TWI386520B - Copper surface treatment agent and surface treatment method - Google Patents
Copper surface treatment agent and surface treatment method Download PDFInfo
- Publication number
- TWI386520B TWI386520B TW097121077A TW97121077A TWI386520B TW I386520 B TWI386520 B TW I386520B TW 097121077 A TW097121077 A TW 097121077A TW 97121077 A TW97121077 A TW 97121077A TW I386520 B TWI386520 B TW I386520B
- Authority
- TW
- Taiwan
- Prior art keywords
- surface treatment
- benzimidazole
- acid
- copper
- melting point
- Prior art date
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims description 54
- 239000010949 copper Substances 0.000 title claims description 48
- 229910052802 copper Inorganic materials 0.000 title claims description 47
- 239000012756 surface treatment agent Substances 0.000 title claims description 31
- 238000000034 method Methods 0.000 title claims description 11
- 238000004381 surface treatment Methods 0.000 title claims description 6
- -1 benzimidazole compound Chemical class 0.000 claims description 51
- 238000002844 melting Methods 0.000 claims description 40
- 230000008018 melting Effects 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 150000001556 benzimidazoles Chemical class 0.000 claims description 15
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 8
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 150000003536 tetrazoles Chemical class 0.000 claims description 4
- 150000003852 triazoles Chemical class 0.000 claims description 4
- 238000005476 soldering Methods 0.000 description 17
- 239000000463 material Substances 0.000 description 14
- 238000002474 experimental method Methods 0.000 description 12
- 229910000679 solder Inorganic materials 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 239000011889 copper foil Substances 0.000 description 7
- 150000003851 azoles Chemical class 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 5
- 150000007524 organic acids Chemical class 0.000 description 5
- 238000003466 welding Methods 0.000 description 5
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 150000002460 imidazoles Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 3
