JP5033979B1 - Acidic aqueous composition for plating comprising tin - Google Patents
Acidic aqueous composition for plating comprising tin Download PDFInfo
- Publication number
- JP5033979B1 JP5033979B1 JP2011214393A JP2011214393A JP5033979B1 JP 5033979 B1 JP5033979 B1 JP 5033979B1 JP 2011214393 A JP2011214393 A JP 2011214393A JP 2011214393 A JP2011214393 A JP 2011214393A JP 5033979 B1 JP5033979 B1 JP 5033979B1
- Authority
- JP
- Japan
- Prior art keywords
- plating
- group
- tin
- aqueous composition
- acidic aqueous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000007747 plating Methods 0.000 title claims abstract description 118
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 19
- 239000000203 mixture Substances 0.000 title claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 150000003222 pyridines Chemical class 0.000 claims abstract description 8
- 239000002563 ionic surfactant Substances 0.000 claims abstract description 6
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 6
- -1 aromatic carbonyl compound Chemical class 0.000 claims description 14
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 13
- 125000006575 electron-withdrawing group Chemical group 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- 150000005041 phenanthrolines Chemical class 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- BZFGKBQHQJVAHS-UHFFFAOYSA-N 2-(trifluoromethyl)pyridine-4-carboxylic acid Chemical compound OC(=O)C1=CC=NC(C(F)(F)F)=C1 BZFGKBQHQJVAHS-UHFFFAOYSA-N 0.000 claims description 3
- KFDVPJUYSDEJTH-UHFFFAOYSA-N 4-ethenylpyridine Chemical compound C=CC1=CC=NC=C1 KFDVPJUYSDEJTH-UHFFFAOYSA-N 0.000 claims description 3
- TWBYWOBDOCUKOW-UHFFFAOYSA-N isonicotinic acid Natural products OC(=O)C1=CC=NC=C1 TWBYWOBDOCUKOW-UHFFFAOYSA-N 0.000 claims description 3
- 125000004076 pyridyl group Chemical group 0.000 claims description 3
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 2
- 239000002671 adjuvant Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 150000001728 carbonyl compounds Chemical class 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 39
- 230000003746 surface roughness Effects 0.000 description 15
- 150000003839 salts Chemical class 0.000 description 11
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 6
- 125000001931 aliphatic group Chemical group 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910000679 solder Inorganic materials 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 229910001128 Sn alloy Inorganic materials 0.000 description 3
- 239000003093 cationic surfactant Substances 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
- 150000001875 compounds Chemical class 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- SUMDYPCJJOFFON-UHFFFAOYSA-N isethionic acid Chemical compound OCCS(O)(=O)=O SUMDYPCJJOFFON-UHFFFAOYSA-N 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 150000003871 sulfonates Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- STTGYIUESPWXOW-UHFFFAOYSA-N 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline Chemical compound C=12C=CC3=C(C=4C=CC=CC=4)C=C(C)N=C3C2=NC(C)=CC=1C1=CC=CC=C1 STTGYIUESPWXOW-UHFFFAOYSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 235000001014 amino acid Nutrition 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 239000002280 amphoteric surfactant Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000003934 aromatic aldehydes Chemical class 0.000 description 2
- 150000008365 aromatic ketones Chemical class 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- CCIVGXIOQKPBKL-UHFFFAOYSA-N ethanesulfonic acid Chemical compound CCS(O)(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- ZRSNZINYAWTAHE-UHFFFAOYSA-N p-methoxybenzaldehyde Chemical compound COC1=CC=C(C=O)C=C1 ZRSNZINYAWTAHE-UHFFFAOYSA-N 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 125000004434 sulfur atom Chemical group 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 1
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 description 1
- 239000001211 (E)-4-phenylbut-3-en-2-one Substances 0.000 description 1
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 description 1
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- SLIBCJURSADKPV-UHFFFAOYSA-N 1,10-dihydro-1,10-phenanthroline-4,7-dione Chemical compound N1C=CC(=O)C2=CC=C3C(=O)C=CNC3=C21 SLIBCJURSADKPV-UHFFFAOYSA-N 0.000 description 1
- SQAINHDHICKHLX-UHFFFAOYSA-N 1-naphthaldehyde Chemical compound C1=CC=C2C(C=O)=CC=CC2=C1 SQAINHDHICKHLX-UHFFFAOYSA-N 0.000 description 1
- AFUKNJHPZAVHGQ-UHFFFAOYSA-N 2,5-dimethoxy-Benzaldehyde Chemical compound COC1=CC=C(OC)C(C=O)=C1 AFUKNJHPZAVHGQ-UHFFFAOYSA-N 0.000 description 1
- SDEJZNDOGDHERS-UHFFFAOYSA-N 2,9-dimethyl-4,7-diphenyl-1h-1,10-phenanthroline-2,3-disulfonic acid Chemical compound C=12C=CC=3C(C=4C=CC=CC=4)=C(S(O)(=O)=O)C(C)(S(O)(=O)=O)NC=3C2=NC(C)=CC=1C1=CC=CC=C1 SDEJZNDOGDHERS-UHFFFAOYSA-N 0.000 description 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- FPYUJUBAXZAQNL-UHFFFAOYSA-N 2-chlorobenzaldehyde Chemical compound ClC1=CC=CC=C1C=O FPYUJUBAXZAQNL-UHFFFAOYSA-N 0.000 description 1
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- PJKVFARRVXDXAD-UHFFFAOYSA-N 2-naphthaldehyde Chemical compound C1=CC=CC2=CC(C=O)=CC=C21 PJKVFARRVXDXAD-UHFFFAOYSA-N 0.000 description 1
- NPAXPTHCUCUHPT-UHFFFAOYSA-N 3,4,7,8-tetramethyl-1,10-phenanthroline Chemical compound CC1=CN=C2C3=NC=C(C)C(C)=C3C=CC2=C1C NPAXPTHCUCUHPT-UHFFFAOYSA-N 0.000 description 1
- USYAMXSCYLGBPT-UHFFFAOYSA-L 3-carboxy-3-hydroxypentanedioate;tin(2+) Chemical compound [Sn+2].OC(=O)CC(O)(C([O-])=O)CC([O-])=O USYAMXSCYLGBPT-UHFFFAOYSA-L 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical group [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 description 1
- 229930064664 L-arginine Natural products 0.000 description 1
- 235000014852 L-arginine Nutrition 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-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
