JP4919501B2 - Silane coupling agent film analysis method - Google Patents
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- JP4919501B2 JP4919501B2 JP2007130798A JP2007130798A JP4919501B2 JP 4919501 B2 JP4919501 B2 JP 4919501B2 JP 2007130798 A JP2007130798 A JP 2007130798A JP 2007130798 A JP2007130798 A JP 2007130798A JP 4919501 B2 JP4919501 B2 JP 4919501B2
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- 239000006087 Silane Coupling Agent Substances 0.000 title claims description 87
- 238000004458 analytical method Methods 0.000 title claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 31
- 239000004020 conductor Substances 0.000 claims description 26
- 229910052802 copper Inorganic materials 0.000 claims description 19
- 239000010949 copper Substances 0.000 claims description 19
- 239000002696 acid base indicator Substances 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- -1 acryloxy group Chemical group 0.000 claims description 8
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-UHFFFAOYSA-N 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 6
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- JCYPECIVGRXBMO-UHFFFAOYSA-N 4-(dimethylamino)azobenzene Chemical compound C1=CC(N(C)C)=CC=C1N=NC1=CC=CC=C1 JCYPECIVGRXBMO-UHFFFAOYSA-N 0.000 claims description 5
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 claims description 5
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 125000003277 amino group Chemical group 0.000 claims description 3
- 125000003700 epoxy group Chemical group 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 3
- 229940012189 methyl orange Drugs 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 125000000524 functional group Chemical group 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 17
- 239000011889 copper foil Substances 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 11
- 238000002845 discoloration Methods 0.000 description 10
- 238000007654 immersion Methods 0.000 description 7
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 7
- 238000005530 etching Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- OTARVPUIYXHRRB-UHFFFAOYSA-N diethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](C)(OCC)CCCOCC1CO1 OTARVPUIYXHRRB-UHFFFAOYSA-N 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000007788 roughening Methods 0.000 description 2
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- DOYKFSOCSXVQAN-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CCO[Si](C)(OCC)CCCOC(=O)C(C)=C DOYKFSOCSXVQAN-UHFFFAOYSA-N 0.000 description 1
- LZMNXXQIQIHFGC-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CO[Si](C)(OC)CCCOC(=O)C(C)=C LZMNXXQIQIHFGC-UHFFFAOYSA-N 0.000 description 1
- OKWYEBJNFREPEV-UHFFFAOYSA-N 3-[dimethoxy(phenylmethoxy)silyl]propan-1-amine Chemical compound NCCC[Si](OC)(OC)OCC1=CC=CC=C1 OKWYEBJNFREPEV-UHFFFAOYSA-N 0.000 description 1
- URDOJQUSEUXVRP-UHFFFAOYSA-N 3-triethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CCO[Si](OCC)(OCC)CCCOC(=O)C(C)=C URDOJQUSEUXVRP-UHFFFAOYSA-N 0.000 description 1
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- ZPLCXHWYPWVJDL-UHFFFAOYSA-N 4-[(4-hydroxyphenyl)methyl]-1,3-oxazolidin-2-one Chemical compound C1=CC(O)=CC=C1CC1NC(=O)OC1 ZPLCXHWYPWVJDL-UHFFFAOYSA-N 0.000 description 1
- PRKPGWQEKNEVEU-UHFFFAOYSA-N 4-methyl-n-(3-triethoxysilylpropyl)pentan-2-imine Chemical compound CCO[Si](OCC)(OCC)CCCN=C(C)CC(C)C PRKPGWQEKNEVEU-UHFFFAOYSA-N 0.000 description 1
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 description 1
- 241000984082 Amoreuxia Species 0.000 description 1
- SQUNKLNGFIILTR-UHFFFAOYSA-N C1(CCCCC1)CO[Si](OC)(OC)CC Chemical compound C1(CCCCC1)CO[Si](OC)(OC)CC SQUNKLNGFIILTR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 description 1
- WWAABJGNHFGXSJ-UHFFFAOYSA-N chlorophenol red Chemical compound C1=C(Cl)C(O)=CC=C1C1(C=2C=C(Cl)C(O)=CC=2)C2=CC=CC=C2S(=O)(=O)O1 WWAABJGNHFGXSJ-UHFFFAOYSA-N 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- PNOXNTGLSKTMQO-UHFFFAOYSA-L diacetyloxytin Chemical compound CC(=O)O[Sn]OC(C)=O PNOXNTGLSKTMQO-UHFFFAOYSA-L 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- XJRPTMORGOIMMI-UHFFFAOYSA-N ethyl 2-amino-4-(trifluoromethyl)-1,3-thiazole-5-carboxylate Chemical compound CCOC(=O)C=1SC(N)=NC=1C(F)(F)F XJRPTMORGOIMMI-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- XEMZLVDIUVCKGL-UHFFFAOYSA-N hydrogen peroxide;sulfuric acid Chemical compound OO.OS(O)(=O)=O XEMZLVDIUVCKGL-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 description 1
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 1
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 1
- RMTGISUVUCWJIT-UHFFFAOYSA-N n-[3-[3-aminopropoxy(dimethoxy)silyl]propyl]-1-phenylprop-2-en-1-amine;hydrochloride Chemical compound Cl.NCCCO[Si](OC)(OC)CCCNC(C=C)C1=CC=CC=C1 RMTGISUVUCWJIT-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000007793 ph indicator Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical group CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Description
本発明はシランカップリング剤皮膜の分析方法に関する。 The present invention relates to a method for analyzing a silane coupling agent film.
