CN104854968A - 提高聚合物膜和金属层之间的粘附性的方法 - Google Patents
提高聚合物膜和金属层之间的粘附性的方法 Download PDFInfo
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Abstract
本发明涉及提高在聚合物基板和形成在所述基板上的金属层之间的粘附性的方法。根据本发明的方法包括以下步骤:(a)对聚合物膜执行表面改性处理;(b)在经表面改性处理的聚合物膜上形成金属层;以及(c)对所述金属层执行从老化处理和/或电流施加处理中选择的至少一种。
Description
技术领域
本发明涉及提高聚合物膜和形成在聚合物膜上的金属层之间的粘附性的方法,更特别地,涉及通过在聚合物膜上形成金属层并且随后单独地或组合地执行老化处理、电流施加、或特定气氛下的老化处理,能够得到比传统方法有所提高的粘附性的方法。
背景技术
当前,作为用于在用作柔性印刷电路板和封装电介质的聚合物膜材料上形成金属电路图案的技术,通常广泛使用的是制备金属电路图案的方法,在该方法中,使用光致抗蚀剂工艺在上面堆叠或沉积有薄铜箔的聚合物的表面上形成具有预定形状的电路图案,并且然后铜被蚀刻。
作为在聚合物材料上形成金属层的方法,使用利用等离子体离子对聚合物膜执行表面改性处理以提高粘附性并且然后通过使用诸如溅射或金属沉积的干表面处理技术在膜的表面上形成导电金属粘附层的方法、根据产品状况使用电镀技术形成金属涂层的方法、将铜膜直接粘结到聚合物膜表面的层合方法或浇铸方法。
然而,这些方法的限制在于,没有促成形成均匀的金属层或者需要高工艺成本。
为了应对这些限制,已经积极进行了通过湿处理对聚合物膜进行金属化处理的研究和开发。然而,由于物理性质(例如,金属层和聚合物膜之间的低粘附性)没有满足市场要求,因此没有实现商业应用。
然而,由于湿处理可具有例如工艺和设备简单、成本低、产量高和形成均匀金属涂层的优点,因此如果解决了市场的要求(例如,金属和聚合物之间的粘附性提高),则湿处理是潜力大的处理。
发明内容
技术问题
本发明的目的是提供当通过湿处理在聚合物膜上形成金属层时通过简单工艺显著提高聚合物膜和聚合物膜上形成的金属层之间的粘附性的方法。
本发明的目的也是提供通过以上方法提高与金属层的粘附性的聚合物膜。
技术方案
根据本发明的第一方面,提供了一种在聚合物膜上形成金属层的方法,所述方法包括以下步骤:(a)对聚合物膜执行表面改性处理;(b)在经表面改性处理的聚合物膜上形成金属层;(c)对所述金属层执行从老化处理或电流施加处理中选择的至少一种。
根据本发明的第二方面,提供了一种在聚合物膜上形成金属层的方法,所述方法包括以下步骤:(a)对聚合物膜执行表面改性处理;(b)在经表面改性处理的聚合物膜上形成金属种层;(c)对所述金属种层执行从老化处理或电流施加处理中选择的至少一种;(d)在所述金属种层上形成金属层。
根据本发明的第一方面或第二方面,所述聚合物膜可以是由从热固性树脂、热塑性树脂、聚酯树脂、聚酰亚胺树脂、缩聚物、或其两种或更多种的混合物中选择的至少一种形成的单层膜或多层膜。
根据本发明的第一方面或第二方面,所述金属层可由从铜(Cu)、镍(Ni)、钴(Co)、钛(Ti)、铝(Al)、铬(Cr)、钼(Mo)或其合金中选择的至少一种形成。
根据本发明的第一方面或第二方面,可在形成所述金属层或所述金属种层之前在所述聚合物膜上形成粘结层。
根据本发明的第一方面或第二方面,可执行所述老化处理达12小时或更长时间,优选地,24小时或更长时间,更优选地,48小时或更长时间。
根据本发明的第一方面或第二方面,可在0℃至100℃的温度范围内,在具有10%或更大,优选地,50%或更大,更优选地,80%或更大的相对湿度的气氛中,执行所述老化处理。
根据本发明的第一方面或第二方面,可通过向所述金属层的表面施加0.005mA/cm2至1A/cm2的电流密度来执行电流施加处理。
根据本发明的第一方面或第二方面,可通过从镀方法或物理汽相沉积(PVD)方法中选择的方法形成所述金属层。