- KLSJWNVTNUYHDU-UHFFFAOYSA-N Amitrole Chemical compound NC1=NC=NN1 KLSJWNVTNUYHDU-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 235000011054 acetic acid Nutrition 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 235000019253 formic acid Nutrition 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- OXFSTTJBVAAALW-UHFFFAOYSA-N 1,3-dihydroimidazole-2-thione Chemical compound SC1=NC=CN1 OXFSTTJBVAAALW-UHFFFAOYSA-N 0.000 description 2
- VJRPHCDQRJAVSR-UHFFFAOYSA-N 2-(naphthalen-1-ylmethyl)-1h-benzimidazole Chemical compound C1=CC=C2C(CC=3NC4=CC=CC=C4N=3)=CC=CC2=C1 VJRPHCDQRJAVSR-UHFFFAOYSA-N 0.000 description 2
- GEQBRULPNIVQPP-UHFFFAOYSA-N 2-[3,5-bis(1-phenylbenzimidazol-2-yl)phenyl]-1-phenylbenzimidazole Chemical compound C1=CC=CC=C1N1C2=CC=CC=C2N=C1C1=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=C1 GEQBRULPNIVQPP-UHFFFAOYSA-N 0.000 description 2
- VSMPBJCKGWINIB-UHFFFAOYSA-N 2-heptan-3-yl-1h-benzimidazole Chemical compound C1=CC=C2NC(C(CC)CCCC)=NC2=C1 VSMPBJCKGWINIB-UHFFFAOYSA-N 0.000 description 2
- QLXNYVPEFIFJIA-UHFFFAOYSA-N 2-pentan-3-yl-1h-benzimidazole Chemical compound C1=CC=C2NC(C(CC)CC)=NC2=C1 QLXNYVPEFIFJIA-UHFFFAOYSA-N 0.000 description 2
- GFKNPGTWLJFDKJ-UHFFFAOYSA-N 2-undecyl-1h-benzimidazole Chemical compound C1=CC=C2NC(CCCCCCCCCCC)=NC2=C1 GFKNPGTWLJFDKJ-UHFFFAOYSA-N 0.000 description 2
- JQEVCCUJHLRAEY-UHFFFAOYSA-N 5-methyl-2-undecyl-1h-imidazole Chemical compound CCCCCCCCCCCC1=NC=C(C)N1 JQEVCCUJHLRAEY-UHFFFAOYSA-N 0.000 description 2
- CLATUPQFGKDFSR-UHFFFAOYSA-N 6-chloro-2-octyl-1h-benzimidazole Chemical compound C1=C(Cl)C=C2NC(CCCCCCCC)=NC2=C1 CLATUPQFGKDFSR-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000001273 butane Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003623 enhancer Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- RBNPOMFGQQGHHO-UHFFFAOYSA-N -2,3-Dihydroxypropanoic acid Natural products OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 description 1
- FMCUPJKTGNBGEC-UHFFFAOYSA-N 1,2,4-triazol-4-amine Chemical compound NN1C=NN=C1 FMCUPJKTGNBGEC-UHFFFAOYSA-N 0.000 description 1
- GYFLDXSJACJFSG-UHFFFAOYSA-N 1-(1H-benzimidazol-2-yl)cyclohexa-2,4-dien-1-amine Chemical compound NC1(CC=CC=C1)C=1NC2=C(N1)C=CC=C2 GYFLDXSJACJFSG-UHFFFAOYSA-N 0.000 description 1