従来からプリント配線板の製造において、銅又は銅合金などの金属からなる導体表面と、ソルダーレジストやプリプレグなどの絶縁樹脂との密着性を向上させるために、金属表面にシランカップリング剤を処理することが行われている。特許文献１には、銅回路表面に水酸基を付与しシラン系カップリング剤を付着させることが開示されている。特許文献２には、回路パターン表面をシランカップリング剤で処理した内層板をボンディングシートと外層金属箔とを積層する。ことが開示されている。特許文献３には、回路表面に銅酸化物層を形成してからエチレンジアミン４酢酸アルカリ塩溶液で溶解除去して凹凸を形成した後、アミノシランカップリング剤で膜を形成した後にプリプレグを積層することが開示されている。特許文献４には、銅回路表面を酸化処理したアミノシラン、エポキシシラン等のカップリング剤で処理することが開示されている。特許文献５には、銅表面をトリアジンチオールなどで処理した後にシランカップリング剤で処理して絶縁樹脂層と積層することが開示されている。 Conventionally, in the production of printed wiring boards, a silane coupling agent is treated on the metal surface in order to improve the adhesion between the conductor surface made of a metal such as copper or copper alloy and an insulating resin such as a solder resist or a prepreg. Things have been done. Patent Document 1 discloses that a hydroxyl group is imparted to the surface of a copper circuit to attach a silane coupling agent. In Patent Document 2, a bonding sheet and an outer layer metal foil are laminated on an inner layer plate whose surface is treated with a silane coupling agent. It is disclosed. In Patent Document 3, a copper oxide layer is formed on a circuit surface, dissolved and removed with an ethylenediaminetetraacetic acid alkali salt solution to form irregularities, a film is formed with an aminosilane coupling agent, and then a prepreg is laminated. Is disclosed. Patent Document 4 discloses that a copper circuit surface is treated with an oxidation-treated coupling agent such as aminosilane or epoxysilane. Patent Document 5 discloses that a copper surface is treated with a triazine thiol or the like and then treated with a silane coupling agent to be laminated with an insulating resin layer.
このようなシランカップリング剤皮膜を金属−樹脂間の密着性向上のために形成する場合、シランカップリング剤皮膜が均一に形成されていないと目的の密着強度が得られないため、シランカップリング剤皮膜の付着状態を確認する必要がある。 When such a silane coupling agent film is formed to improve the adhesion between the metal and the resin, the desired adhesion strength cannot be obtained unless the silane coupling agent film is formed uniformly. It is necessary to check the adhesion state of the agent film.
従来はシランカップリング剤皮膜の付着状況はＸ線光電子分光分析装置（ＸＰＳ）など詳細な表面分析によって銅及び銅合金表面を測定し、銅及び銅合金表面に存在するＳｉ量の測定などを行うことでシランカップリング剤皮膜の有無を確認してきた。
しかし、従来のＸ線光電子分光分析装置（ＸＰＳ）などによる詳細分析には、（１）真空条件での測定を要し時間がかかる、（２）装置が高価である、（３）装置使用者のトレーニングが必要であるなどの問題点があり、特に基板量産時におけるシランカップリング剤皮膜の分析方法としては実施が困難であると考えられる。 However, detailed analysis using a conventional X-ray photoelectron spectrometer (XPS) or the like requires (1) measurement under vacuum conditions and takes time, (2) the apparatus is expensive, and (3) the user of the apparatus. It is considered that it is difficult to implement as a method for analyzing a silane coupling agent film particularly during mass production of substrates.
本発明は、前記従来の問題を解決するため、シランカップリング剤皮膜の有無、及び被覆状態を効率よく分析する方法を提供する。 In order to solve the above-mentioned conventional problems, the present invention provides a method for efficiently analyzing the presence or absence of a silane coupling agent film and the coating state.