根据本发明的第二方面,可通过从无电镀方法、无电镀加电镀方法、或PVD方法中选择的方法形成所述金属种层。
根据本发明的第一方面或第二方面,所述表面改性处理可包括从浸入酸或碱溶液中、紫外线(UV)处理或等离子体处理中选择的至少一种。
有益效果
当根据本发明对金属种层或金属层单独地或组合地执行老化处理、电流施加处理和在特定气氛中的老化处理时,形成在聚合物膜上的金属层的粘附性大大提高。
另外,由于通过对金属种层和/或金属层执行的诸如老化处理、短时间电流施加或在特定气氛中的老化处理的简单过程,执行根据本发明的提高粘附性的方法,因此可以以低成本提高粘附性。
此外,根据本发明的提高粘附性的方法不限于湿处理,但还可用于干处理。
附图说明
图1示出测量根据老化处理的粘附性变化的结果;
图2示出测量根据电流施加处理的粘附性变化的结果;
图3示出测量气氛中根据老化处理的粘附性变化的结果;
图4示出测量在气氛中进行老化处理之后由于留存而导致的粘附性变化的结果。
具体实施方式
下文中,根据具体示例,将更详细地描述本发明。然而,下面的示例只是被提供用于更清楚地理解本发明,并不限制本发明的范围。
本发明的发明人进行了研究,以提高当在聚合物膜上形成金属层时,特别地,当通过能够以低成本形成金属层的湿处理形成金属层时,聚合物膜和金属层之间的粘附性。
结果,本发明的发明人认识到,如果在聚合物膜上形成金属层(金属种层)并且随后对金属层执行预定处理,例如,老化处理(特别地,水环境或水下环境中的老化)或电流施加处理,则聚合物和金属层之间的粘附性显著提高。
根据本发明的提高聚合物和金属层之间的粘附性的方法包括:(a)对聚合物膜执行表面改性处理;(b)在经过表面改性处理的聚合物膜上形成金属层;(c)对金属层执行从老化处理或电流施加处理中选择的至少一种。
在这种情况下,在形成金属层的过程中,在形成金属种层之后形成金属层的情况下,例如,在通过无电镀在聚合物膜上形成种层并且随后通过电镀形成金属层的情况下,对金属种层执行从老化处理或电流施加处理中选择的至少一种,然后可形成金属层。
另外,在形成金属层或金属种层之前,可在聚合物膜上形成粘结层(tiecoat layer)。
聚合物膜可以是由从热固性树脂、热塑性树脂、聚酯树脂、聚酰亚胺树脂、缩聚物、或其两种或更多种的混合物中选择的至少一种形成的单层或多层膜。
另外,可使用苯酚树脂、苯酚醛树脂、呋喃树脂、氨基塑料树脂、醇酸树脂、烯丙基树脂、环氧树脂、环氧预浸料、聚氨酯树脂、热固性聚酯树脂或硅树脂作为热固性树脂。
此外,可使用聚乙烯、聚丙烯、乙烯/乙烯基共聚物或乙烯丙烯酸共聚物作为热塑性树脂。
另外,可使用由二价脂族和芳香羧酸和二醇或三醇制成的树脂作为聚酯树脂。
可使用聚酰胺、聚醚酰亚胺、聚砜、聚醚砜、聚苯并咪唑和芳族聚砜作为缩聚物。
作为金属层和金属种层,可使用诸如铜(Cu)、镍(Ni)或其合金,但本发明不限于此。
另外,相对于金属种层,由于将形成在金属种层上的金属层在金属种层厚度过小时会难以形成为均匀厚度,因此金属种层可形成为至少100nm或更大的厚度。
粘结层可由Ni、铬(Cr)、钼(Mo)、钴(Co)或其合金形成。
粘结层可形成为1nm至40nm的厚度。
这样的原因在于,当厚度小于1nm时,粘附性的提高可能不充分,并且当厚度大于40nm时,会无法促成后续的蚀刻过程。
可执行各种表面处理(诸如,根据聚合物类型浸入酸或碱溶液中、紫外线(UV)处理或等离子体处理)作为表面改性处理。
表面改性处理可包括在执行主要表面处理之后执行催化剂和活化处理。
在经表面改性处理的聚合物膜上形成金属层或金属种层的过程中,可使用已知的膜形成方法(诸如,在无电镀、溅射、真空沉积和离子镀之后执行电镀的方法)。
对金属层或金属种层进行的老化处理代表其中形成金属层和金属种层并且随后留存至少12小时,优选地24小时,最优选地48小时而不对金属层或金属种层执行后续处理的处理。
在这种情况下,空气气氛可以用作老化处理的气氛。然而,例如,老化处理可与所谓的“气氛处理”并行执行,“气氛处理”是在富含水状态而非正常空气气氛中执行的。
在进行气氛处理期间,0℃至100℃的温度范围内的相对湿度必须是至少10%或更大,可以是50%或更大,并且例如,可以是80%或更大。