- KJUGUADJHNHALS-UHFFFAOYSA-N 1H-tetrazole Substances C=1N=NNN=1 KJUGUADJHNHALS-UHFFFAOYSA-N 0.000 description 1
- LIGZUQZUEDNPGG-UHFFFAOYSA-N 2-(1h-benzimidazol-2-yl)benzoic acid Chemical compound OC(=O)C1=CC=CC=C1C1=NC2=CC=CC=C2N1 LIGZUQZUEDNPGG-UHFFFAOYSA-N 0.000 description 1
- OILIYWFQRJOPAI-UHFFFAOYSA-N 2-(2-chlorophenyl)-1h-benzimidazole Chemical compound ClC1=CC=CC=C1C1=NC2=CC=CC=C2N1 OILIYWFQRJOPAI-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- XBXVUKKKEYEPTR-UHFFFAOYSA-N 2-(2-methylphenyl)-1h-benzimidazole Chemical compound CC1=CC=CC=C1C1=NC2=CC=CC=C2N1 XBXVUKKKEYEPTR-UHFFFAOYSA-N 0.000 description 1
- ZGHVPBISEIPFJS-UHFFFAOYSA-N 2-(tetrazol-1-yl)ethanamine Chemical compound NCCN1C=NN=N1 ZGHVPBISEIPFJS-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- SLLDUURXGMDOCY-UHFFFAOYSA-N 2-butyl-1h-imidazole Chemical compound CCCCC1=NC=CN1 SLLDUURXGMDOCY-UHFFFAOYSA-N 0.000 description 1
- QGFGLYOMJKJZIC-UHFFFAOYSA-N 2-dodecyl-1h-benzimidazole Chemical compound C1=CC=C2NC(CCCCCCCCCCCC)=NC2=C1 QGFGLYOMJKJZIC-UHFFFAOYSA-N 0.000 description 1
- PQAMFDRRWURCFQ-UHFFFAOYSA-N 2-ethyl-1h-imidazole Chemical compound CCC1=NC=CN1 PQAMFDRRWURCFQ-UHFFFAOYSA-N 0.000 description 1
- DAPXOJOQSNBLKY-UHFFFAOYSA-N 2-hexyl-1h-imidazole Chemical compound CCCCCCC1=NC=CN1 DAPXOJOQSNBLKY-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- MMDFSEGJGPURPF-UHFFFAOYSA-N 2-octyl-1h-imidazole Chemical compound CCCCCCCCC1=NC=CN1 MMDFSEGJGPURPF-UHFFFAOYSA-N 0.000 description 1
- OYGJENONTDCXGW-UHFFFAOYSA-N 2-pentyl-1h-benzimidazole Chemical compound C1=CC=C2NC(CCCCC)=NC2=C1 OYGJENONTDCXGW-UHFFFAOYSA-N 0.000 description 1
- MKBBSFGKFMQPPC-UHFFFAOYSA-N 2-propyl-1h-imidazole Chemical compound CCCC1=NC=CN1 MKBBSFGKFMQPPC-UHFFFAOYSA-N 0.000 description 1
- IRPJFDNQCGTROV-UHFFFAOYSA-N 2-tetradecyl-1h-benzimidazole Chemical compound C1=CC=C2NC(CCCCCCCCCCCCCC)=NC2=C1 IRPJFDNQCGTROV-UHFFFAOYSA-N 0.000 description 1
- OZRZZNNKEBHRGQ-UHFFFAOYSA-N 2-tridecyl-1h-benzimidazole Chemical compound C1=CC=C2NC(CCCCCCCCCCCCC)=NC2=C1 OZRZZNNKEBHRGQ-UHFFFAOYSA-N 0.000 description 1
- LLEASVZEQBICSN-UHFFFAOYSA-N 2-undecyl-1h-imidazole Chemical compound CCCCCCCCCCCC1=NC=CN1 LLEASVZEQBICSN-UHFFFAOYSA-N 0.000 description 1