本発明のシランカップリング剤皮膜の分析方法は、導体表面に形成されたシランカップリング剤皮膜の分析方法であって、前記シランカップリング剤皮膜上に酸塩基指示薬を含む指示液を滴下し、その変色を確認することでシランカップリング剤皮膜の有無、及び被覆状態を分析することを特徴とする。
The method for analyzing a silane coupling agent film of the present invention is an analysis method for a silane coupling agent film formed on a conductor surface, and an indicator solution containing an acid-base indicator is dropped on the silane coupling agent film, The presence or absence of the silane coupling agent film and the coating state are analyzed by confirming the discoloration.
本発明の導体層と樹脂層との密着性の分析方法は、金属、金属酸化物、合金から選ばれる少なくとも１つの導体層と、樹脂層の密着を向上させるために、導体表面にシランカップリング剤が塗布されたプリント回路基板における密着性の分析方法であって、前記プリント回路基板に、酸塩基指示薬液を滴下し、変色を確認することで導体層と樹脂層の密着性を分析することを特徴とする。
The method for analyzing the adhesion between the conductor layer and the resin layer according to the present invention includes a silane coupling on the conductor surface in order to improve the adhesion between the resin layer and at least one conductor layer selected from metals, metal oxides, and alloys. agent is an analytical method of adhesion in the printed circuit board coated, the printed circuit board, was added dropwise an acid-base indicator solution, by confirming discoloration analyzing the adhesion of the conductive layer and the resin layer It is characterized by.
本発明は、銅及び／又は銅合金などの導体表面にシランカップリング剤皮膜を形成してから、シランカップリング剤皮膜上に酸塩基指示薬を滴下し、変色を確認することで簡単にシランカップリング剤皮膜の有無、及び被覆状態を分析することができるため、高価な装置やそれを扱う熟練が不要で、特にプリント回路基板などを製造する現場でのシランカップリング剤皮膜分析に好適である。また、この方法により、特に銅及び／又は銅合金からなる導体層と樹脂層の密着性をシランカップリング剤皮膜の形成状態で分析する場合に有用なシランカップリング剤皮膜の分析方法及び銅−樹脂間の密着性の分析方法を提供できる。
In the present invention, a silane coupling agent film is formed on the surface of a conductor such as copper and / or a copper alloy, and then an acid-base indicator is dropped on the silane coupling agent film to confirm discoloration. Since it can analyze the presence or absence of the ring agent film and the coating state, it does not require expensive equipment or skill to handle it, and is particularly suitable for silane coupling agent film analysis in the field of manufacturing printed circuit boards etc. . Also, by this method, a method for analyzing a silane coupling agent film, which is particularly useful for analyzing the adhesion between a conductor layer made of copper and / or a copper alloy and a resin layer in the formation state of the silane coupling agent film, and copper- An analysis method for adhesion between resins can be provided.
（１）シランカップリング剤皮膜
本発明の金属など導体上に形成されるシランカップリング剤皮膜は、銅及び／又は銅合金などの金属と絶縁樹脂との密着性を向上させるために塗布されるもので、基本的にはカップリング効果を示すシランカップリング剤であればどのようなシランカップリング剤の皮膜でもよい。特に本発明の分析方法に適したシランカップリング剤皮膜を形成するシランカップリング剤としては、エポキシ基、アミノ基、アクリロキシ基、メタクリロキシ基、ビニル基などの官能基を有するシランカップリング剤が適している。
(1) Silane coupling agent film The silane coupling agent film formed on a conductor such as a metal of the present invention is applied to improve the adhesion between a metal such as copper and / or a copper alloy and an insulating resin. Basically, any silane coupling agent film may be used as long as it is a silane coupling agent exhibiting a coupling effect. As a silane coupling agent that forms a silane coupling agent film particularly suitable for the analysis method of the present invention, a silane coupling agent having a functional group such as an epoxy group, an amino group, an acryloxy group, a methacryloxy group, or a vinyl group is suitable. ing.
エポキシ基を有するシランカップリング剤としては、３−グリシドキシプロピルトリメトキシシラン、３−グリシドキシプロピルメチルジエトキシシラン、３−グリシドキシプロピルトリエトキシシラン、２−（３，４−エポキシシクロヘキシル）エチルトリメトキシシラン、３−グリシドキシプロピルメチルジエトキシシラン等が挙げられる。 Examples of the silane coupling agent having an epoxy group include 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 3-glycidoxypropyltriethoxysilane, and 2- (3,4-epoxy. (Cyclohexyl) ethyltrimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane and the like.
