CN101133187B - 树脂基材、对其实施无电镀而成的电子部件基材、和电子部件基材的制造方法 - Google Patents
树脂基材、对其实施无电镀而成的电子部件基材、和电子部件基材的制造方法 Download PDFInfo
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- CN101133187B CN101133187B CN2006800070309A CN200680007030A CN101133187B CN 101133187 B CN101133187 B CN 101133187B CN 2006800070309 A CN2006800070309 A CN 2006800070309A CN 200680007030 A CN200680007030 A CN 200680007030A CN 101133187 B CN101133187 B CN 101133187B
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Classifications
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/31—Coating with metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/38—Improvement of the adhesion between the insulating substrate and the metal
- H05K3/389—Improvement of the adhesion between the insulating substrate and the metal by the use of a coupling agent, e.g. silane
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/46—Manufacturing multilayer circuits
- H05K3/4644—Manufacturing multilayer circuits by building the multilayer layer by layer, i.e. build-up multilayer circuits
- H05K3/4661—Adding a circuit layer by direct wet plating, e.g. electroless plating; insulating materials adapted therefor
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明提供一种可适于作为基板材料的一般树脂基材的，可以提高该基材与金属镀层的密合强度的技术，也就是说，提供一种与金属镀层的密合强度提高了的一般的树脂基材。本发明是：使用含有咪唑硅烷、和具有无电镀的催化作用的钯等贵金属化合物的溶液，处理对该溶液具有溶胀性的表面，从而得到的环氧树脂等树脂基材，以及在该树脂基材上实施了无电镀的电子部件基材。
Description
技术领域
本发明涉及特别是可作为电子部件基材使用的树脂基材。详细地说，是涉及可以用作能形成与树脂层密合性好的无电镀层的电子部件基材的树脂基材。
背景技术
近年来，由于印刷基板设备的小型化、高性能化的需要，其配线密度不断增大。伴随而来的是，为了使配线细微化，而使基板表面低轮廓(low-profile)化，由于其表面的低粗化趋势，所以难于获得基板与在基板上形成的金属镀膜的足够的密合性。另外，为了满足上述要求，还需要提高此密合强度。
为适应这样的需要，已经有了各种提案。其中，在专利文献1或2中，公开了一种技术，即，在聚酰亚胺树脂基材上涂布含钯化合物的聚酰亚胺树脂前体溶液，并干燥，形成聚酰亚胺树脂前体层，接着在氢供体的存在下照射紫外线，形成基底镀核，然后通过无电镀处理形成基底金属镀层，进一步在形成表面镀层后或形成前，加热上述聚酰亚胺树脂前体层，使之亚胺化，制成聚酰亚胺树脂层。这是通过在聚酰亚胺树脂层内形成基底镀核从而产生的固着效果，使聚酰亚胺树脂层与基底金属镀层的密合强度提高。
专利文献1：特开2002-30216号公报