对金属层或金属种层的电流施加处理是以下过程:0.05mA/cm2至1A/cm2的电流密度被瞬时施加到金属层或金属种层的表面,特别地,在通过作为湿处理的无电镀形成金属种层并且接着通过进行0.1秒至1小时的电镀在金属种层上形成金属层的情况下,被瞬时施加到金属种层。
通过以上过程,可显著增加金属层和聚合物之间的粘附性。
可执行电流施加处理达最少0.1秒或更长时间,并且由于即使执行1小时或更长时间的处理,以上效果也可能是饱和的,因此不期望执行1小时或更长时间的电流施加处理。
依据可通过相比于老化处理的短时间处理得到提高的粘附性的事实,电流施加处理相比于老化处理可以是更有利的方法。
[实例1]
在通过无电镀和电镀在聚合物膜上形成镀铜层的过程中,本发明的实例1对应于执行其中在形成无电镀层或形成电镀层之后在气氛中保持预定时间的老化处理。
具体地,使用得自美国杜邦公司(DuPont)的25μm厚的聚酰亚胺Kapton膜作为聚合物膜。
首先,按表面改性处理、冲洗处理、中性化处理、冲洗处理、催化剂处理、冲洗处理和活化处理的顺序,执行对聚酰亚胺膜的预处理。
通过在50℃下将聚酰亚胺膜浸入1M KOH和0.9M乙二胺(EDA)的混合溶液5分钟的方法,执行表面改性处理,并且通过将聚酰亚胺膜浸入0.2M HCL溶液5分钟的方法,执行中性化处理。另外,在室温下,分别使用SnCl2和PdCl2执行催化剂或活化处理4分钟和2分钟。
使用无电镀镀铜溶液,在12.5的PH值下将经受预处理的聚酰亚胺膜镀10分钟,在无电镀镀铜溶液中,在硫酸铜溶液(10g/L)中添加作为还原剂的甲醛(20mL/L)、作为络合剂的罗谢尔盐(50g/L)和作为PH调节剂的氢氧化钠。由此形成的无电镀铜层的厚度是大约100nm。
随后,对无电镀镀铜层执行镀铜,以形成具有大约10μm厚度的镀层。
经受无电镀镀铜的样本立即被电镀,然后,将上面形成有电镀镀铜层的样本分别留存在空气中达0小时、12小时、24小时和48小时。然后,评价电镀铜层的粘附性。
另外,将无电镀镀铜层分别保持在气氛中达0小时、12小时、24小时和48小时并且立即形成电镀镀铜层。然后,也评价电镀镀铜层的粘附性。
也就是说,评价其中连续执行无电镀镀铜和电镀镀铜并且随后执行老化处理的情况和其中执行无电镀(即,种层),然后执行中间的老化处理并且执行电镀镀铜的情况,看聚酰亚胺膜和镀铜层之间的粘附性是否有任何差异。
通过使用Instron 3344(万能试验机)以50.8mm/min的十字头速度(Cross headspeed)通过T剥离测试(180°剥离),执行聚酰亚胺膜和镀铜层之间的粘附性测量,在图1中体现出其结果。
如图1中所示,其中连续执行无电镀镀铜和电镀镀铜并且随后执行老化处理的样本和在执行无电镀之后执行老化处理并且随后执行电镀的情况表现出相同的趋势,即,当执行老化处理时,粘附性快速增加直至24小时,然后饱和。
然而,可理解,在对无电镀层(种层)执行老化处理之后形成电镀层的情况比连续执行无电镀和电镀的情况具有高出大约20%或更高的粘附性。
也就是说,对种层进行老化处理的优点是,相比于在完成金属层之后执行老化处理的情况,增大了聚合物膜和金属层之间的粘附性。
[实例2]
在通过无电镀和电镀在聚合物膜上形成镀铜层的过程中,本发明的实例2对应于执行其中向无电镀层和/或电镀层施加预定电流的电流施加处理。
在与实例1相同的无电镀铜和电镀铜条件下,连续执行无电镀和电镀。然后,制备三个对应于各情况下的样本,即,执行2天在空气中的老化并且随后在两种条件下执行电流施加处理的情况、以及用于与电流施加处理的效果进行比较的只执行2天老化处理的情况。
在2天内执行电流施加处理,即,在执行2天老化处理之后施加1mA电流1秒的情况和在执行2天老化处理之后施加1mA电流20分钟的情况。在这种情况下,形成在样本上的各镀层的面积是60cm2。
测量由此制备的样本的粘附性,图2中体现出其结果。
如图2中所示,在不执行电流施加处理的情况下只执行2天老化处理的情况表现出大约397gf/cm的剥离强度,施加电流的两种情况分别表现出454gf/cm和471gf/cm的剥离强度。