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical class 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
- KJCVRFUGPWSIIH-UHFFFAOYSA-N alpha-naphthol Natural products C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 1
- 229930008407 benzylideneacetone Natural products 0.000 description 1
- JWAZRIHNYRIHIV-UHFFFAOYSA-N beta-hydroxynaphthyl Natural products C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- JALQQBGHJJURDQ-UHFFFAOYSA-L bis(methylsulfonyloxy)tin Chemical compound [Sn+2].CS([O-])(=O)=O.CS([O-])(=O)=O JALQQBGHJJURDQ-UHFFFAOYSA-L 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Chemical group 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 229940117916 cinnamic aldehyde Drugs 0.000 description 1
- KJPRLNWUNMBNBZ-UHFFFAOYSA-N cinnamic aldehyde Natural products O=CC=CC1=CC=CC=C1 KJPRLNWUNMBNBZ-UHFFFAOYSA-N 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 230000002950 deficient 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
- STWJKLMRMTWJEY-UHFFFAOYSA-N diphenyl 1,10-phenanthroline-4,7-disulfonate Chemical compound C=1C=NC(C2=NC=CC(=C2C=C2)S(=O)(=O)OC=3C=CC=CC=3)=C2C=1S(=O)(=O)OC1=CC=CC=C1 STWJKLMRMTWJEY-UHFFFAOYSA-N 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229960000445 ethisterone Drugs 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229940045996 isethionic acid Drugs 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 229910052751 metal Chemical class 0.000 description 1
- 239000002184 metal Chemical class 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- IYRGXJIJGHOCFS-UHFFFAOYSA-N neocuproine Chemical compound C1=C(C)N=C2C3=NC(C)=CC=C3C=CC2=C1 IYRGXJIJGHOCFS-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
- 229940044652 phenolsulfonate Drugs 0.000 description 1
- 229940044654 phenolsulfonic acid Drugs 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 229910000375 tin(II) sulfate Inorganic materials 0.000 description 1
- 125000002088 tosyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1C([H])([H])[H])S(*)(=O)=O 0.000 description 1
- BWHOZHOGCMHOBV-BQYQJAHWSA-N trans-benzylideneacetone Chemical compound CC(=O)\C=C\C1=CC=CC=C1 BWHOZHOGCMHOBV-BQYQJAHWSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
- C25D3/32—Electroplating: Baths therefor from solutions of tin characterised by the organic bath constituents used
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
- C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
【課題】コストに与える影響を抑制しつつ、得られためっきにおける「ヨリ」の発生を抑制することが可能な、スズ系めっき用酸性水系組成物を提供する。
【解決手段】水溶性第一スズ含有物質と、非イオン性界面活性剤およびポリオキシアルキレン基を有するイオン性界面活性剤からなる群から選ばれる一種または二種以上の界面活性剤と、芳香族カルボニル化合物からなる光沢成分と、2位および4位の少なくとも一つが電子求引性基により置換されたピリジン誘導体からなる光沢補助剤とを含有するスズ系めっき用酸性水系組成物が提供される。
【選択図】 なしAn acidic aqueous composition for tin plating capable of suppressing the occurrence of “twist” in the obtained plating while suppressing the effect on cost is provided.
One or more surfactants selected from the group consisting of water-soluble stannous-containing substances, nonionic surfactants and ionic surfactants having a polyoxyalkylene group, and aromatics There is provided an acidic aqueous composition for tin plating containing a gloss component comprising a carbonyl compound and a gloss adjuvant comprising a pyridine derivative in which at least one of the 2-position and 4-position is substituted with an electron-attracting group.
[Selection figure] None
Description
本発明は、スズ系めっき用酸性水系組成物に関する。
本発明において、「スズ系めっき」なる用語は、スズからなるめっきおよびスズ合金からなるめっきの総称として用いられる。
The present invention relates to an acidic aqueous composition for tin plating.
In the present invention, the term “tin-based plating” is used as a general term for plating made of tin and plating made of a tin alloy.
スズ系めっきは、半導体チップ部品、水晶発振子、コンデンサ、コネクタピン、リードフレーム、プリント回路基板などの電気・電子部品における接点部やはんだ接続部に広く使用されている。スズ系めっきのうち、光沢めっきは、無光沢めっきに比べて、疵がつきにくい、はんだ濡れ性に優れるといった利点を有しているため、上記用途に本来適している。 Tin-based plating is widely used for contact parts and solder connection parts in electrical / electronic parts such as semiconductor chip parts, crystal oscillators, capacitors, connector pins, lead frames, and printed circuit boards. Among the tin-based platings, the bright plating is inherently suitable for the above-mentioned applications because it has advantages such as less wrinkling and better solder wettability than the non-gloss plating.
しかしながら、電気・電子部品は、その製造の過程でリフロー処理などの加熱処理を経る場合があるところ、従来技術に係る光沢めっきはこのような加熱処理を経るとめっきに「ヨリ」が発生しやすいという問題点を有する。ここで、「ヨリ」とは、加熱処理を受けることによってスズ系めっきの厚さが局所的に変動する現象であり、その変動によって生じためっきの凹凸は波状や木目状の模様の外観をもたらすことがある。しかも、めっきの凹部においてはめっきの下地(ニッケルなど)やスズと下地金属との金属間化合物が露出する場合があり、この場合にはその露出部分のはんだ濡れ性が極端に低下してしまい、そのような露出部分が生じた電気・電子部品は廃棄対象となることもある。 However, electrical and electronic parts may be subjected to heat treatment such as reflow treatment in the course of their production, and gloss plating according to the prior art tends to generate “twist” in the plating after such heat treatment. Has the problem. Here, “twist” is a phenomenon in which the thickness of the tin-based plating varies locally by being subjected to heat treatment, and the unevenness of the plating caused by the variation brings about the appearance of a wavy or woody pattern. Sometimes. In addition, in the plating recess, the plating base (such as nickel) or the intermetallic compound of tin and the base metal may be exposed, and in this case, the solder wettability of the exposed portion is extremely reduced, Electrical / electronic components with such exposed parts may be discarded.
このような「ヨリ」の発生を抑制するべく様々な技術が提案されている。
例えば、特許文献1には、(a)第一スズ塩と、第一スズ塩及び銅、ビスマス、銀、インジウム、亜鉛、ニッケル、コバルト、アンチモンから選ばれた金属の塩とのいずれかよりなる可溶性塩と、(b)アルカンスルホン酸、アルカノールスルホン酸よりなる群から選ばれた脂肪族スルホン酸の少なくとも一種を含有するスズ及びスズ合金メッキ浴において、上記脂肪族スルホン酸(b)が、同スルホン酸以外の不純物としてのイオウ化合物をゼロ濃度に排除するか、微量濃度にまで低減した精製脂肪族スルホン酸であって、上記不純物としてのイオウ化合物が、分子内に酸化途上のイオウ原子を有する化合物と、分子内にイオウ原子と塩素原子を併有する化合物との少なくとも一種である、スズ及びスズ合金の脂肪族スルホン酸メッキ浴が提案されている。
Various techniques have been proposed to suppress the occurrence of such “twisting”.