专利文献2：特开2002-374055号公报
发明内容
不过，在上述提案中基板材料限定于聚酰亚胺树脂，通常不能适用于电子部件用基板。另外，为了使钯活化而需要紫外线处理，进而为了亚胺化而需要高温加热等，其处理工序繁杂。
本发明提供一种适合作为基板材料的一般树脂基材使用的，可以更简易地提高该基材与金属镀层的密合强度的技术。即本发明的目的在于，提供与金属镀层的密合强度提高的可作为电子部件基材使用的一般的树脂基材。
本发明人进行了精心研究，结果发现，使用含有无电镀催化剂贵金属化合物和能捕捉它的咪唑硅烷的溶液，可有效地处理对该溶液具有溶胀性的树脂基材表面，从而完成了本发明。即，本发明涉及：
[1]一种树脂基材，是使用含有咪唑硅烷和贵金属化合物的溶液，处理对该溶液具有溶胀性的B级的热固性树脂基材的表面，从而形成的。
[2]如上述[1]所述的经表面处理而成的树脂基材，上述B级的热固性树脂基材是B级的环氧树脂。
[3]如上述[1]或2所述的经表面处理而成的树脂基材，贵金属化合物是钯化合物。
[4]一种电子部件基材，在上述[1]～[5]的任一项所述的经表面处理而成的树脂基材上实施了无电镀。
[5]如上述[4]所述的电子部件基材，树脂基材为环氧树脂。
[6]如上述[4]或[5]所述的电子部件基材，其中，电子部件基材为构建(build-up)基板。
[7]一种电子部件基材的制造方法，含有以下工序：使用含有咪唑硅烷和贵金属化合物的溶液处理对该溶液具有溶胀性的B级的热固性树脂基材的表面，在所形成的树脂基材上，实施无电镀。
[8]如上述[7]所述的电子部件基材的制造方法，上述B级的热固性树脂基材为B级的环氧树脂。
[9]如上述[7]或[8]所述的电子部件基材的制造方法，电子部件基材为构建基板。
根据本发明，树脂基材在用含有咪唑硅烷和贵金属化合物的溶液进行表面处理时，由于该溶液而引起表面溶胀，所以使贵金属催化剂经表面潜入内部的树脂层中，并存在于内部的树脂层。为此，通过对该树脂基材进行无电镀，金属也可以同样析出到树脂层内部。通过此金属镀层的固定效果，可以使树脂基材的树脂层与通过无电镀形成的金属层之间的密合强度提高。
具体实施方式
作为本发明使用的树脂基材，只要是通过上述作用，用含有咪唑硅烷和贵金属化合物的溶液进行处理表面，其表面被溶胀的树脂材料，就没有特别限制。例如可以举出，环氧树脂、酚树脂、聚氨酯树脂、三聚氰胺树脂、硅树脂等。这些树脂是热固性树脂的情况下，优选所谓的B级树脂，它通过用上述溶液处理表面而容易溶胀，是完全固化前的阶段的树脂。
在本发明中，特别优选的树脂基材是环氧树脂。作为环氧树脂，例如可以举出，双酚A、双酚F等双酚类二缩水甘油醚化物(双酚型环氧树脂)，侧链、或主链被橡胶、聚氨脂、聚醚、聚酯等挠性树脂改性的环氧树脂，苯酚线型酚醛清漆树脂、甲酚线型酚醛清漆树脂等缩水甘油醚化合物(线型酚醛清漆型环氧树脂)、或者聚丁二烯等共轭二烯聚合物的环氧化物等。作为本发明使用的咪唑硅烷，优选可以捕捉贵金属化合物的以下(1)、(2)和(3)所示的化合物。
(其中，R1是氢或碳数为1～20的烷基，R2是氢、乙烯基或碳数1～5的烷基，R3、R4为碳数1～3的烷基，n表示1～3。)
在上述式(1)、(2)、(3)中，R1～R4具有上述那样的各自规定的意义，不过，特别从合成的难易性角度考虑，R1优选氢、甲基、乙基、十一烷基、十七烷基，R2优选氢、甲基、乙基，R3、R4优选甲基、乙基。
关于上述合成法，被公开在特开平5-186479号公报中。
即，可通过以下所示的咪唑化合物(通式(4))与3-(环氧丙氧基)丙基硅烷化合物(通式(5))的等摩尔反应来合成。另外，在通过此合成法获得上述(1)、(2)、(3)所示的咪唑硅烷混合物的情况下，也不需要特别的分离，以混合形态使用较便利。
(上述式中，R1是氢或碳数为1～20的烷基，R2是氢、乙烯基或碳数1～5的烷基，R3和R4为碳数1～3的烷基，n表示1～3。)
作为上述通式(4)所示的咪唑化合物优选的是，咪唑、2-烷基咪唑、2，4-二烷基咪唑、4-乙烯基咪唑等。其中特别优选的可以列举出，咪唑；作为2-烷基咪唑的2-甲基咪唑、2-乙基咪唑、2-十一烷基咪唑、2-十七烷基咪唑；还有作为2，4-二烷基咪唑的2-乙基-4-甲基咪唑等。