アミノ基を有するシランカップリング剤としては、３−アミノプロピルトリメトキシシラン、３−アミノプロピルトリエトキシシラン、Ｎ−２−（アミノエチル）−３−アミノプロピルメチルジメトキシシラン、Ｎ−２−（アミノエチル）−３−アミノプロピルトリメトキシシラン、Ｎ−２−（アミノエチル）−３−アミノプロピルトリエトキシシラン、３−トリエトキシシリル−Ｎ−（１，３−ジメチル−ブチリデン）プロピルアミン、Ｎ−フェニル−３−アミノプロピルトリメトキシシラン、Ｎ−（ビニルベンジル）−２−アミノエチル−３−アミノプロピルトリメトキシシラン塩酸塩等が挙げられる。 Examples of the silane coupling agent having an amino group include 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-2- (aminoethyl) -3-aminopropylmethyldimethoxysilane, and N-2- (amino Ethyl) -3-aminopropyltrimethoxysilane, N-2- (aminoethyl) -3-aminopropyltriethoxysilane, 3-triethoxysilyl-N- (1,3-dimethyl-butylidene) propylamine, N- Examples include phenyl-3-aminopropyltrimethoxysilane, N- (vinylbenzyl) -2-aminoethyl-3-aminopropyltrimethoxysilane hydrochloride, and the like.
アクリロキシ基を有するシランカップリング剤としては、３−アクリロキシプロピルトリメトキシシラン等が挙げられる。 Examples of the silane coupling agent having an acryloxy group include 3-acryloxypropyltrimethoxysilane.
メタクリロキシ基を有するシランカップリング剤としては、３−メタクリロキシプロピルトリメトキシシラン、３−メタクリロキシプロピルトリエトキシシラン、３−メタクリロキシプロピルメチルジメトキシシラン、３−メタクリロキシプロピルメチルジエトキシシラン等が挙げられる。 Examples of the silane coupling agent having a methacryloxy group include 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropyltriethoxysilane, 3-methacryloxypropylmethyldimethoxysilane, and 3-methacryloxypropylmethyldiethoxysilane. It is done.
ビニル基を有するシランカップリング剤としては、ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリクロルシラン等が挙げられる。 Examples of the silane coupling agent having a vinyl group include vinyltrimethoxysilane, vinyltriethoxysilane, and vinyltrichlorosilane.
その他、３−ウレイドプロピルトリエトキシシランなどのウレイド基を有するシランカップリング剤、３−メルカプトプロピルトリメトキシシランなどのメルカプト基を有するシランカップリング剤、３−イソシアネートプロピルトリエトキシシランなどのイソシアネート基を有するシランカップリング剤なども使用できる。 In addition, silane coupling agents having a ureido group such as 3-ureidopropyltriethoxysilane, silane coupling agents having a mercapto group such as 3-mercaptopropyltrimethoxysilane, and isocyanate groups such as 3-isocyanatopropyltriethoxysilane. The silane coupling agent which has can also be used.
適切な被覆量は、下地導体層の種類及び樹脂の種類などに応じて適宜調整可能である。 The appropriate coating amount can be appropriately adjusted according to the type of the underlying conductor layer and the type of resin.
このシランカップリング剤皮膜の形成状態と、銅及び／又は銅合金と絶縁樹脂とのピール強度には相関関係がある。特に、高温、高湿度の条件下ではピール強度は低下傾向にあるが、シランカップリング剤皮膜が適切に形成されている場合、すなわち、均一に欠損部分なくシランカップリング剤皮膜が金属表面に形成されている場合には、ピール強度が高く維持できる。ピール強度との関係で好ましい被覆量は、例えば日本電子社製ＪＰＳ−９０１０ＭＣで、Ｍｇ線源、エネルギーステップ０．１ｅＶ、パスエネルギー５０ｅＶ、積算時間２００ｍｓの測定条件でＳｉ 2p3/2 ピークを測定した場合、ピーク強度が１５，０００以上、より好ましくは２０，０００以上のピーク強度である。
（２）金属、金属酸化物、合金など導体層
本発明の分析方法で分析可能なシランカップリング剤皮膜を形成する導体下地としては、例えば、銅、ニッケル、亜鉛、チタン及びこれらの合金などが挙げられるが、この中でも、プリント回路基板の導体層に用いられる銅及び／又は銅合金上にシランカップリング剤皮膜を形成した場合の分析として本発明は適している。
There is a correlation between the formation state of the silane coupling agent film and the peel strength between copper and / or a copper alloy and the insulating resin. In particular, the peel strength tends to decrease under conditions of high temperature and high humidity, but when the silane coupling agent film is properly formed, that is, the silane coupling agent film is uniformly formed on the metal surface without any defects. If it is, the peel strength can be kept high. A preferable coating amount in relation to the peel strength is, for example, JPS-9010MC manufactured by JEOL Ltd., and a Si 2p3 / 2 peak was measured under the measurement conditions of Mg source, energy step 0.1 eV, pass energy 50 eV, and integration time 200 ms. In this case, the peak intensity is 15,000 or more, more preferably 20,000 or more.
