CN101802264A - 在非催化性基材上无电沉积金属的方法 - Google Patents
在非催化性基材上无电沉积金属的方法 Download PDFInfo
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Abstract
本发明提供一种用于在基本无催化剂的基材上无电沉积金属的方法,该方法包括:(a)提供基本无催化剂的基材;以及(b)将所述基本无催化剂的基材暴露于无电镀液中以便在基材上沉积金属,该溶液包含金属离子及用于将金属离子还原成金属的还原剂,其中至少基材表面的温度(T1)或者是被加热到的温度(T1)高于溶液的温度(T2)。
Description
技术领域
本发明涉及一种在基本无催化剂的基材上无电沉积金属的方法,一种包括用所述方法获得的基材的电路,以及一种包括此类电路的电气装置。
背景技术
已知有各种在诸如塑料、陶瓷或金属基材等物体上沉积金属的方法。此类方法包括电镀法,其中利用电流在导电物体,例如基材上沉积金属层。物体以及即将要在该物体上沉积的金属组分均置于溶液之中,其中待镀物体充做阴极,而金属组分充做阳极。溶液中含有相应金属的一种或多种盐,同时还有其它使电流得以通过溶液的离子。向待镀膜物体供电,使得溶液中的金属离子还原成金属,沉积在该物体上,但该金属组分发生溶解并补充溶液中的金属离子。这样一种电镀工艺被用来例如改善待镀物体的各种性质,例如耐磨性和防腐蚀性。
无电镀膜法构成另一类可以将金属沉积至基材之上的工艺。无电镀膜法依赖于在含有还原剂的水溶液中将金属离子催化还原,其原理是金属离子在不使用外部电流的情况下还原成相应的金属并沉积在待镀物体上。相关金属的沉积发生在催化性基材上。少数金属能够引发并催化金属在基材上的无电沉积,例如Pd、Ag、Au、Pt、Cu和Ni。需要金属化但又并非由这些催化性金属组成或者含有这些催化性金属的基材,通常通过在基材的表面上吸附催化性胶体使其具有催化性。大多数情况下的做法是在要沉积所需金属的基材的表面上吸附钯胶体。除基材之外,要沉积至基材上的金属也应当对还原反应具有催化作用,使该过程本身具有自催化作用。关于无电镀膜工艺的一般性描述,可以例如参见1990年在纽约出版的Glenn O.Mallor和JuanB.Hajdu编著的Electroless Plating Fundamentals &Applications一书。如果与电镀法相比,无电镀膜法的一般优势在于不需要电力供应,还在于可以形成在沉积物的均匀性和应力方面得到改善的金属涂层。
发明内容
本发明的目的在于提供一种其中无需金属催化剂引发并催化金属在基材表面上的沉积的无电镀覆法。
令人惊喜的是,研究发现,当需要在其上沉积金属的表面的温度高于含有该金属离子及还原剂的溶液的温度时,即可达到上述结果。
因此,本发明涉及一种用于在基本无催化剂的基材上无电沉积金属或合金的方法,该方法包括以下步骤:
(a)提供基本无催化剂的基材;以及
(b)将所述基本无催化剂的基材暴露于无电镀液中以便在基材上沉积金属,该溶液包含金属离子及用于将该金属离子还原成金属的还原剂,其中至少基材的表面的温度(T1)或者是被加热到的温度(T1)高于溶液的温度(T2)。
依据本发明的方法的优点在于不需要在基材表面上应用金属催化剂来引发并催化该金属化过程。此外,金属沉积因应用的温度高而快速完成。因此,在本发明的上下文中,基本无催化剂的基材是一种未在其上应用金属催化剂以引发或催化在其表面上的金属或合金的沉积的基材。因此,基本无催化剂的基材未曾接种(seeded with)催化剂。除可能的杂质外,基本无催化剂的基材不含催化剂。在优选实施方式中,本发明使用无催化剂的基材。
基材接触无电镀溶液的方式各种各样。例如,无电镀溶液可以通过喷墨打印的方式与基本无催化剂的基材相接触,可以将基材浸在无电镀溶液中,或者如果基材是一种模制产品的话,可以使无电镀溶液与处于模具中的已经制成或正在制作的模制产品相接触。
较佳地,基本无催化剂的基材浸在包含金属离子和还原剂的无电镀的溶液中。
合适的做法是,要沉积至基本无催化剂的基材上的金属或合金选自下组:镍、铜、金、银、锡、或它们的合金、及镍-硼和镍-磷。
较佳地,要沉积至基本无催化剂的基材上的金属是铜。较佳地,要沉积至基本无催化剂的基材上的合金是镍-磷或镍-硼合金。
依据本发明,至少基材表面的温度(T1)或者是被加热到的温度(T1)高于溶液的温度(T2)
合适的是,温度T1在50-200℃的范围内。较佳地,温度T1在80-180℃的范围内,更佳的是在70-140℃的范围内。
合适的是,温度T2在15-90℃的范围内。较佳地,温度T2在15-60℃的范围内。更佳的是15-25℃的范围内。换言之,合适的T2可以是环境温度。