For example, Patent Document 1 includes (a) any one of a stannous salt and a metal salt selected from a stannous salt and copper, bismuth, silver, indium, zinc, nickel, cobalt, and antimony. In a tin and tin alloy plating bath containing a soluble salt and (b) at least one aliphatic sulfonic acid selected from the group consisting of alkanesulfonic acid and alkanolsulfonic acid, the aliphatic sulfonic acid (b) is the same as It is a purified aliphatic sulfonic acid in which sulfur compounds as impurities other than sulfonic acid are eliminated to zero concentration or reduced to a trace concentration, and the sulfur compounds as impurities have sulfur atoms in the molecule during oxidation An aliphatic sulfonic acid plating bath of tin and a tin alloy, which is at least one of a compound and a compound having both a sulfur atom and a chlorine atom in the molecule; It is draft.
また、特許文献2には、a)基体表面上にスズ皮膜をめっきする工程;b)基体表面上の該スズ皮膜を、リフロー処理する前に、グリシンおよびL−アルギニンからなる群から選択される1以上のアミノ酸を含む水溶液で処理する工程;およびc)該スズ皮膜をリフロー処理する工程を含むスズめっき皮膜の表面処理方法が提案されている。 In Patent Document 2, a) a step of plating a tin film on the surface of the substrate; b) the tin film on the surface of the substrate is selected from the group consisting of glycine and L-arginine before the reflow treatment. There has been proposed a surface treatment method for a tin plating film, comprising a step of treating with an aqueous solution containing one or more amino acids; and c) a step of reflowing the tin film.
しかしながら、特許文献1に開示されるめっき浴は、そのめっき浴に大量に含有される脂肪族スルホン酸を高度に精製しておく必要があり、めっき浴の生産コストの大幅な上昇は避けられない。スズ系めっきは低コストであることが他のめっき、例えば金めっきなどの貴金属系めっきに対する有利な点であることから、スズ系めっきが高コストではその価値は著しく低下してしまう。 However, in the plating bath disclosed in Patent Document 1, it is necessary to highly purify the aliphatic sulfonic acid contained in a large amount in the plating bath, and a significant increase in the production cost of the plating bath is inevitable. . The low cost of tin-based plating is an advantage over other plating, for example, noble metal-based plating such as gold plating. Therefore, the value of tin-based plating is significantly reduced at high cost.
また、特許文献2に開示される方法は、特定のアミノ酸を含有する水溶液で処理する工程が追加されることになるため、電気・電子部品の生産コストの上昇をもたらしてしまう。 In addition, the method disclosed in Patent Document 2 adds a step of treatment with an aqueous solution containing a specific amino acid, and thus increases the production cost of electric / electronic parts.
このため、コストに与える影響を小さくしつつ「ヨリ」の発生を抑制する手段が望まれている。 For this reason, means for suppressing the occurrence of “twisting” while reducing the effect on cost is desired.
本発明は、このような技術背景を鑑み、コストに与える影響を抑制しつつ、得られためっきにおける「ヨリ」の発生を抑制することが可能な、スズからなるめっき用酸性水系組成物を提供することを課題とする。
In view of such a technical background, the present invention provides an acidic aqueous composition for plating made of tin capable of suppressing the occurrence of “twist” in the obtained plating while suppressing the effect on cost. The task is to do.
上記課題を解決するために提供される本発明は次のとおりである。
(1)水溶性第一スズ含有物質と、非イオン性界面活性剤およびポリオキシアルキレン基を有するイオン性界面活性剤からなる群から選ばれる一種または二種以上の界面活性剤と、芳香族カルボニル化合物からなる光沢成分と、2位および4位の少なくとも一つが電子求引性基により置換されたピリジン誘導体からなる光沢補助剤と、フェナントロリン系化合物の一種または二種以上とを含有することを特徴とするスズからなるめっき用酸性水系組成物。
The present invention provided to solve the above problems is as follows.
(1) One or more surfactants selected from the group consisting of a water-soluble stannous-containing substance, a nonionic surfactant and an ionic surfactant having a polyoxyalkylene group, and an aromatic carbonyl A gloss component comprising a compound, a gloss auxiliary comprising a pyridine derivative in which at least one of the 2-position and 4-position is substituted with an electron-attracting group, and one or more phenanthroline compounds are contained. An acidic aqueous composition for plating made of tin.
(2)前記電子求引性基がビニル基、カルボキシル基およびピリジル基からなる群から選ばれる一種または二種以上である、上記(1)に記載のめっき用酸性水系組成物。
(2) The acidic aqueous composition for plating according to (1) , wherein the electron withdrawing group is one or more selected from the group consisting of a vinyl group, a carboxyl group, and a pyridyl group.
(3)前記ピリジン誘導体は、4−ビニルピリジンおよび4−ピリジンカルボン酸の一種または二種を含む上記(1)に記載のめっき用酸性水系組成物。
(3) The acidic aqueous composition for plating according to (1) , wherein the pyridine derivative contains one or two of 4-vinylpyridine and 4-pyridinecarboxylic acid.
(4)前記ピリジン誘導体が2,2’−ビピリジンを含む上記(1)に記載のめっき用酸性水系組成物。 (4) The acidic aqueous composition for plating according to the above (1) , wherein the pyridine derivative contains 2,2′-bipyridine.
上記の発明によれば、コストに与える影響を抑制しつつ、「ヨリ」の発生が抑制されたスズ系めっきを形成可能な酸性水系組成物を提供することが実現される。 According to said invention, it is implement | achieved to provide the acidic aqueous composition which can form the tin-type plating by which generation | occurrence | production of "twist" was suppressed, suppressing the influence which acts on cost.
1.スズからなるめっき用酸性水系組成物
本発明は一実施形態として、水溶性第一スズ含有物質と、非イオン性界面活性剤およびポリオキシアルキレン基を有するイオン性界面活性剤からなる群から選ばれる一種または二種以上の界面活性剤と、芳香族カルボニル化合物からなる光沢成分と、2位および4位の少なくとも一つが電子求引性基により置換されたピリジン誘導体からなる光沢補助剤とを含有するスズからなるめっき用酸性水系組成物を提供する。かかる組成物を用いて適切な条件においてめっきを行えば、「ヨリ」の発生が抑制された光沢外観を有するスズからなるめっきが得られる。
1. An acidic aqueous composition for plating comprising tin The present invention is selected from the group consisting of a water-soluble stannous-containing substance, a nonionic surfactant and an ionic surfactant having a polyoxyalkylene group as an embodiment. 1 type or 2 or more types of surfactant, the gloss component which consists of an aromatic carbonyl compound, and the gloss adjuvant which consists of a pyridine derivative by which at least one of 2-position and 4-position was substituted by the electron withdrawing group An acidic aqueous composition for plating comprising tin is provided. When plating is carried out under appropriate conditions using such a composition, plating made of tin having a glossy appearance in which generation of “twist” is suppressed can be obtained.