(2) Conductor layers such as metals, metal oxides, and alloys Examples of the conductor base for forming a silane coupling agent film that can be analyzed by the analysis method of the present invention include copper, nickel, zinc, titanium, and alloys thereof. Among them, among these, the present invention is suitable as an analysis when a silane coupling agent film is formed on copper and / or a copper alloy used for a conductor layer of a printed circuit board.
また、導体表面には、樹脂との密着性を向上させるために、バフ研磨などの機械的粗化や、エッチング液などによる化学的粗化処理や、その他密着性を向上させるために浸漬めっきによる接着性金属層が形成されていてもよい。要は、酸塩基指示薬によって呈色反応が生じる表面を有する導体層であればよい。
（３）酸塩基指示薬
本発明で使用される酸塩基指示薬は、特に限定されるものではなく、ブロモフェノールブルー、メチルオレンジ、メチルイエロー、ブロモクレゾールグリーン、メチルレッド、リトマス、メチルパープル、ブロモクレゾールパープル、クロロフェノールレッド、ブロモチモールブルー、Ｐ−ニトロフェノールなどが挙げられる。
Also, on the conductor surface, mechanical roughening such as buffing to improve adhesion to the resin, chemical roughening treatment with an etching solution, etc., and immersion plating to improve other adhesion An adhesive metal layer may be formed. In short, any conductor layer having a surface that causes a color reaction by an acid-base indicator may be used.
(3) acid-base indicator ph indicator used in the present invention is not limited in particular, bromophenol blue, methyl orange, methyl yellow, bromocresol green, methyl red, litmus, methyl purple, bromocresol purple Chlorophenol red, bromothymol blue, P-nitrophenol, and the like.
本発明は、導体表面の酸塩基性及びシランカップリング剤皮膜の酸塩基性に基づく酸塩基指示薬の呈色反応によるものである。酸塩基指示薬は対象の酸塩基性によって示す色が変化するので、例えば銅、ニッケル、アルミなど、又はこれらの合金表面と、シランカップリング剤皮膜表面に付着した場合では、酸塩基指示薬の呈色に違いがでるため、目視によって簡単に分析ができる。金属など導体表面にシランカップリング剤皮膜が均一且つ十分に形成されていれば、シランカップリング剤皮膜の特性に由来する呈色を示す。一方、シランカップリング剤皮膜が十分に形成されていなければ、下地の導体表面が露出していることになるため、導体表面特性に由来する呈色を示す。すなわち、金属表面の酸塩基性とシランカップリング剤皮膜の酸塩基性が異なれば、その酸塩基性の相違点に適した変色域を持つ酸塩基指示薬を選択することにより、シランカップリング剤皮膜の存在及び被覆状態を分析することができる。
The present invention is based on the color reaction of an acid-base indicator based on the acid-basicity of the conductor surface and the acid-basicity of the silane coupling agent film. Since the color of the acid-base indicator changes depending on the acid-basicity of the target, for example, when it adheres to the surface of copper, nickel, aluminum, or an alloy thereof and the surface of the silane coupling agent film, the color of the acid-base indicator Because of the difference, it is easy to analyze visually. If the silane coupling agent film is uniformly and sufficiently formed on the surface of a conductor such as metal, a color derived from the characteristics of the silane coupling agent film is exhibited. On the other hand, if the silane coupling agent film is not sufficiently formed, the underlying conductor surface is exposed, and thus coloration derived from the conductor surface characteristics is exhibited. That is, if the acid-basicity of the metal surface is different from the acid-basicity of the silane coupling agent film, the silane coupling agent film is selected by selecting an acid-base indicator having a color change range suitable for the difference in acid-basicity. Presence and coverage can be analyzed.
この酸塩基指示薬のなかでも、特にプリント回路基板の導体として多く使用される銅及び／又は銅合金に適している酸塩基指示薬としては、変色ｐＨ域が２．５〜６．５の範囲にある酸塩基指示薬が、変色が明確に認識できるため分析が容易であり、特に適している。
Among these acid-base indicators , particularly as an acid-base indicator suitable for copper and / or copper alloys that are often used as conductors for printed circuit boards, the discoloration pH range is in the range of 2.5 to 6.5. Acid-base indicators are particularly suitable because they can clearly recognize discoloration and are easy to analyze.
例えば、ブロモフェノールブルー、メチルオレンジ、メチルイエロー、ブロモクレゾールグリーン、メチルレッド、及びこれらの混合液などが挙げられる。 Examples thereof include bromophenol blue, methyl orange, methyl yellow, bromocresol green, methyl red, and a mixed solution thereof.
なお、ブロモフェノールブルーは、銅及び／又は銅合金表面に付着した場合には青色を示し、シランカップリング剤皮膜に付着した場合には黄色を示す。 Note that bromophenol blue shows blue when attached to the copper and / or copper alloy surface, and yellow when attached to the silane coupling agent film.