合适的是,本发明中所用的基本无催化剂的基材可以适当包括液晶聚合物(LCP)、聚酰胺(PA6、PA6,6、PA4,6、或PA12)、聚苯硫醚(PPS)、聚醚酰亚胺(PEI)、聚对苯二甲酸丁二醇酯(PBT)、间同立构聚苯乙烯(SPS)、聚对苯二甲酸乙二醇酯(PET)、聚碳酸酯(PC)、丙烯腈-丁二烯-苯乙烯(ABS)、聚碳酸酯/ABS、聚丙烯(PP)、聚乙烯(PE)、诸如环氧化物或聚酯混合物等热硬化材料或陶瓷材料。
在本发明方法的一个实施方式中,可以选择无电镀液中尽可能高的金属离子和还原剂的浓度,即接近最大溶解度,同时维持室温下的稳定性。
合适的是,依据本发明使用的还原剂选自下组:甲醛、二甲氨基硼烷、次磷酸(hypophosphite)、硼氢化钠和肼。
合适的是,依据本发明使用的无电镀溶液还包含络合剂。合适的是,所述络合剂选自下组:乙酸盐、丙酸盐、琥珀酸盐、羟基乙酸盐、氨、羟基丙酸盐、乙醇酸、氨基乙酸盐、乙二胺、氨基丙酸盐、丙二酸盐、焦磷酸盐、苹果酸盐、柠檬酸盐、葡糖酸盐、酒石酸盐、EDTA、丙腈、四亚乙基四胺、1,5,8,12-四氮杂十一烷、1,4,8,12-四氮杂环十五烷、和1,4,8,11-四氮杂癸烷(tetraazandecane)。
合适的是,依据本发明使用的无电镀液还包含缓冲剂。合适的是,所述缓冲剂选自下组:乙酸、丙酸、琥珀酸、戊二酸、己二酸、有机胺、和羧酸。
合适的是,本发明方法中使用的无电镀液还包含稳定剂。合适的是,所述稳定剂包含重金属离子、有机或无机的含硫、含硒或含碲化合物(tellur-containing compound)。
在一个特定实施方式中,本发明的方法在模具中执行,因此,所述基材用三维注塑法在模具中制成。
除此之外,本发明还涉及一种包括用本发明的方法获得的基材的电路。
本发明还涉及一种包括依据本发明获得的基材的装置。
合适的装置包括但不限于天线结构、互连元件传感器、致动器。
较佳地,依据本发明的装置是包括依据本发明的电路的电气装置。
实施例I
所用的无电镀溶液含有0.06摩尔/升的硫酸铜。该无电镀溶液用浓度为0.2摩尔/升的三乙醇胺进行缓冲。无电镀溶液的pH为9.0。随后用1,4,8,11-四氮杂十一烷作为络合剂按0.05摩尔/升的用量对如此获得的无电镀液进行稳定化处理。该无电镀液还含有作为还原剂的二甲氨基硼烷,其含量是0.06摩尔/升。随后将环境温度下的无电镀溶液与表面温度为130℃的聚酰胺基材(Stanyl TE200F6型,DSM公司提供)接触。在20秒内获得封闭的(closed)金属化导电表面。
实施例II
所用的无电镀液含有0.08摩尔/升的硫酸铜。该无电镀液用浓度为0.2摩尔/升的三乙醇胺进行缓冲。无电镀液的pH为9.0。随后用1,4,8,11-四氮杂十一烷作为络合剂按0.08摩尔/升的用量对如此获得的无电镀液进行稳定化处理。该无电镀液还含有作为还原剂的二甲氨基硼烷,其含量是0.06摩尔/升。随后使环境温度下的无电镀液与表面温度为90℃的液晶聚合物基材(Vectra 820i型,Ticona公司提供)接触。在该步骤之前,基材已经在热(80℃)的碱性溶液中进行了蚀刻以便活化。在20秒内获得封闭的金属化导电表面。
Claims (20)
1.一种用于在基本无催化剂的基材上无电沉积金属的方法,该方法包括:
(a)提供基本无催化剂的基材;以及
(b)将所述基本无催化剂的基材暴露于无电镀溶液中以便在基材上沉积金属,该溶液包含金属离子及用于将所述金属离子还原成金属的还原剂,其中至少基材表面的温度(T1)或者是被加热到的温度(T1)高于溶液的温度(T2)。
2.如权利要求1所述的方法,其中,将所述基材浸在所述溶液中。
3.如权利要求1或2所述的方法,其中,所述金属选自下组:铜、镍、金、银、锡、或其任意合金、及镍-硼和镍-磷。
4.如权利要求3所述的方法,其中,所述金属是铜。
5.如权利要求3所述的方法,其中,所述合金是镍-磷或镍-硼。
6.如权利要求1至5中任一项所述的方法,其中,所述温度T1在50-200℃范围内。
7.如权利要求6所述的方法,其中,所述温度T1在70-140℃范围内。
8.如权利要求1至7中任一项所述的方法,其中,所述温度T2在15-90℃范围内。
9.如权利要求8所述的方法,其中,所述温度T2在15-25℃范围内。
10.如权利要求1至9中任一项所述的方法,其中,所述基材包括液晶聚合物(LCP)、聚酰胺(PA6、PA6,6、PA4,6、或PA12)、聚苯硫醚(PPS)、聚醚酰亚胺(PEI)、聚对苯二甲酸丁二醇酯(PBT)、间同立构聚苯乙烯(SPS)、聚对苯二甲酸乙二醇酯(PET)、聚碳酸酯(PC)、丙烯腈-丁二烯-苯乙烯(ABS)、聚碳酸酯/ABS、聚丙烯(PP)、聚乙烯(PE)、诸如环氧化物或聚酯混合物等热硬化材料或陶瓷材料。