本実施形態において、「光沢」を有する表面とは、表面粗さに係るパラメータのうち、中心線平均粗さ(以下、「表面粗さ」と略称する。)Raが0.6μm以下であることを意味する。表面粗さRaが0.5μm以下であれば優れた光沢を有する表面といえる。 In the present embodiment, the surface having “gloss” refers to a center line average roughness (hereinafter abbreviated as “surface roughness”) Ra among parameters related to surface roughness of 0.6 μm or less. Means. If the surface roughness Ra is 0.5 μm or less, it can be said that the surface has excellent gloss.
また、表面粗さのパラメータの一つである最大高さRmaxを用いて「ヨリ」が発生した表面を表現すれば、リフロー後の表面における最大高さRmaxがスズ系めっきの厚さよりも大きい表面であるといえる。この点を具体的に数値で説明すれば、3μm程度の厚さのスズ系めっきが形成されたプリント基板を260℃で1分間静置してリフローを再現したときに、「ヨリ」が発生した表面では、最大高さRmaxが10〜40μmとなる場合もある。 Further, if the surface where “twist” is generated is expressed using the maximum height Rmax which is one of the parameters of the surface roughness, the surface where the maximum height Rmax in the surface after reflow is larger than the thickness of the tin-based plating You can say that. Explaining this point in terms of numerical values, when the printed circuit board on which the tin-based plating having a thickness of about 3 μm was formed was left at 260 ° C. for 1 minute and reflow was reproduced, “twist” occurred. On the surface, the maximum height Rmax may be 10 to 40 μm.
(1)水溶性第一スズ含有物質
本実施形態に係るスズからなるめっき用酸性水系組成物(以下、「めっき液」ともいう。)は水溶性第一スズ含有物質を含む。「水溶性第一スズ含有物質」とは、スズの二価の陽イオン(Sn2+)およびこれを含有する水溶性物質からなる群から選ばれる一種または二種以上からなる物質をいう。
(1) Water-soluble stannous-containing material The acidic aqueous composition for plating (hereinafter also referred to as “plating solution”) made of tin according to the present embodiment includes a water-soluble stannous-containing material. The “water-soluble stannous-containing substance” refers to a substance composed of one or more selected from the group consisting of a divalent cation (Sn 2+ ) of tin and a water-soluble substance containing the same.
水溶性第一スズ含有物質をめっき液に供給する原料物質(本実施形態において、「第一スズ源」ともいう。)として、硫酸第一スズ、塩化第一スズ、ホウフッ化第一スズ等の無機系酸第一スズ;イセチオン酸第一スズなどのアルカノールスルホン酸第一スズ、メタンスルホン酸第一スズ、エタンスルホン酸第一スズ等のアルカンスルホン酸第一スズ;フェノールスルホン酸第一スズ、クレゾールスルホン酸第一スズ等の芳香族系スルホン酸第一スズ、クエン酸第一スズ、酢酸第一スズ等のカルボン酸第一スズなどが例示される。これらは単独で用いてもよいし、複数種類を組み合わせて用いてもよい。 As a raw material for supplying a water-soluble stannous-containing substance to the plating solution (also referred to as “stannous source” in this embodiment), such as stannous sulfate, stannous chloride, stannous borofluoride, etc. Stannous alkanol sulfonates such as stannous isethionate, stannous methanesulfonate, stannous ethane sulfonate, etc. stannous phenol sulfonate; Examples include aromatic stannous sulfonates such as stannous cresol sulfonate, stannous carboxylates such as stannous citrate and stannous acetate. These may be used alone or in combination of a plurality of types.
本実施形態に係るめっき液における水溶性第一スズ含有物質のスズ換算含有量は、5g/L以上200g/L以下とすることが好ましく、30g/L以上100g/L以下とすることがさらに好ましい。水溶性第一スズ含有物質の含有量が過度に低い場合にはスズ系めっきを析出させることができなくなる。一方、水溶性第一スズ含有物質の含有量が過度に高い場合には、めっき液の粘度が高くなったことに基づいてめっきの付きまわり性が低下することが懸念される。なお、第一スズ源の配合量が過度に高くなると、めっき液中にはめっき液に溶解した状態にある水溶性第一スズ含有物質とめっき液中で固体の状態にある第一スズ源とが含まれることとなり、このとき、水溶性第一スズ含有物質のめっき液中の含有量は第一スズ源の溶解度に依存する。 The tin-converted content of the water-soluble stannous-containing substance in the plating solution according to this embodiment is preferably 5 g / L or more and 200 g / L or less, and more preferably 30 g / L or more and 100 g / L or less. . When the content of the water-soluble stannous-containing substance is excessively low, tin-based plating cannot be deposited. On the other hand, when the content of the water-soluble stannous-containing substance is excessively high, there is a concern that the throwing power of the plating is lowered based on the increase in the viscosity of the plating solution. If the amount of stannous source is excessively high, the plating solution contains a water-soluble stannous-containing substance that is dissolved in the plating solution and a stannous source that is in a solid state in the plating solution. In this case, the content of the water-soluble stannous-containing substance in the plating solution depends on the solubility of the stannous source.
(2)界面活性剤
本実施形態に係るめっき液は、非イオン性界面活性剤およびポリオキシアルキレン基を有するイオン性界面活性剤からなる群から選ばれる一種または二種以上の界面活性剤を含む。
(2) Surfactant The plating solution according to the present embodiment includes one or more surfactants selected from the group consisting of a nonionic surfactant and an ionic surfactant having a polyoxyalkylene group. .