ブロモクレゾールグリーン／メチルレッド又はブロモクレゾールグリーン／メチルイエローの混合液は、銅及び／又は銅合金表面に付着した場合には緑色を示し、シランカップリング剤皮膜に付着した場合には赤色を示す。 The mixed liquid of bromocresol green / methyl red or bromocresol green / methyl yellow shows green when attached to the copper and / or copper alloy surface, and red when attached to the silane coupling agent film.
酸塩基指示薬の濃度は、０．０１ｗｔ％〜５．０ｗｔ％が好ましく、さらに好ましくは０．０４ｗｔ％〜１．０ｗｔ％、特に好ましくは０．０５ｗｔ％〜０．５ｗｔ％である。この範囲より指示薬濃度が低いと目視での呈色反応が困難となり、また濃度が高すぎても指示薬自体の酸塩基性の影響が大きく呈色反応を観察することが困難となる。
The concentration of the acid-base indicator is preferably 0.01 wt% to 5.0 wt%, more preferably 0.04 wt% to 1.0 wt%, and particularly preferably 0.05 wt% to 0.5 wt%. If the concentration of the indicator is lower than this range, the color reaction by visual observation becomes difficult, and if the concentration is too high, the influence of the acid basicity of the indicator itself is great and it is difficult to observe the color reaction.
以下実施例を用いて本発明をさらに具体的に説明する。なお、本発明は下記の実施例に限定されない。 Hereinafter, the present invention will be described more specifically with reference to examples. In addition, this invention is not limited to the following Example.
（実施例１）
厚さ３５μｍの電解銅箔（プリント配線板用電解銅箔、三井金属鉱業社製商品名“３ＥＣ−ＩＩＩ”）を縦横各１０ｃｍの正方形に切断し、硫酸−過酸化水素系のエッチング液で常温２５℃、３０秒間浸漬処理をして表面を洗浄し、水洗、乾燥させた。次に、シランカップリング剤処理として、３−グリシドキシプロピルトリメトキシシラン１ｗｔ％水溶液で３０℃、６０秒浸漬処理した。
Example 1
Cut an electrolytic copper foil with a thickness of 35 μm (electrolytic copper foil for printed wiring boards, trade name “3EC-III”, manufactured by Mitsui Kinzoku Mining Co., Ltd.) into squares 10 cm in length and breadth, and use a sulfuric acid-hydrogen peroxide etching solution at room temperature. The surface was washed by immersion treatment at 25 ° C. for 30 seconds, washed with water and dried. Next, as a silane coupling agent treatment, immersion treatment was performed at 30 ° C. for 60 seconds with a 1 wt% 3-glycidoxypropyltrimethoxysilane aqueous solution.
（実施例２）
シランカップリング剤処理をする前に、銅箔の表面処理として有機酸系のエッチング剤（メック社製商品名“メックエッチボンド”）で１μｍエッチング処理を行う以外は実施例１と同様に処理した。
(Example 2)
Before the silane coupling agent treatment, the same treatment as in Example 1 was conducted except that a 1 μm etching treatment was performed with an organic acid-based etching agent (trade name “Meck Etch Bond” manufactured by MEC) as a surface treatment of the copper foil. .
（実施例３）
上記実施例２のエッチング処理の代わりに、上記銅箔の表面に表面処理として、浸漬めっきによる接着性金属層を形成したものを実施例３とした。この浸漬めっき液としては、酢酸、酢酸第一スズ、酢酸銀、チオ尿素、ジエチレングリコール、イオン交換水などからなる水溶液を使用して、これに３０℃、３０秒間の条件で浸漬した後、水洗することで、銅箔表面に銅とわずかな錫を含む銅合金層が形成された。
(Example 3)
Instead of the etching treatment of Example 2, Example 3 was obtained by forming an adhesive metal layer by immersion plating on the surface of the copper foil as a surface treatment. As this immersion plating solution, an aqueous solution composed of acetic acid, stannous acetate, silver acetate, thiourea, diethylene glycol, ion-exchanged water, and the like is used. After immersion in this at 30 ° C. for 30 seconds, it is washed with water. Thus, a copper alloy layer containing copper and a slight amount of tin was formed on the surface of the copper foil.
（実施例４）
実施例３のシランカップリング剤処理を、３−グリシドキシプロピルトリメトキシシラン０．５ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを実施例４とした。
Example 4
Example 4 was obtained by immersing the silane coupling agent treatment of Example 3 with a 0.5 wt% aqueous solution of 3-glycidoxypropyltrimethoxysilane at 30 ° C. for 60 seconds.
（実施例５）
実施例３のシランカップリング剤処理を、３−グリシドキシプロピルトリメトキシシラン２．０ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを実施例５とした。
(Example 5)
Example 5 was obtained by immersing the silane coupling agent treatment of Example 3 with a 2.0 wt% 3-glycidoxypropyltrimethoxysilane aqueous solution at 30 ° C. for 60 seconds.