另外，上述通式(5)所示的3-(环氧丙氧基)丙基硅烷化合物，为3-(环氧丙氧基)丙基三烷氧基硅烷、3-(环氧丙氧基)丙基二烷氧基烷基硅烷、3-(环氧丙氧基)丙基烷氧基二烷基硅烷，其中特别优选的化合物可以列举出：作为3-(环氧丙氧基)丙基三烷氧基硅烷的3-(环氧丙氧基)丙基三甲氧基硅烷、3-(环氧丙氧基)丙基三乙氧基硅烷；作为3-(环氧丙氧基)丙基二烷氧基烷基硅烷的3-(环氧丙氧基)丙基二甲氧基甲基硅烷；作为3-(环氧丙氧基)丙基烷氧基二烷基硅烷的3-(环氧丙氧基)丙基乙氧基二甲基硅烷等。
另外，本发明使用的贵金属化合物可以使用在无电镀(electrolessplating)中一直使用的贵金属化合物催化剂。作为这些贵金属化合物，可以列举出，在使铜、镍等金属从无电镀液析出在被镀物表面上时，可显示催化作用的钯皂、钯、银、铂、金等的氯化物、氢氧化物、氧化物、硫酸盐、铵盐等胺配合物等。在上述化合物中优选钯化合物，特别优选环烷酸钯等钯皂。贵金属化合物在上述处理液中以1～30000mg/L的浓度使用，优选以10～20000mg/L的浓度使用。
本发明中使用的咪唑硅烷，在上述处理液中以1～30000mg/L的浓度使用，优选以10～20000mg/L的浓度使用。
作为此处理液中使用的溶剂，只要可溶解咪唑硅烷和贵金属化合物，且通过用此处理液对树脂基材进行表面处理，可使该树脂溶胀的溶剂，就没有限制。
作为上述溶剂，特别优选甲基乙基酮、辛醇、丁醇等。另外，虽然咪唑硅烷不溶于水，但可以通过使用水与乙二醇等有机溶剂的混合物作为溶剂，从而溶解制成水溶液。这样的水与乙二醇等的混合溶液作为溶剂也是优选的。
作为表面处理方法，可以用通常的处理方法，可列举出涂布、浸渍等。在涂布、浸渍后，干燥、除去溶剂。
另外，在上述表面处理前，通过用高锰酸等处理，使表面粗化，由此可进一步提高密合强度。
另外，为了使通过贵金属化合物与咪唑硅烷处理了的树脂基材的无电镀活性进一步活化，优选在进行无电镀前，通过还原剂进行处理。作为该还原剂，在无电镀时可以使用通常使用的公知还原剂，优选可以列举出，次磷酸、次磷酸钠等次磷酸的碱金属盐、二甲基硼烷等。
在本发明中，无电镀其自身可以用公知的方法，并没有特别的限制。无电镀优选镀铜，不过也可以是镀镍、钴等。
另外，可以在无电镀后进行电镀。关于此电镀法没有特别限制，可以使用公知技术。例如可使用铜、铬、镍、银等。
另外，作为基材使用完全固化前的树脂时，优选进行电镀后，或者进行无电镀后，进行加热，使之完全固化。
本发明包含：在由含有贵金属化合物和咪唑硅烷的溶液处理过的树脂基材上，进行了无电镀的电子部件基材和构建基板。
实施例
实施例1
将5g咪唑硅烷[咪唑与3-(环氧丙氧基)丙基三甲氧基硅烷的等摩尔反应生成物]、和10g环烷酸钯混合溶解到1L甲乙酮中，用贝克涂布器(Baker applicator)涂布在半固化状态(140℃固化)的环氧树脂(松下电工社制，环氧树脂预浸渍物，R-1661T)的表面上。在120℃进行溶剂干燥。涂布层为0.1μm。浸渍到浓度为30g/L的次亚磷酸(次磷酸)的还原液中，然后进行水洗处理，使Pd活化后，进行无电镀铜(高温类型的福尔马林系镀铜液，KC500(日鉱メタルプレ一テイング(株)制)，0.3μm厚)和电镀铜(硫酸铜镀，1.5A/dm2，35μm厚)。170℃充分熟化后的剥离强度为1.0kgf/cm。且剥离强度为90°的剥离强度(JIS C 6481)。以下也相同。
实施例2
将5g咪唑硅烷[咪唑与3-(环氧丙氧基)丙基三甲氧基硅烷的等摩尔反应生成物]、和10g环烷酸钯混合溶解到1L辛醇中，用贝克涂布器涂布在半固化状态(100℃固化)的环氧树脂(松下电工社制，环氧树脂预浸渍物，R-1661T)的表面上。在120℃进行溶剂干燥。涂布层为0.1μm。浸渍到浓度为30g/L的次亚磷酸(次磷酸)的还原液中，然后进行水洗处理，使Pd活化后，进行无电镀铜(高温类型的福尔马林系镀铜液，KC500(日鉱メタルプレ一テイング(株)制)，0.3μm厚)和电镀铜(硫酸铜镀，1.5A/dm2，35μm厚)。在170℃充分熟化后的剥离强度为1.2kgf/cm。
实施例3
将5g咪唑硅烷[咪唑与3-(环氧丙氧基)丙基三甲氧基硅烷的等摩尔反应生成物]与10g环烷酸钯混合溶解到1L辛醇中，使环氧树脂(松下电工社制，环氧树脂预浸渍物，R-1661T)处于半固化状态(140℃固化)且进一步用高锰酸进行粗化处理，然后在环氧树脂表面上，用贝克涂布器涂布。在120℃进行溶剂干燥，涂布层为0.1μm。将环氧树脂浸渍到浓度为30g/L的次亚磷酸(次磷酸)的还原液中，然后进行水洗处理，使Pd活化，然后进行无电镀铜(高温类型的福尔马林系镀铜液，KC500(日鉱メタルプレ一テイング(株)制)，0.3μm厚)和电镀铜(硫酸铜镀，1.5A/dm2，35μm厚)。在170℃充分熟化后的剥离强度为1.4kgf/cm。