非イオン性界面活性剤としては、ポリオキシアルキレンアルキルフェノールエーテル、ポリオキシアルキレン高級アルコールエーテル、ポリオキシアルキレン−α−またはβ−ナフトールエーテル、ポリオキシアルキレン−モノ−、ジ−またはトリ−スチレン化フェノールエーテル、ポリオキシエチレン−ポリオキシプロピレン−ブロックポリマー、エチノンジアミンのポリオキシエチレン−ポリオキシプロピレン縮合物、ポリオキシアルキレン付加アルキルアミン、ポリオキシアルキレン付加アルキルアミド等が例示される。これらは単独で用いてもよいし、複数種類を組み合わせて用いてもよい。 Nonionic surfactants include polyoxyalkylene alkylphenol ethers, polyoxyalkylene higher alcohol ethers, polyoxyalkylene-α- or β-naphthol ethers, polyoxyalkylene-mono-, di- or tri-styrenated phenol ethers. , Polyoxyethylene-polyoxypropylene-block polymer, polyoxyethylene-polyoxypropylene condensate of ethinone diamine, polyoxyalkylene-added alkylamine, polyoxyalkylene-added alkylamide and the like. These may be used alone or in combination of a plurality of types.
ポリオキシアルキレン基を有するイオン性界面活性剤としては、アルキルフェノキシポリオキシアルキレンエチルスルホン酸およびその塩、高級アルコールのポリオキシアルキレンエチルスルホン酸およびその塩等のアニオン性界面活性剤、N,N−ジポリオキシアルキレン−N,N−ジアルキルアンモニウム塩酸塩等のカチオン性界面活性剤が例示される。これらは単独で用いてもよいし、複数種類を組み合わせて用いてもよい。 Examples of the ionic surfactant having a polyoxyalkylene group include anionic surfactants such as alkylphenoxy polyoxyalkylene ethyl sulfonic acid and salts thereof, polyoxyalkylene ethyl sulfonic acid of higher alcohols and salts thereof, N, N— Illustrative are cationic surfactants such as dipolyoxyalkylene-N, N-dialkylammonium hydrochloride. These may be used alone or in combination of a plurality of types.
上記の界面活性剤の含有量は限定されない。当該含有量が過度に少ない場合には得られためっきに光沢が得られにくくなる。一方、含有量が過度に多い場合には発泡が盛んになって消泡剤を用いなければめっきを行うことが不可能になることが懸念される。上記の界面活性剤の含有量の好ましい一例を挙げれば、0.5g/L以上40g/L以下である。 The content of the surfactant is not limited. When the content is excessively small, it is difficult to obtain gloss in the obtained plating. On the other hand, when the content is excessively large, foaming becomes active and there is a concern that it is impossible to perform plating unless an antifoaming agent is used. If a preferable example of content of said surfactant is given, it will be 0.5 g / L or more and 40 g / L or less.
本実施形態に係るめっき液は上記の界面活性剤以外の界面活性剤を含有してもよい。そのような界面活性剤として、カチオン性界面活性剤、両性界面活性剤が例示される。カチオン性界面活性剤の具体例として、N−モノアルキル−N−トリメチルアンモニウム塩、N,N−ジアルキル−N−ジメチルアンモノウム塩、N−アルキル−イソキノリニウム塩および1−アルキル−1−ヒドロキシエチル−イミダゾリウム塩が挙げられる。両性界面活性剤の具体例として、1−ヒドロキシエチル−1−カルボキシアルキレン−2−アルキルイミダゾリウムベタイン、およびN,N−ジメチル−N−アルキルベタインが挙げられる。 The plating solution according to the present embodiment may contain a surfactant other than the above surfactants. Examples of such surfactants include cationic surfactants and amphoteric surfactants. Specific examples of the cationic surfactant include N-monoalkyl-N-trimethylammonium salt, N, N-dialkyl-N-dimethylammonium salt, N-alkyl-isoquinolinium salt and 1-alkyl-1-hydroxyethyl. -Imidazolium salts. Specific examples of the amphoteric surfactant include 1-hydroxyethyl-1-carboxyalkylene-2-alkylimidazolium betaine and N, N-dimethyl-N-alkylbetaine.
本実施形態に係るめっき液が含有する界面活性剤の合計含有量は特に限定されないが、0.5g/L以上80g/L以下の範囲で用いられることが好ましく、1g/L以上50g/L以下であればさらに好ましい。 Although the total content of the surfactant contained in the plating solution according to this embodiment is not particularly limited, it is preferably used in the range of 0.5 g / L to 80 g / L, and preferably 1 g / L to 50 g / L. More preferably.
(3)光沢成分
本実施形態に係るめっき液は芳香族カルボニル化合物からなる光沢成分を含有する。
芳香族カルボニル化合物としては、芳香族アルデヒド、芳香族ケトンなどが例示される。
(3) Gloss component The plating solution which concerns on this embodiment contains the gloss component which consists of an aromatic carbonyl compound.
Examples of the aromatic carbonyl compound include aromatic aldehydes and aromatic ketones.
芳香族アルデヒドの具体例として、ベンズアルデヒド、o−クロルベンズアルデヒド、トルアルデヒド、アニスアルデヒド、シンナムアルデヒド、2,5−ジメトキシベンズアルデヒド、および1−または2−ナフトアルデヒドが例示される。芳香族ケトンの具体例として、ベンジリデンアセトンおよびアルキルナフチルケトンが例示される。 Specific examples of the aromatic aldehyde include benzaldehyde, o-chlorobenzaldehyde, tolualdehyde, anisaldehyde, cinnamaldehyde, 2,5-dimethoxybenzaldehyde, and 1- or 2-naphthaldehyde. Specific examples of the aromatic ketone include benzylideneacetone and alkyl naphthyl ketone.
上記の光沢成分の含有量は限定されない。過度に少ない場合には得られるめっきに光沢を付与することができなくなり、過度に多い場合にはめっき液の安定性が低下することを考慮して適宜設定すればよい。好ましい含有量の範囲は0.005g/L(5ppm)以上5g/L以下であり、0.01g/L(10ppm)以上2g/L以下とすればさらに好ましい。 The content of the gloss component is not limited. When the amount is excessively small, gloss cannot be imparted to the obtained plating, and when it is excessively large, the plating solution may be deteriorated in stability, so that it may be set appropriately. The range of preferable content is 0.005 g / L (5 ppm) or more and 5 g / L or less, and more preferably 0.01 g / L (10 ppm) or more and 2 g / L or less.