（実施例６）
実施例３のシランカップリング剤処理を、３−グリシドキシプロピルトリメトキシシラン１０．０ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを実施例６とした。
(Example 6)
Example 6 was obtained by immersing the silane coupling agent treatment of Example 3 with a 10.0 wt% aqueous solution of 3-glycidoxypropyltrimethoxysilane at 30 ° C. for 60 seconds.
（実施例７）
実施例３のシランカップリング剤処理を、３−アクリロキシプロピルトリメトキシシラン１ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを実施例７とした。
(Example 7)
Example 7 was obtained by immersing the silane coupling agent treatment of Example 3 with a 1 wt% 3-acryloxypropyltrimethoxysilane aqueous solution at 30 ° C. for 60 seconds.
（実施例８）
実施例３のシランカップリング剤処理を、ビニルトリメトキシシラン１ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを実施例８とした。
(Example 8)
Example 8 was obtained by immersing the silane coupling agent treatment of Example 3 with a 1 wt% vinyltrimethoxysilane aqueous solution at 30 ° C. for 60 seconds.
（実施例９）
実施例３のシランカップリング剤処理を、３−メタクリロキシプロピルトリメトキシシラン１ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを実施例９とした。
Example 9
Example 9 was obtained by immersing the silane coupling agent treatment of Example 3 with a 1 wt% 3-methacryloxypropyltrimethoxysilane aqueous solution at 30 ° C. for 60 seconds.
（実施例１０）
実施例３のシランカップリング剤処理を、３−アミノプロピルトリメトキシシラン１ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを実施例１０とした。
(Example 10)
Example 10 was obtained by immersing the silane coupling agent treatment of Example 3 with a 1 wt% 3-aminopropyltrimethoxysilane aqueous solution at 30 ° C. for 60 seconds.
上記実施例１〜１０に示すシランカップリング剤処理銅箔の表面に、０．１ｗｔ％ブロモフェノールブルーを数滴滴下し、数秒から１分間放置し、指示薬の変色を観察した。 A few drops of 0.1 wt% bromophenol blue were dropped on the surface of the copper foil treated with the silane coupling agent shown in Examples 1 to 10 and allowed to stand for a few seconds to 1 minute, and the discoloration of the indicator was observed.
（実施例１１）
実施例３と同様の銅箔に、０．１ｗｔ％ブロモクレゾールグリーン／メチルレッドを数滴滴下し、数秒から１分間放置し、指示薬の変色を観察したものを実施例１１とした。
(Example 11)
Example 11 was obtained by dropping several drops of 0.1 wt% bromocresol green / methyl red on the same copper foil as in Example 3 and allowing it to stand for a few seconds to 1 minute and observing the discoloration of the indicator.
（実施例１２）
実施例３と同様の銅箔に、０．１ｗｔ％ブロモクレゾールグリーン／メチルイエローを数滴滴下し、数秒から１分間放置し、指示薬の変色を観察したものを実施例１２とした。
(Example 12)
A few drops of 0.1 wt% bromocresol green / methyl yellow were dropped on the same copper foil as in Example 3, and left for a few seconds to 1 minute, and the color change of the indicator was observed as Example 12.
（比較例１）
実施例１と同様の銅箔にシランカップリング剤処理をしなかったものを比較例１とした。
(Comparative Example 1)
The same copper foil as in Example 1 was not treated with the silane coupling agent, and was designated as Comparative Example 1.
（比較例２）
実施例２と同様の銅箔にシランカップリング剤処理をしなかったものを比較例２とした。
(Comparative Example 2)
The same copper foil as in Example 2 was not treated with a silane coupling agent, and was designated as Comparative Example 2.
（比較例３）
実施例３と同様の銅箔にシランカップリング剤処理をしなかったものを比較例３とした。
(Comparative Example 3)
The same copper foil as in Example 3 was not treated with the silane coupling agent, and was designated as Comparative Example 3.
（比較例４）
実施例３のシランカップリング剤処理を、３−グリシドキシプロピルトリメトキシシラン０．２ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを比較例４とした。
(Comparative Example 4)
Comparative Example 4 was obtained by immersing the silane coupling agent in Example 3 with a 0.2 wt% aqueous solution of 3-glycidoxypropyltrimethoxysilane at 30 ° C. for 60 seconds.
（比較例５）
実施例３のシランカップリング剤処理を、３−グリシドキシプロピルトリメトキシシラン０．１ｗｔ％水溶液で３０℃、６０秒浸漬処理したものを比較例５とした。
(Comparative Example 5)
Comparative Example 5 was obtained by subjecting the silane coupling agent treatment of Example 3 to immersion treatment at 30 ° C. for 60 seconds with a 0.1 wt% 3-glycidoxypropyltrimethoxysilane aqueous solution.