- ULRPISSMEBPJLN-UHFFFAOYSA-N 2h-tetrazol-5-amine Chemical compound NC1=NN=NN1 ULRPISSMEBPJLN-UHFFFAOYSA-N 0.000 description 1
- HLHNOIAOWQFNGW-UHFFFAOYSA-N 3-bromo-4-hydroxybenzonitrile Chemical compound OC1=CC=C(C#N)C=C1Br HLHNOIAOWQFNGW-UHFFFAOYSA-N 0.000 description 1
- SMTGVJNPFRLURH-UHFFFAOYSA-N 4-ethyltriazol-1-amine Chemical compound CCC1=CN(N)N=N1 SMTGVJNPFRLURH-UHFFFAOYSA-N 0.000 description 1
- SJZRECIVHVDYJC-UHFFFAOYSA-N 4-hydroxybutyric acid Chemical compound OCCCC(O)=O SJZRECIVHVDYJC-UHFFFAOYSA-N 0.000 description 1
- AWQSAIIDOMEEOD-UHFFFAOYSA-N 5,5-Dimethyl-4-(3-oxobutyl)dihydro-2(3H)-furanone Chemical compound CC(=O)CCC1CC(=O)OC1(C)C AWQSAIIDOMEEOD-UHFFFAOYSA-N 0.000 description 1
- KYRMPMCAOPMOIR-UHFFFAOYSA-N 5-ethyl-2h-tetrazole Chemical compound CCC=1N=NNN=1 KYRMPMCAOPMOIR-UHFFFAOYSA-N 0.000 description 1
- XZGLNCKSNVGDNX-UHFFFAOYSA-N 5-methyl-2h-tetrazole Chemical compound CC=1N=NNN=1 XZGLNCKSNVGDNX-UHFFFAOYSA-N 0.000 description 1
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-N Caprylic acid Natural products CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- RBNPOMFGQQGHHO-UWTATZPHSA-N D-glyceric acid Chemical compound OC[C@@H](O)C(O)=O RBNPOMFGQQGHHO-UWTATZPHSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- KDPAWGWELVVRCH-UHFFFAOYSA-N bromoacetic acid Chemical compound OC(=O)CBr KDPAWGWELVVRCH-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- YTIVTFGABIZHHX-UHFFFAOYSA-N butynedioic acid Chemical compound OC(=O)C#CC(O)=O YTIVTFGABIZHHX-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- XWXMGTIHBYFTIE-UHFFFAOYSA-N chembl203360 Chemical compound OC1=CC=CC=C1C1=NC2=CC=CC=C2N1 XWXMGTIHBYFTIE-UHFFFAOYSA-N 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- PKWIYNIDEDLDCJ-UHFFFAOYSA-N guanazole Chemical compound NC1=NNC(N)=N1 PKWIYNIDEDLDCJ-UHFFFAOYSA-N 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Classifications
-
- 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/52—Treatment of copper or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
-
- C—CHEMISTRY; METALLURGY
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Description
本發明係關於銅表面處理劑及使用其之表面處理方法。