(4)光沢補助剤
本実施形態に係るめっき液は、2位および4位の少なくとも一つが電子求引性基により置換されたピリジン誘導体からなる光沢補助剤を含有する。以下、かかる光沢補助剤を「ピリジン系光沢補助剤」ともいう。ピリジン系光沢補助剤を与える電子求引性基として、ビニル基、カルボキシル基、トシル基、塩素などのハロゲン原子、シアノ基、ベンゾイル基、アセチル基、ピリジル基などが例示される。これらの中でも、ビニル基およびカルボキシル基が好ましい電子求引性基である。したがって、4−ビニルピリジンおよび4−ピリジンカルボン酸が特に好ましいピリジン系光沢補助剤である。
(4) Gloss adjuvant The plating solution which concerns on this embodiment contains the gloss adjuvant which consists of a pyridine derivative by which at least one of 2-position and 4-position was substituted by the electron withdrawing group. Hereinafter, such a gloss auxiliary is also referred to as a “pyridine-based gloss auxiliary”. Examples of the electron withdrawing group that gives the pyridine-based gloss auxiliary include halogen groups such as vinyl group, carboxyl group, tosyl group, chlorine, cyano group, benzoyl group, acetyl group, and pyridyl group. Among these, a vinyl group and a carboxyl group are preferable electron withdrawing groups. Accordingly, 4-vinylpyridine and 4-pyridinecarboxylic acid are particularly preferred pyridine-based gloss adjuvants.
ピリジン系光沢補助剤の含有量は、0.005g/L(5ppm)以上0.2g/L(200ppm)以下とすることが好ましい。ピリジン系光沢補助剤の含有量が過度に少ない場合にはこれを含有させた効果を得ることができなくなることが懸念される。一方、過度に多い場合には他の添加成分とのバランスが崩れ、所望の外観(例えば光沢)が得られなくなったり、めっきの析出速度が低下したりすることが懸念される。 The content of the pyridine-based gloss auxiliary is preferably 0.005 g / L (5 ppm) or more and 0.2 g / L (200 ppm) or less. When the content of the pyridine-based gloss auxiliary is excessively small, there is a concern that the effect of containing this cannot be obtained. On the other hand, when it is excessively large, there is a concern that the balance with other additive components may be lost, and a desired appearance (for example, gloss) may not be obtained, or the deposition rate of plating may be reduced.
(5)その他の成分
本実施形態に係るめっき液は、上記の成分に加えて、めっき液の導電性を高めるための成分(以下、「電解質成分」ともいう。)を含有する。電解質成分の種類は特に限定されない。硫酸、塩酸、ホウ酸、ホウフッ化水素酸等の無機酸;イセチオン酸等のアルカノールスルホン酸、メタンスルホン酸等のアルカンスルホン酸、フェノールスルホン酸等の芳香族系スルホン酸などのスルホン酸;および酢酸、クエン酸、リンゴ酸、酒石酸等のカルボン酸などの酸ならびにこれら酸のアンモニウム塩、ナトリウム塩、カリウム塩等の塩が例示され、これらは単独で用いられてもよいし、複数種類が用いられてもよい。これらの中でもスルホン酸および/またはスルホン酸塩が好ましい。
(5) Other Components In addition to the above components, the plating solution according to the present embodiment contains a component for enhancing the conductivity of the plating solution (hereinafter also referred to as “electrolyte component”). The kind of electrolyte component is not particularly limited. Inorganic acids such as sulfuric acid, hydrochloric acid, boric acid, borohydrofluoric acid; sulfonic acid such as alkanol sulfonic acid such as isethionic acid, alkane sulfonic acid such as methane sulfonic acid, aromatic sulfonic acid such as phenol sulfonic acid; and acetic acid And acids such as carboxylic acids such as citric acid, malic acid and tartaric acid, and salts such as ammonium salts, sodium salts and potassium salts of these acids, which may be used alone or in combination. May be. Of these, sulfonic acids and / or sulfonates are preferred.
電解質成分の含有量は限定されず、めっきにおける電流密度などに基づいて適宜設定されるべきものである。その含有量の範囲の一例を挙げれば、遊離酸換算含有量として50g/L以上300g/L以下である。 The content of the electrolyte component is not limited, and should be appropriately set based on the current density in plating. If an example of the range of the content is given, it will be 50 g / L or more and 300 g / L or less as free acid conversion content.
また、本実施形態に係るめっき液は、好ましい一態様において、少なくとも一種のフェナントロリン系化合物を含有する。「フェナントロリン化合物」なる用語は、フェナントレンの縮合環を構成する14個の炭素のうち2つを窒素で置換した縮合芳香族化合物およびその誘導体の総称として用いられる。フェナントロリン化合物を含有することにより、得られたスズ系めっきはめっき直後の表面粗さRaが小さくなる。このため、リフロー後に「ヨリ」の発生に至るまで表面粗さRaが増大することが抑制される。 Moreover, the plating solution which concerns on this embodiment contains an at least 1 type of phenanthroline type compound in a preferable one aspect | mode. The term “phenanthroline compound” is used as a general term for condensed aromatic compounds in which two of the 14 carbons constituting the condensed ring of phenanthrene are substituted with nitrogen, and derivatives thereof. By containing the phenanthroline compound, the obtained tin-based plating has a small surface roughness Ra immediately after plating. For this reason, it is suppressed that surface roughness Ra increases until generation | occurrence | production of "twist" after reflow.
フェナントロリン化合物の具体例を示せば、1,10‐フェナントロリン、2,9‐ジメチルフェナントロリン、3,4,7,8‐テトラメチルフェナントロリン、4,7‐ジヒドロキシフェナントロリン、4,7‐ジフェニル‐1,10‐フェナントロリン(バソフェナントロリン)、4,7‐ジフェニル‐2,9‐ジメチルフェナントロリン(バソクプロイン)、4,7‐ジフェニル‐1,10‐フェナントロリン‐ジスルホン酸およびその塩(バソフェナントロリンジスルホン酸およびその塩)、ならびに4,7‐ジフェニル‐2,9‐ジメチル‐1,10‐フェナントロリン‐ジスルホン酸およびその塩(バソクプロインジスルホン酸及びその塩)が挙げられる。 Specific examples of phenanthroline compounds include 1,10-phenanthroline, 2,9-dimethylphenanthroline, 3,4,7,8-tetramethylphenanthroline, 4,7-dihydroxyphenanthroline, 4,7-diphenyl-1,10. -Phenanthroline (vasophenanthroline), 4,7-diphenyl-2,9-dimethylphenanthroline (basocuproin), 4,7-diphenyl-1,10-phenanthroline-disulfonic acid and salts thereof (vasophenanthroline disulfonic acid and salts thereof), And 4,7-diphenyl-2,9-dimethyl-1,10-phenanthroline-disulfonic acid and salts thereof (bathocuproin disulfonic acid and salts thereof).