以上结果表明,对金属层进行电流施加处理在提高聚合物膜和金属层之间的粘附性方面是有效的。
特别地,由于电流施加处理可在短时间段内执行并且还可几乎没有处理成本地执行,因此电流施加处理可被用作提高金属层的粘附性的最有效方法。
[实例3]
在通过无电镀和电镀在聚合物膜上形成镀铜层的过程中,本发明的实例3对应于当在形成无电镀层或形成电镀层之后执行老化处理时调节用于执行老化处理的气氛。
在与实例1相同的无电镀铜和电镀铜条件下,连续执行无电镀铜和电镀铜。然后,在将样本在25℃下相对湿度为95%的气氛、氮气气氛、真空气氛和水下气氛中分别留存之后,测量随时间推移的粘附性,在图3中体现其结果。
在1天或更长时间内在以上气氛中分别执行老化处理的情况下,在水下气氛中执行老化处理的情况和在25℃下相对湿度为95%的气氛中执行老化处理的情况表现出最高的剥离强度。
粘附性以空气气氛、氮气气氛和真空气氛的顺序减小。
根据以上结果,可理解,为了提高聚酰亚胺膜和镀铜层之间的粘附性,有利的是,在相比于空气气氛具有高湿度的水下气氛或富含水的气氛中执行老化处理。
另外,参照图3,根据执行老化处理的气氛,聚酰亚胺膜和铜层之间的粘附性差异达到大约2倍,可理解的是,需要在气氛中进行老化处理持续至少1天来充分提高粘附性。
另外,在图4中,在25℃下相对湿度为95%的气氛中执行老化处理并且随后将样本在空气中留存的情况下,为了确认增大的剥离强度是否返回到留存在空气中的状态,比较在25℃下相对湿度为95%的气氛中留存5天并且在空气中留存4天的样本的粘附性和在25℃下相对湿度为95%的气氛中留存9天的样本的粘附性。
如图4中所示,在将气氛变成空气之后将样本留存4天的情况表现出相对高的剥离强度。
考虑到在相同条件下在空气中留存6天的样本的剥离强度是大约450gf/cm的事实,可理解,即使气氛变化,因气氛中的老化处理而增加的粘附性得以保持。
Claims (11)
1.一种提高聚合物膜和金属层之间的粘附性的方法,所述方法包括以下步骤:
(a)对聚合物膜执行表面改性处理;
(b)在经表面改性处理的聚合物膜上形成金属层;以及
(c)对所述金属层执行从老化处理或电流施加处理中选择的至少一种。
2.一种提高聚合物膜和金属层之间的粘附性的方法,所述方法包括以下步骤:
(a)对聚合物膜执行表面改性处理;
(b)在经表面改性处理的聚合物膜上形成金属种层;
(c)对所述金属种层执行从老化处理或电流施加处理中选择的至少一种;以及
(d)在所述金属种层上形成金属层。
3.根据权利要求1或2所述的方法,其中,所述聚合物膜是由从热固性树脂、热塑性树脂、聚酯树脂、聚酰亚胺树脂、缩聚物、或其两种或更多种的混合物中选择的至少一种形成的单层膜或多层膜。
4.根据权利要求1或2所述的方法,其中,所述金属层由铜Cu、镍Ni、钴Co、钛Ti、铝Al、铬Cr、钼Mo或其合金形成。
5.根据权利要求1或2所述的方法,其中,在形成所述金属层或所述金属种层之前在所述聚合物膜上形成粘结层。
6.根据权利要求1或2所述的方法,其中,执行所述老化处理达12小时或更长时间。
7.根据权利要求6所述的方法,其中,在0℃至100℃的温度范围内,在具有10%或更大的相对湿度的气氛中,执行所述老化处理。
8.根据权利要求1或2所述的方法,其中,通过向所述金属层的表面施加0.1mA/cm2至1A/cm2的电流密度来执行所述电流施加处理。
9.根据权利要求1或2所述的方法,其中,通过从镀方法或物理汽相沉积PVD方法中选择的方法形成所述金属层。
10.根据权利要求2所述的方法,其中,通过从无电镀方法、无电镀加电镀方法、或PVD方法中选择的方法形成所述金属种层。
11.根据权利要求1或2所述的方法,其中,所述表面改性处理包括从浸入酸或碱溶液中、紫外线UV处理、或等离子体处理中选择的至少一种。
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CN106413266B (zh) * | 2015-07-29 | 2018-11-23 | 苏州卫鹏机电科技有限公司 | 一种聚酰亚胺无胶柔性印刷线路板的制备方法 |