銅之表面處理劑其使用目的係為了例如防鏽或焊接性提升等而於形成配線之銅表面形成皮膜。上述表面處理劑已知有含有咪唑合物(為所形成之皮膜的主成分)者。例如,專利文獻1中係揭示併用2位烷基苯并咪唑化合物(2-alkylbenzimidasole compound)與有機酸。專利文獻2~4中係揭示含有咪唑化合物之表面處理劑。專利文獻5中係揭示含有咪唑系化合物之預焊劑之使用方法。專利文獻6係揭示了含有4,4-亞甲基-雙-(2-十一基-5-甲基咪唑)與2-十一基-4-甲基咪唑之二種咪唑化合物之銅表面處理劑。專利文獻7係揭示了含有2-烷基-4-甲基苯并咪唑7合物與2-烷基-5-甲基苯并咪唑化合物之二種苯并咪唑化合物之銅表面處理劑。
此種銅表面處理劑所形成之防鏽皮膜必須是即使於高溫下經反覆回流焊接(reflow)後亦安定者。又,雖亦必須維持焊接性,但以往之銅表面處理劑係難以滿足耐熱性與焊接性兩者。
專利文獻1:日本專利特開平4-80375號公報
專利文獻2:日本專利特開平5-25407號公報專利文獻3:日本專利特開平5-186888號公報專利文獻4:日本專利特開平7-54169號公報專利文獻5:日本專利特開平5-186880號公報專利文獻6:日本專利特開昭61-23775號公報專利文獻7:日本專利特開平4-99285號公報
本發明為了解決上述以往之問題而提供一種可滿足耐熱性與焊接性兩者之銅表面處理劑及表面處理方法。
本發明之銅表面處理劑,係含有酸、苯并咪唑化合物及水者,其特徵在於:係至少含有第1苯并咪唑化合物、與熔點低於此第1苯并咪唑化合物達70℃以上之第2苯并咪唑化合物作為該苯并咪唑化合物。
其中,上述本發明中之「銅」可為由純銅所構成者,亦可為銅合金所構成者。又,本明細書中「銅」係指純銅或銅合金。
又,本發明之表面處理方法,其特徵在於:係使用上述本發明之銅表面處理劑來處理銅之表面。
本發明為了滿足耐熱性與焊接性兩者而著眼於苯并咪唑化合物。熔點高之苯并咪唑化合物(第1苯并
咪唑化合物)由於熔點高,故於焊接溫度皮膜難以軟化,雖然耐熱性高,但焊接性不良。熔點低之苯并咪唑化合物(第2苯并咪唑化合物)雖然焊接性良好,但焊接時於高溫下之耐熱性低。本發明藉由將上述第1苯并咪唑化合物與上述第2苯并咪唑化合物混合,可滿足耐熱性與焊接性兩者。上述第1苯并咪唑化合物熔點為200℃~300℃較佳,230℃~270℃更佳。又,上述第2苯并咪唑化合物熔點為95℃~130℃較佳,98℃~120℃更佳。
(第1苯并咪唑化合物之例)
第1苯并咪唑化合物之例係如下所示。
2-(1’-乙基丙基)苯并咪唑(EPrBI):熔點265℃、2-(2’-羧基苯基)苯并咪唑:熔點264℃、2-(2’-羥基苯基)苯并咪唑:熔點242℃、2-(1-萘基甲基)苯并咪唑(NMBI):熔點241℃、2-(2’-氯苯基)苯并咪唑:熔點232℃、2-(2’-甲基苯基)苯并咪唑:熔點218℃、2-(1’-胺基苯基)苯并咪唑:熔點214℃、2-(1’-乙基戊基)苯并咪唑(EPeBI):熔點207℃
該等可單獨使用,亦可混合使用。
(第2苯并咪唑化合物之例)
第2苯并咪唑化合物之例係如下所示。
2-壬基苯并咪唑(NBI):熔點127℃、
2-(5’-甲苯基)亞戊基苯并咪唑(TPBI):熔點
121℃、1,4-雙苯并咪唑丁烷(BBIB):熔點120℃、2-癸基苯并咪唑:熔點114℃、2-(5’-茬基)亞戊基苯并咪唑(XPBI):熔點112℃、2-十一基苯并咪唑(UBI):熔點109℃、2-十二基苯并咪唑:熔點109℃、2-十三基苯并咪唑:熔點105℃、5-氯-2-辛基苯并咪唑(COBI):熔點100℃、2-四癸基苯并咪唑:熔點99℃
該等可單獨使用,亦可混合使用。
第1及第2苯并咪唑化合物之合計濃度為0.05重量%~0.4重量%之範圍較佳,0.1重量%~0.3重量%之範圍更佳。苯并咪唑化合物之合計濃度只要為前述範圍,即可易於形成皮膜,亦可滿足溶解性。
第1及第2苯并咪唑化合物之較佳比率較佳為重量比為1:9~9:1之範圍,3:7~7:3之範圍更佳。各苯并咪唑化合物之配合比率若為前述範圍,則可滿足2成分系之優點亦即耐熱性與焊接性。
其中,本發明之銅表面處理劑中含有第1及第2苯并咪唑化合物分別為1種以上即可。又,除了第1及第2苯并咪唑化合物以外亦可再含有其他的苯并咪唑化合物。亦可含有例如熔點為第1及第2苯并咪唑化合物之中間值之第3苯并咪唑化合物。其中,苯并咪唑化合物由於與其他咪唑化合物相比耐熱性優異,
故於焊接時之高溫下皮膜亦難以軟化。
(酸之例)
本發明之銅表面處理劑所含之酸雖可使用有機酸亦可使用無機酸,但由苯并咪唑化合物之溶解性優異且防鏽皮膜之附著性良好之觀點來看尤佳為有機酸。有機酸可舉出:乙酸、甲酸、丙酸、乙醇酸、丁酸、丙烯酸、巴豆酸、草酸、丙二酸、琥珀酸、己二酸、馬來酸、乙炔二羧酸、一氯乙酸、三氯乙酸、一溴乙酸、三溴乙酸、乳酸、羥基酪酸、甘油酸、酒石酸、蘋果酸、檸檬酸、己酸、庚酸等。前述有機酸亦可併用2種以上。例如,混合使用上述乙酸、甲酸、與己酸、庚酸等的情況時,可使苯并咪唑化合物於特別安定之狀態溶解。己酸、庚酸可作為可溶化劑之功能,可使苯并咪唑化合物安定地溶解於乙酸、甲酸與水之混合溶劑中。
本發明之銅表面處理劑,必須使熔點有差異之2種以上的苯并咪唑化合物溶解,該等之苯并咪唑化合物對酸之溶解度各不同,尤其是混合上述列舉之酸來使用更具有效果。
其中,可使用於本發明之銅表面處理劑之無機酸可舉出例如鹽酸、硫酸、硝酸、磷酸等。