本実施形態に係るめっき液が含有するフェナントロリン化合物は一種であってもよいし、二種以上であってもよい。また、フェナントロリン化合物の含有量は限定されないが、その効果を安定的に得る観点から、含有させる場合には0.0001g/L以上(0.1ppm)含有させることが好ましく、0.001g/L(1ppm)以上含有させることがさらに好ましい。一方、フェナントロリン化合物を過度に含有させるとめっきの析出速度の低下が顕著となるため、1g/L程度を上限とすることが好ましく、0.1g/L以下とすることがさらに好ましい。 The phenanthroline compound contained in the plating solution according to this embodiment may be one type or two or more types. Further, the content of the phenanthroline compound is not limited, but from the viewpoint of stably obtaining the effect, when it is contained, 0.0001 g / L or more (0.1 ppm) is preferably contained, and 0.001 g / L ( 1 ppm) or more is more preferable. On the other hand, if the phenanthroline compound is excessively contained, the deposition rate of the plating is remarkably lowered. Therefore, the upper limit is preferably about 1 g / L, and more preferably 0.1 g / L or less.
本実施形態に係るめっき液は、必要に応じて、酸化防止剤や消泡剤をさらに含有してもよい。酸化防止剤はめっき液中のスズ第一イオンが酸化されることを抑制するためのものであり、カテコール、ハイドロキノンなどが例示される。その含有量は限定されないが、好ましい一例を挙げれば0.05g/L以上20g/L以下であり、0.1g/L以上15g/L以下とすればさらに好ましい。 The plating solution which concerns on this embodiment may further contain antioxidant and an antifoamer as needed. The antioxidant is for suppressing the oxidation of tin first ions in the plating solution, and examples thereof include catechol and hydroquinone. The content is not limited, but a preferred example is 0.05 g / L or more and 20 g / L or less, and more preferably 0.1 g / L or more and 15 g / L or less.
(6)溶媒、pH
本実施形態に係るめっき液の溶媒は水を主成分とする。水以外の溶媒としてアルコール、エーテル、ケトンなど水への溶解度が高い有機溶媒を混在させてもよい。この場合には、めっき液全体の安定性および廃液処理への負荷の緩和の観点から、その比率は全溶媒に対して10体積%以下とすることが好ましい。
(6) Solvent, pH
The solvent of the plating solution according to this embodiment contains water as a main component. As a solvent other than water, an organic solvent having high solubility in water, such as alcohol, ether, and ketone, may be mixed. In this case, the ratio is preferably 10% by volume or less with respect to the total solvent from the viewpoint of the stability of the entire plating solution and the relaxation of the load on the waste solution treatment.
本実施形態に係るめっき液は酸性である。好ましい一態様においては強酸性であり、そのpHは通常1以下である。前述の電解質成分を含有させるにあたり、酸として加える量を調整することによって、めっき液を所望のpHに設定することができる。 The plating solution according to this embodiment is acidic. In a preferred embodiment, it is strongly acidic and its pH is usually 1 or less. When the above-described electrolyte component is contained, the plating solution can be set to a desired pH by adjusting the amount added as an acid.
2.めっき条件
本実施形態に係るめっき液のめっき条件は特に限定されない。各条件についての好ましい態様は次のとおりである。
2. Plating conditions The plating conditions of the plating solution according to the present embodiment are not particularly limited. Preferred embodiments for each condition are as follows.
(1)電流密度
「ヨリ」の発生が問題となるような電気・電子部品用途における電流密度は通常10A/dm2以下であり、7A/dm2以下とされる場合が多い。得られためっきに光沢を安定的に付与する観点からは、3A/dm2以上とすることが好ましく、5A/dm2以上とすればさらに好ましい。
(1) Current density The current density in electrical / electronic component applications where the occurrence of “twist” is a problem is usually 10 A / dm 2 or less, and often 7 A / dm 2 or less. From the viewpoint of stably imparting gloss to the obtained plating, it is preferably 3 A / dm 2 or more, more preferably 5 A / dm 2 or more.
(2)めっき温度
めっき温度は特に限定されない。通常、20℃以上50℃以下の範囲で実施される。温度の変動はめっき外観の変化をもたらす場合があるため、めっき温度の管理幅は5℃程度とすることが好ましい。
(2) Plating temperature The plating temperature is not particularly limited. Usually, it is carried out in the range of 20 ° C or higher and 50 ° C or lower. Since fluctuations in temperature may cause changes in plating appearance, the management range of the plating temperature is preferably about 5 ° C.
(3)積算電流量
積算電流量は特に限定されない。積算電流量が過度に少ない場合にはニッケルなどからなる下地金属を十分に覆うことができず、はんだ濡れ性を向上させることができなくなることが懸念される。一方、積算電流量が過度に多い場合には経済的な観点から不利となる。積算電流量の範囲は、これらを考慮して適宜設定されるべきものである。
(3) Integrated current amount The integrated current amount is not particularly limited. When the accumulated current amount is excessively small, it is feared that the base metal made of nickel or the like cannot be sufficiently covered and the solder wettability cannot be improved. On the other hand, when the accumulated current amount is excessively large, it is disadvantageous from an economical viewpoint. The range of the integrated current amount should be appropriately set in consideration of these.
以下、本発明の効果を実施例に基づいて説明するが、本発明はこれに限定されるものではない。 Hereinafter, although the effect of the present invention is explained based on an example, the present invention is not limited to this.
(実施例1)
(1)めっき液の調製
表1に示されるめっき液1〜7を調製した。
Example 1
(1) Preparation of plating solution The plating solutions 1-7 shown in Table 1 were prepared.
(2)めっき処理
得られためっき液1〜7のそれぞれを用いて、下記のめっき条件にてめっきを行った。なお、めっきの基板は、Cu1020からなる配線上に電気ニッケルめっき(スルファミン酸浴、1μm)が形成されたオープンフレームのプリント基板であって、公知の方法で洗浄・活性化を行ったものとした。
電流密度:5、10、15A/dm2
めっき温度:25℃ (管理幅:±1℃)
積算電流量:300A・sec/dm2
その他のめっき条件:攪拌あり(攪拌子にて500rpmで回転)、揺動あり(カソードロッカにて5m/分)
(2) Plating treatment Plating was performed using the obtained plating solutions 1 to 7 under the following plating conditions. The plating substrate is an open frame printed circuit board in which electric nickel plating (sulfamic acid bath, 1 μm) is formed on a wiring made of Cu1020, and is cleaned and activated by a known method. .
Current density: 5, 10, 15 A / dm 2
Plating temperature: 25 ° C (Control width: ± 1 ° C)
Integrated current amount: 300 A · sec / dm 2
Other plating conditions: Stirring (rotation at 500 rpm with a stirrer), rocking (5 m / min with cathode rocker)
(3)リフロー試験
上記のめっき処理により得られたスズ系めっきが形成されたプリント基板を、260℃に保持されたホットプレート上に1分間静置して、リフローさせた。
(3) Reflow test The printed circuit board on which the tin-based plating obtained by the above-described plating treatment was formed was allowed to stand for 1 minute on a hot plate maintained at 260 ° C. and reflowed.