11.如权利要求1至10中任一项所述的方法,其中所述还原剂选自下组:甲醛、二甲氨基硼烷、次磷酸盐、硼氢化钠和肼。
12.如权利要求1至11中任一项所述的方法,其中所述溶液还包含络合剂。
13.如权利要求12所述的方法,其中所述络合剂选自下组:乙酸盐、丙酸盐、琥珀酸盐、羟基乙酸盐、氨、羟基丙酸盐、乙醇酸盐、氨基乙酸盐、乙二胺、氨基丙酸盐、丙二酸盐、焦磷酸盐、苹果酸盐、柠檬酸盐、葡糖酸盐、酒石酸盐、EDTA、丙腈、四亚乙基四胺、1,5,8,12-四氮杂十一烷、1,4,8,12-四氮杂环十五烷、和1,4,8,11-四氮杂癸烷。
14.如权利要求1至13中任一项所述的方法,其中,所述溶液还包含缓冲剂。
15.如权利要求14所述的方法,其中,所述缓冲剂选自下组:乙酸、丙酸、琥珀酸、戊二酸、己二酸、有机胺、和羧酸。
16.如权利要求1至15中任一项所述的方法,其中,所述溶液还包含稳定剂。
17.如权利要求16所述的方法,其中,所述稳定剂包括重金属离子、有机或无机的含硫、含硒或含碲化合物。
18.如权利要求1至17中任一项所述的方法,其中,在模具中进行该方法,其中所述基材采用三维注塑法在模具中制成。
19.一种电路,其包括根据如权利要求1至18中的任一项所述的方法获得的基材。
20.一种电气装置,其包括如权利要求19所述的电路。
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EP20070115731 EP2034049A1 (en) | 2007-09-05 | 2007-09-05 | An electroless process for depositing a metal on a non-catalytic substrate |
EP07115731.7 | 2007-09-05 | ||
PCT/NL2008/050583 WO2009031892A1 (en) | 2007-09-05 | 2008-09-05 | An electroless process for depositing a metal on a non-catalytic substrate |
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CN101802264A true CN101802264A (zh) | 2010-08-11 |
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US (1) | US20100215974A1 (zh) |
EP (2) | EP2034049A1 (zh) |
JP (1) | JP2010538166A (zh) |
CN (1) | CN101802264A (zh) |
WO (1) | WO2009031892A1 (zh) |
Cited By (7)
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CN104815693A (zh) * | 2015-04-02 | 2015-08-05 | 同济大学 | 一种贵金属纳米粒子修饰多孔载体催化材料及其制备方法 |
CN105779980A (zh) * | 2016-03-09 | 2016-07-20 | 昆山艾森半导体材料有限公司 | 一种化学镀铜剂及其制备方法 |
CN106917077A (zh) * | 2015-12-25 | 2017-07-04 | 钧泽科技有限公司 | 无电镀铜镀液及增加铜镀层硬度的无电镀铜方法 |
CN106929832A (zh) * | 2015-12-30 | 2017-07-07 | 凯基有限公司 | 聚乙酰胺或聚对苯二甲酸乙二酯基材的湿式金属化处理监测控制系统 |
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CN110139948A (zh) * | 2016-12-28 | 2019-08-16 | 德国艾托特克公司 | 锡电镀浴液和在衬底的表面上沉积锡或锡合金的方法 |
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EP2033756A1 (en) * | 2007-09-05 | 2009-03-11 | Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO | A process for preparing a moulded product |