实施例4
在含有200mg/L咪唑硅烷[咪唑与3-(环氧丙氧基)丙基三甲氧基硅烷的等摩尔反应的生成物]、100mg/L氯化钯(换算成Pd为60mg/L)、与30g/L的乙二醇的溶液中，浸渍环氧树脂(松下电工社制，环氧树脂预浸渍物，R·1661T)为半固化状态(100℃固化)且用高锰酸粗化处理过的环氧树脂。在120℃干燥后，浸渍到浓度为30g/L的次亚磷酸(次磷酸)的还原液中，然后进行水洗处理，使Pd活化，然后进行无电镀铜(高温类型的福尔马林系镀铜液，KC500(日鉱メタルプレ一テイング(株)制)，0.3μm厚)和电镀铜(硫酸铜镀，1.5A/dm2，35μm厚)。在170℃充分熟化后的剥离强度为1.1kgf/cm。
实施例5
除了将环氧树脂改成聚酰亚胺树脂(三菱ガス化学社制，BT树脂预浸渍物，GHPL-950K)以外，其他与实施例1进行同样的处理。剥离强度为1.1kgf/cm。
比较例1
除了将环氧树脂(松下电工社制，环氧树脂预浸渍物，R·1661T)变成C态品(完全固化品)以外，其他与实施例1进行相同的处理。剥离强度为0.4kgf/cm。
Claims (9)
1.一种树脂基材，是使用含有咪唑硅烷和贵金属化合物的溶液，处理对该溶液具有溶胀性的B级的热固性树脂基材的表面，从而形成的。
2.如权利要求1所述的树脂基材，上述B级的热固性树脂基材是B级的环氧树脂。
3.如权利要求1或2所述的树脂基材，贵金属化合物是钯化合物。
4.一种电子部件基材，是在权利要求1～3的任一项所述的树脂基材上，实施无电镀而形成的。
5.如权利要求4所述的电子部件基材，树脂基材为环氧树脂。
6.如权利要求4或5所述的电子部件基材，电子部件基材为构建基板。
7.一种电子部件基材的制造方法，含有以下工序：在使用含有咪唑硅烷和贵金属化合物的溶液，处理对该溶液具有溶胀性的B级的热固性树脂基材的表面从而形成的B级的树脂基材上，实施无电镀。
8.如权利要求7所述的电子部件基材的制造方法，上述B级的热固性树脂基材为B级的环氧树脂。
9.如权利要求7或8所述的电子部件基材的制造方法，电子部件基材为构建基板。
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| KR101445461B1 (ko) * | 2010-03-23 | 2014-09-26 | 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 | 무전해 도금 전처리제, 그것을 이용하는 무전해 도금 방법 및 무전해 도금물 |
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| CN1406288A (zh) * | 2000-04-25 | 2003-03-26 | 株式会社日矿材料 | 镀覆用预处理剂和使用它的金属镀覆方法 |
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| US20080138629A1 (en) | 2008-06-12 |
| KR101106845B1 (ko) | 2012-01-19 |
| JP4428579B2 (ja) | 2010-03-10 |
| KR100976313B1 (ko) | 2010-08-16 |
| TWI313687B (en) | 2009-08-21 |
| US8043705B2 (en) | 2011-10-25 |
| CN101133187A (zh) | 2008-02-27 |
| TW200640938A (en) | 2006-12-01 |
| JPWO2006095589A1 (ja) | 2008-08-14 |
| WO2006095589A1 (ja) | 2006-09-14 |
| KR20090126317A (ko) | 2009-12-08 |
| KR20070110100A (ko) | 2007-11-15 |
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