(4)評価
めっき後のプリント基板の任意の位置におけるめっき面の表面粗さRaを測定した。測定長さは1354μmであり、3箇所の測定結果の平均値を求めた。なお、電流密度が大きい場合などにおいて表面が粗面化している領域がある場合には、その領域が可能な限り測定範囲内に含まれるようにして測定を行った。
また、リフロー後のプリント基板を観察し、ヨリが発生している場合には、ヨリが発生している領域が可能な限り測定範囲内に含まれるようにして、めっきが施された部分における表面粗さRaを測定した。測定長さは1354μmであり、3箇所の測定結果の平均値を求めた。
得られたリフロー後の表面粗さRaについて、全ての電流密度においてRaが0.6μm以下の場合には良好(光沢あり)と判定し、表面粗さRaが0.6μm超となる結果を少なくとも一つ含む場合には不良(光沢なし)と判定した。また、上記の基準に基づき良好と判定された結果のうち、近時のめっき条件を考慮して、電流密度を5A/dm2としたときにおけるめっき後およびリフロー後の表面粗さRaが0.5μm以下となる場合には、特に良好と判定した。
(4) Evaluation The surface roughness Ra of the plated surface at an arbitrary position on the printed circuit board after plating was measured. The measurement length was 1354 μm, and the average value of the measurement results at three locations was determined. When there is a region where the surface is roughened when the current density is large or the like, the measurement was performed so that the region was included in the measurement range as much as possible.
In addition, when the printed circuit board after reflow is observed, and there is a twist, the surface where the plating has been applied so that the twisted region is included in the measurement range as much as possible. The roughness Ra was measured. The measurement length was 1354 μm, and the average value of the measurement results at three locations was determined.
Regarding the obtained surface roughness Ra after reflow, when Ra is 0.6 μm or less at all current densities, it is determined to be good (glossy), and the result that the surface roughness Ra exceeds 0.6 μm is at least When one was included, it was determined to be defective (no gloss). Of the results determined to be good based on the above criteria, the surface roughness Ra after plating and after reflowing when the current density is 5 A / dm 2 in consideration of the recent plating conditions is 0. When it was 5 μm or less, it was determined to be particularly good.
(5)結果
評価結果を表2に示す。
表2に示されるように、めっき液1から3については、少なくともリフロー後の表面粗さRaは電流密度にかかわらず0.6μm以下の光沢となり、ヨリが発生しなかった。特に、めっき液1および2については、5A/dm2のときの表面粗さRaが0.5μm以下となった。
一方、めっき液4から6については、リフロー後の表面粗さRaは0.6μmを超える場合があり、ヨリが発生した。
As shown in Table 2, with respect to the plating solutions 1 to 3, at least the surface roughness Ra after reflow became a gloss of 0.6 μm or less regardless of the current density, and no twist occurred. In particular, for plating solutions 1 and 2, the surface roughness Ra at 5 A / dm 2 was 0.5 μm or less.
On the other hand, with respect to the plating solutions 4 to 6, the surface roughness Ra after reflow sometimes exceeds 0.6 μm, and twisting occurred.
(実施例2)
表3に示されるめっき液8〜10を調製した。得られためっき液8〜10のそれぞれを用いて、実施例1と同様のめっき処理およびリフロー試験を行い、それらの結果を実施例1の場合と同様の方法で評価した。
(Example 2)
Plating solutions 8 to 10 shown in Table 3 were prepared. Using each of the obtained plating solutions 8 to 10, the same plating treatment and reflow test as in Example 1 were performed, and the results were evaluated by the same method as in Example 1.
評価結果を表4に示す。
めっき液1とめっき液8との対比により、フェナントロリン化合物を含有させることによってめっき後の表面粗さRaが小さくなり、その結果、リフロー後においても表面粗さRaは0.5μmよりも十分に小さくなって、優れた光沢が得られることが確認された。
また、めっき液1、めっき液9およびめっき液10の対比により、ピリジン系光沢補助剤の含有量を100ppmとしても十分にヨリの発生を抑制できることが確認された。
By comparing the plating solution 1 and the plating solution 8, the surface roughness Ra after plating is reduced by containing a phenanthroline compound. As a result, the surface roughness Ra is sufficiently smaller than 0.5 μm even after reflow. Thus, it was confirmed that excellent gloss was obtained.
Moreover, it was confirmed by the contrast of the plating solution 1, the plating solution 9, and the plating solution 10 that generation | occurrence | production of a twist can fully be suppressed even if content of a pyridine type gloss adjuvant is 100 ppm.
Claims (4)
非イオン性界面活性剤およびポリオキシアルキレン基を有するイオン性界面活性剤からなる群から選ばれる一種または二種以上の界面活性剤と、
芳香族カルボニル化合物からなる光沢成分と、
2位および4位の少なくとも一つが電子求引性基により置換されたピリジン誘導体からなる光沢補助剤と、
フェナントロリン系化合物の一種または二種以上とを含有すること
を特徴とするスズ系めっき用酸性水系組成物。 A water-soluble stannous-containing substance;
One or more surfactants selected from the group consisting of nonionic surfactants and ionic surfactants having a polyoxyalkylene group;
A glossy component comprising an aromatic carbonyl compound;
A gloss auxiliary comprising a pyridine derivative substituted at least one of the 2-position and 4-position with an electron-withdrawing group ;
An acidic aqueous composition for tin plating , comprising one or more phenanthroline compounds .
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JP6677873B2 (en) * | 2018-03-26 | 2020-04-08 | 三菱マテリアル株式会社 | Tin or tin alloy plating solution and bump forming method using the same |
WO2019181906A1 (en) * | 2018-03-20 | 2019-09-26 | 三菱マテリアル株式会社 | Tin or tin-alloy plating solution and bump forming method |
CN111206272B (en) * | 2020-02-25 | 2021-08-10 | 广州三孚新材料科技股份有限公司 | Plating solution additive and plating solution for electroplating matte tin on heterojunction cell, and preparation method and application of plating solution additive and plating solution |
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JP2009114548A (en) * | 2001-05-24 | 2009-05-28 | Rohm & Haas Electronic Materials Llc | Tin plating |
JP2007197790A (en) * | 2006-01-27 | 2007-08-09 | Daiwa Fine Chemicals Co Ltd (Laboratory) | Discoloration preventing agent composition |
JP2010265491A (en) * | 2009-05-12 | 2010-11-25 | Ishihara Chem Co Ltd | Bath for tin or tin-alloy plating, and barrel-plating process using the plating bath |
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CN103154328A (en) | 2013-06-12 |
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