载，也成功地抑制了气泡的形成。
接下来，说明对上述实施例的表面处理的铜箔进行X射线光电子能谱分析的结果。作为分析对象的是以与上述实施例相同的条件形成铬酸盐处理层，但是未进行硅烷偶合处理的表面处理铜箔。XPS分析仪使用PHI Quantum 2000(ULVAC-PHI公司制)。XPS分析仪具有光束直径为10至200μm的Al-Kα的X射线源，然后使用加速至2KeV(对应于10nm/min SiO2的溅射速率)的Ar离子对表面处理铜箔的表面进行溅射蚀刻，以在深度方向进行分析。结果显示于图2。
图2绘制了由XPS分析仪获得的在深度方向上各元素的原子浓度。水平轴表示深度，水平轴值对应于用加速至2KeV的Ar离子溅射的氧化硅(SiO2)的深度。从图2的结果确认混合了铬、钼、锌以及镍四种金属。并证实在膜的深度方向上存在少量的Cr。通过XPS分析获得的与氧的结合能峰更进一步发现，由于四种金属皆放置于空气中，因此以氧化物形式混合。
从XPS分析的结果推测，本实施例的表面处理铜箔由于形成了耐热处理层，该耐热处理层是由铬、钼、锌和镍的四元金属氧化物及其化合物构成的膜，并在膜中混合多种氧化物，因而实现了对高温热处理的适应性等特性，因此，该表面处理铜箔熔点提高，并有助于进行耐热处理后形成的铬酸盐处理层和硅烷偶联剂处理层牢固地结合。
Claims (3)
1.一种高频电路用表面处理铜箔，具有形成于厚度35μm以下的铜箔的耐热处理层，其中，
该耐热处理层为包括铬、钼、锌以及镍的四级金属氧化物以及其化合物的膜。
2.根据权利要求1所述的高频电路用表面处理铜箔，其中，该耐热处理层具有以金属计，镀覆重量为0.1至18mg/m2的铬、10至45mg/m2的钼、30至70mg/m2的锌、以及10至30mg/m2的镍。
3.一种高频电路用表面处理铜箔的制造方法，包括下列步骤：
采用四级金属膜的镀覆浴，以金属计，包括0.2至6.0g/L的铬、1.0至9.0g/L的钼、1.0至8.0g/L的锌、以及1.0至7.0g/L的镍；
pH为3至4以及电流密度为0.5至5.0A/dm2的条件下对厚度35μm以下的铜箔进行表面处理；以及接着
将该表面处理铜箔在空气中置放10至50秒。
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| KR20210117916A (ko) | 2021-09-29 |
| EP3882378A1 (en) | 2021-09-22 |
| JP7194716B2 (ja) | 2022-12-22 |
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