上記比較例１〜比較例５の銅箔の表面に、０．１ｗｔ％ブロモフェノールブルーを数滴滴下し、数秒から１分間放置し、指示薬の変色を観察した。 A few drops of 0.1 wt% bromophenol blue were dropped on the surface of the copper foils of Comparative Examples 1 to 5, and left for a few seconds to 1 minute, and the discoloration of the indicator was observed.
（比較例６）
実施例１１のシランカップリング剤処理をしなかったものを比較例６とした。
(Comparative Example 6)
The product of Example 11 that was not treated with the silane coupling agent was referred to as Comparative Example 6.
（比較例７）
実施例１２のシランカップリング剤処理をしなかったものを比較例７とした。
(Comparative Example 7)
The product of Example 12 that was not treated with the silane coupling agent was referred to as Comparative Example 7.
また、実施例のうち、実施例１〜１２及びシランカップリング剤処理をした比較例４及び５の表面をＸＰＳで測定したところ（測定条件：日本電子社製ＪＰＳ−９０１０ＭＣ、Ｍｇ線源、エネルギーステップ０．１ｅＶ、パスエネルギー５０ｅＶ、積算時間２００ｍｓの測定条件でＳｉ 2p3/2 ピークを測定した）実施例１〜１２はいずれもシランカップリング剤皮膜が十分に形成されていることがわかった。 Moreover, when the surface of Examples 1-12 and Comparative Examples 4 and 5 treated with a silane coupling agent was measured by XPS among the examples (measurement conditions: JPS-9010MC manufactured by JEOL Ltd., Mg source, energy The Si 2p3 / 2 peak was measured under the measurement conditions of step 0.1 eV, pass energy 50 eV, and integration time 200 ms). In each of Examples 1 to 12, it was found that the silane coupling agent film was sufficiently formed.
一方、比較例４及び５については、それぞれシランカップリング剤皮膜が十分に形成されていないことがわかった。 On the other hand, in Comparative Examples 4 and 5, it was found that the silane coupling agent film was not sufficiently formed.
なお、シランカップリング剤皮膜付着状態の評価は、ピーク強度が２０，０００以上であれば○、未満であれば×とした。 In addition, evaluation of the adhesion state of the silane coupling agent film was evaluated as “good” when the peak intensity was 20,000 or more, and “x” when the peak intensity was less.
上記結果を表１に示す。 The results are shown in Table 1.
これらの結果より、シランカップリング剤皮膜の有無及び被覆状態は、指示薬の変色によって簡単に判別できることがわかる。 From these results, it can be seen that the presence or absence of the silane coupling agent film and the covering state can be easily discriminated by the discoloration of the indicator.
以上から、本発明は、銅及び／又は銅合金などの導体表面に形成されているシランカップリング剤皮膜上に酸塩基指示薬を滴下し、変色を確認することで簡単にシランカップリング剤皮膜の有無、及び被覆状態を分析することができる。このため、高価な装置やそれを扱う熟練が不要で、特にプリント回路基板などを製造する現場でのシランカップリング剤皮膜分析に好適であることが確認できた。 From the above, the present invention simply drops an acid-base indicator on a silane coupling agent film formed on the surface of a conductor such as copper and / or a copper alloy, and confirms the discoloration, thereby easily changing the silane coupling agent film. Presence / absence and covering state can be analyzed. For this reason, an expensive apparatus and the skill to handle it are unnecessary, and it has been confirmed that it is particularly suitable for silane coupling agent film analysis in the field of manufacturing printed circuit boards and the like.
Claims (7)
前記シランカップリング剤皮膜上に酸塩基指示薬を含む指示液を滴下し、その変色を確認することでシランカップリング剤皮膜の有無、及び被覆状態を分析することを特徴とするシランカップリング剤皮膜の分析方法。 A method for analyzing a silane coupling agent film formed on a conductor surface,
A silane coupling agent film characterized in that an indicator solution containing an acid-base indicator is dropped on the silane coupling agent film, and the presence or absence of the silane coupling agent film and the coating state are analyzed by confirming the color change. Analysis method.
前記プリント回路基板に、酸塩基指示薬液を滴下し、変色を確認することで導体層と樹脂層の密着性を分析することを特徴とする導体層と樹脂層との密着性の分析方法。 A method for analyzing adhesion in a printed circuit board in which a silane coupling agent is applied to a conductor surface in order to improve adhesion between at least one conductor layer selected from metal, metal oxide, and alloy and a resin layer. ,
Wherein the printed circuit board, was added dropwise an acid-base indicator solution, the method analyzes the adhesion between the conductor layer and the resin layer, characterized in that analyzing the adhesion of the conductive layer and the resin layer by checking the color change.
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