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DD157989A3 (de) * | 1980-10-10 | 1982-12-22 | Lothar Gierth | Verfahren zur strukturierten chemisch-reduktiven metallabscheidung |
DD249495A1 (de) * | 1986-06-02 | 1987-09-09 | Zeiss Jena Veb Carl | Verfahren und vorrichtung zur chemisch-reduktiven abscheidung von nickel |
US20020086102A1 (en) * | 2001-01-02 | 2002-07-04 | John Grunwald | Method and apparatus for improving interfacial chemical reactions in electroless depositions of metals |
US6805911B2 (en) * | 2001-01-02 | 2004-10-19 | J.G. Systems, Inc. | Method and apparatus for improving interfacial chemical reactions |
US20030152690A1 (en) * | 2002-02-07 | 2003-08-14 | Yuh Sung | Method for operating and controlling electroless plating |
US6846519B2 (en) * | 2002-08-08 | 2005-01-25 | Blue29, Llc | Method and apparatus for electroless deposition with temperature-controlled chuck |
US6773760B1 (en) * | 2003-04-28 | 2004-08-10 | Yuh Sung | Method for metallizing surfaces of substrates |
DE102005009072B4 (de) * | 2005-02-28 | 2016-12-08 | Advanced Micro Devices, Inc. | Verfahren und Vorrichtung zur Metallabscheidung durch stromloses Plattieren unter Anwendung eines Aktivierungsschemas mit einem Substraterwärmungsprozess |
-
2007
- 2007-09-05 EP EP20070115731 patent/EP2034049A1/en not_active Withdrawn
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2008
- 2008-09-05 US US12/675,985 patent/US20100215974A1/en not_active Abandoned
- 2008-09-05 JP JP2010523972A patent/JP2010538166A/ja not_active Withdrawn
- 2008-09-05 WO PCT/NL2008/050583 patent/WO2009031892A1/en active Application Filing
- 2008-09-05 EP EP20080829258 patent/EP2198072A1/en not_active Withdrawn
- 2008-09-05 CN CN200880106054A patent/CN101802264A/zh active Pending
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EP2198072A1 (en) | 2010-06-23 |
EP2034049A1 (en) | 2009-03-11 |
WO2009031892A1 (en) | 2009-03-12 |
JP2010538166A (ja) | 2010-12-09 |
US20100215974A1 (en) | 2010-08-26 |
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