該等酸係用以使上述苯并咪唑化合物安定並使之溶解而添加者,較佳之含量因苯并咪唑化合物之種類、使用量等而異,故無法概括規定,但設定成可使
上述苯并咪唑化合物安定溶解於銅表面處理劑中之範圍,通常為1重量%~40重量%之範圍。
本發明之銅表面處理劑較佳為進一步含有苯并咪唑化合物以外之選自咪唑類、三唑類及四唑類之至少1種之唑類。其原因在於由於皮膜之形成速度快,故處理時間可短縮。
上述咪唑類可例示:咪唑、2-甲基咪唑、2-乙基咪唑、2-丙基咪唑、2-丁基咪唑、2-己基咪唑、2-辛基咪唑、2-壬基咪唑、2-癸基咪唑、2-十一基咪唑、2-乙基-4-甲基咪唑、2-十一基-4-甲基咪唑等。上述三唑類可例示:三唑、3-胺基-1,2,4-三唑、3-胺基-5-乙基三唑、4-胺基-1,2,4-三唑、3,5-二胺基-1,2,4-三唑等。上述四唑類可例示:四唑、5-胺基四唑、5-甲基四唑、5-乙基四唑、1-(β-胺乙基)四唑等。該等唑類具有易於吸附於銅表面之性質,且不具有分子量大之基而溶解性良好,故可於短時間於銅表面形成皮膜。其中,由溶解性之觀點來看分子量為250以下之唑類較佳。且由溶解性及皮膜之形成速度的觀點來看,分子量為250以下且具有選自甲基、乙基、及碳數3以上之直鏈烷基之至少一個之取代基之唑類更佳。
本發明之銅表面處理劑含有上述唑類的情況時,上述唑類之濃度除以上述第1及第2苯并咪唑化合物之合計濃度之值為例如0.01~0.10,較佳為0.03~0.10,更佳為0.03~0.07。只要在此範圍內,可以不阻礙耐
熱性與焊接性提升效果之程度,提升皮膜之形成速度。
(其他成分)
除此之外,可適當地添加作為耐熱性提升劑之鋅或含有鋅之化合物、作為焊接性提升劑之溴化物或溴化合物、作為皮膜形成至銅表面之促進劑之銅或銅化合物等。該等成分之含量為例如0.01重量%~2.0重量%左右。
本發明之銅表面處理劑可藉由使上述苯并咪唑化合物等溶解於酸與水之混合溶劑而容易地調製。上述水較佳為除去離子性物質或不純物之水,例如離子交換水、純水、超純水等較佳。
以下,藉由實施例具體說明本發明。
(實驗1)
準備於玻璃環氧基材(日立化成工業製GEA-67N、厚度:1.6mm)之兩面貼附有厚18μm銅箔之雙面銅張積層板(寬:7.8cm、長4.8cm),於此形成0.8mm直徑的通孔160個製作被處理材。
接著,將此被處理材浸漬於美庫布來特CB-801(mec股份有限公司製微蝕劑)將銅箔表面蝕刻1μm並進行水洗後,分別一片一片地浸漬60秒於以下表1所示之組成的實施例1~26及比較例1~4銅表面處理
劑,並進行水洗、乾燥。其中,銅表面處理劑之溫度皆定為30℃。
接著,分別針對乾燥後之被處理材進行2次回流焊接處理。回流焊接處理係使用熱風循環型回流焊接爐,每一次的回流焊接處理係以被處理材表面溫度成為240℃~245℃之溫度加熱40秒。
接著,藉由噴霧將被處理材以後焊劑(post flux)處理。後焊劑係使用朝日化學研究所股份有限公司製之AGF-880。其後,進行回流焊接處理。回流焊接處理中,首先,於被處理材表面溫度成為100℃之溫度進行加熱80秒作為預熱處理後,於焊料溫度成為255℃之條件下進行雙波(double wave)處理。此時,使用之焊料重量比(Sn:Ag:Cu)為96.5:3:0.5。
其中,本實驗之雙波處理中,使被處理材與焊料接觸2.5秒後,分開2.5秒之間隔,再度使被處理材與焊料接觸3秒進行處理。
然後,分別針對上述被處理材確認焊接不良率。焊接不良率係160個通孔之中,發生焊接不良之通孔的比例。其中,本實驗之焊接不良係指以目視觀察可確認到焊料未完全充填於通孔內的情況。
(實驗2)
準備於玻璃環氧基材(日立化成工業製GEA-67N、厚度:1.6mm)之單面貼附有厚18μm銅箔之單面銅張積層板,於此形成40個0.3mm×8mm之方形導體
圖案製作被處理材。接著,將此被處理材浸漬於美庫布來特CB-801(mec股份有限公司製微蝕劑)將銅箔表面蝕刻1μm並進行水洗後,分別一片一片地浸漬60秒於以下表1所示之組成的實施例1~26及比較例1~4銅表面處理劑,並進行水洗、乾燥。其中,銅表面處理劑之溫度皆定為30℃。
其後,於上述導體圖案上之中央部印刷焊接膏(soldercoat公司製TAS650 S10/011/M9.5)。此時,印刷圖案係圓形。
又,各個印刷圖案直徑為0.4mm,厚度為100μm。印刷後,使用與上述實驗1相同之回流焊接爐於被處理材表面溫度成為225℃~230℃之溫度進行加熱40秒。
然後,針對因此回流焊接處而擴大之焊料區域(40處),以顯微鏡分別計測最長之直徑的長度,算出其平均值作為焊料擴大之長度。
(焊接性判定基準)
針對實驗1中焊接不良率為3%以下,且實驗2中焊料擴散長度為2mm以上之調配組合,定為焊接性A。又,針對焊接不良率超過3%且為7%以下,且焊料擴散長度為1mm以上之調配組合,定為焊接性B。又,焊接不良率超過7%者定為焊接性C。結果示於表1。
(實驗3)
準備於玻璃環氧基材(日立化成工業製GEA-67N、厚度:1.6mm)之兩面貼著有厚18μm銅箔之雙面銅張積層板(8cm×8cm)。將此被處理材浸漬於美庫布來特CB-801(mec股份有限公司製微蝕劑)將銅箔表面蝕刻1μm並進行水洗後,分別一片一片地浸漬60秒於以下表1所示之組成的實施例1~26及比較例1~4銅表面處理劑,並進行水洗、乾燥。其中,銅表面處理劑之溫度皆定為30℃。接著,分別針對乾燥後之被處理材進行2次回流焊接處理。回流焊接處理係使用與上述實驗1相同之回流焊接爐,每一次的回流焊接處理係以被處理材表面溫度成為240℃~245℃之溫度加熱40秒。