KR102422569B1 (ko) * | 2019-12-27 | 2022-07-20 | 주식회사 아모그린텍 | 브레이징 리본 및 그 제조방법 |
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KR100831760B1 (ko) * | 2006-09-29 | 2008-05-23 | 한국생산기술연구원 | 습식표면처리 및 무전해도금으로 제조된 rfid용 기판 |
KR101298746B1 (ko) * | 2006-09-29 | 2013-08-21 | 한국생산기술연구원 | 습식표면처리기술을 이용한 비전도성 폴리머 기판의 금속화방법 |
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KR101189133B1 (ko) * | 2012-01-20 | 2012-10-10 | 엘에스엠트론 주식회사 | 연성회로 동장 적층판과 이를 이용한 인쇄회로 기판 및 그 제조 방법 |
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- 2012-12-13 KR KR1020120145504A patent/KR101396919B1/ko active IP Right Grant
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- 2013-11-01 US US14/652,127 patent/US20150329971A1/en not_active Abandoned
- 2013-11-01 WO PCT/KR2013/009825 patent/WO2014092335A1/ko active Application Filing
- 2013-11-01 CN CN201380065555.8A patent/CN104854968A/zh active Pending
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CN1189125A (zh) * | 1996-04-18 | 1998-07-29 | 古尔德电子有限公司 | 无粘合剂柔韧层合制品及其制作方法 |
US20110318602A1 (en) * | 2009-02-25 | 2011-12-29 | Jx Nippon Mining & Metals Corporation | Metal-Coated Polyimide Resin Substrate with Excellent Thermal Aging Resistance Properties |
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CN107371338A (zh) * | 2016-05-13 | 2017-11-21 | 苏州卫鹏机电科技有限公司 | 一种超薄金属层的印刷线路板的制备方法 |
CN107371338B (zh) * | 2016-05-13 | 2019-08-20 | 苏州卫鹏机电科技有限公司 | 一种超薄金属层的印刷线路板的制备方法 |
CN112368416A (zh) * | 2018-07-02 | 2021-02-12 | 东丽尖端素材株式会社 | 挠性覆铜板及其制备方法 |
Also Published As
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KR101396919B1 (ko) | 2014-05-19 |
WO2014092335A1 (ko) | 2014-06-19 |
US20150329971A1 (en) | 2015-11-19 |
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