(耐熱性判定基準)
以目視確認實驗3之結果、有無變色,並將幾乎沒有變色者定為A,稍微變色者定為B,嚴重變色者定為C。結果示於表1。
和上述實驗1相同的方式將被處理材浸漬於實施例1~26及比較例1~4之各銅表面處理劑,並水洗、乾燥後,將此被處理材浸漬於鹽酸(氯化氫為35重量%)與甲醇之混合液25mL(重量比為鹽酸:甲醇=0.5:99.5)5分鐘,使附著於銅箔上之皮膜成分溶解於上述混合液中。然後,將溶解有皮膜成分之上述混合
液進行取樣,以紫外可見分光光度計(島津製作所製UV-1600),測定位於278nm附近之第1及第2苯并咪唑化合物之峰值的吸光度,將此值作為皮膜量。結果示於表1。
(備註)
實施例1~26及比較例1~4之其餘部份皆為離子交換水。又,表1中各成分括號內的數值皆表示重量百分比濃度。其中,表1中苯并咪唑化合物之正式名稱及熔點如下:EPrBI:2-(1’-乙基丙基)苯并咪唑、熔點265℃ NMBI:2-(1-萘基甲基)苯并咪唑、熔點241℃ EPeBI:2-(1’-乙基戊基)苯并咪唑、熔點207℃ NBI:2-壬基苯并咪唑、熔點127℃ TPBI:2-(5’-甲苯基)亞戊基苯并咪唑、熔點121℃ BBIB:1,4-雙苯并咪唑丁烷、熔點120℃ XPBI:2-(5’-茬基)亞戊基苯并咪唑、熔點112℃ UBI:2-十一基苯并咪唑、熔點109℃ COBI:5-氯-2-辛基苯并咪唑、熔點100℃
由表1可明顯確認到藉由併用熔點差異為70℃以上之2種以上苯并咪唑化合物作為苯并咪唑化合物,可滿足耐熱性與焊接性兩者。
(實驗4)
銅表面處理劑之浸漬處理時間定為30秒,除此之外係以與上述相同之方式評估焊接性、耐熱性及皮膜量。結果示於表2。
針對添加苯并咪唑化合物以外的唑類之實施例12~26與其他例來比較皮膜量時,可瞭解到藉由添加既定量以上之上述唑類,皮膜之形成速度會變快。其結果,實施例13、14、16、17、19、20、22、23、25、26,耐熱性及焊接性之至少一者與其他實施例相比獲得良好之結果。
本發明之銅表面處理劑及表面處理方法,藉由併用熔點差異為70℃以上之2種以上苯并咪唑化合物作為苯并咪唑化合物,可滿足耐熱性與焊接性兩者。
Claims (5)
- 一種銅表面處理劑,係含有酸、苯并咪唑化合物及水者,其特徵在於:係至少含有第1苯并咪唑化合物、與熔點低於此第1苯并咪唑化合物達70℃以上之第2苯并咪唑化合物作為該苯并咪唑化合物;且其係進一步含有苯并咪唑化合物以外之選自咪唑類、三唑類及四唑類之至少1種之唑類;且該唑類之濃度除以該第1及第2苯并咪唑化合物之合計濃度之值為0.03~0.10。
- 如申請專利範圍第1項之銅表面處理劑,其中,該第1苯并咪唑化合物熔點為200℃~300℃,且該第2苯并咪唑化合物熔點為95℃~130℃。
- 如申請專利範圍第1項之銅表面處理劑,其中,該第1及第2苯并咪唑化合物之合計濃度為0.05重量%~0.4重量%。
- 如申請專利範圍第1項之銅表面處理劑,其中,該第1苯并咪唑化合物與該第2苯并咪唑化合物之配合比為重量比1:9~9:1。
- 一種表面處理方法,其係用以處理銅表面,其特徵在於:使用申請專利範圍第1至4項中任一項之銅表面處理劑來處理銅之表面。
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JPWO2014156361A1 (ja) * | 2013-03-28 | 2017-02-16 | 古河電気工業株式会社 | 表面処理電解銅箔 |
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JPH0779061A (ja) * | 1993-09-07 | 1995-03-20 | Mec Kk | 銅および銅合金の表面処理剤 |
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JP2005226082A (ja) * | 2004-02-10 | 2005-08-25 | Tamura Kaken Co Ltd | 金属の表面処理剤、プリント回路基板およびプリント回路基板の金属の表面処理方法 |
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JPH11177218A (ja) * | 1997-12-12 | 1999-07-02 | Tamura Kaken Co Ltd | 電子回路用金属面具備部品及びその表面保護剤 |
JP2005226082A (ja) * | 2004-02-10 | 2005-08-25 | Tamura Kaken Co Ltd | 金属の表面処理剤、プリント回路基板およびプリント回路基板の金属の表面処理方法 |
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