CN108103540B - Tin alloy electroplating solution - Google Patents
Tin alloy electroplating solution Download PDFInfo
- Publication number
- CN108103540B CN108103540B CN201810067046.3A CN201810067046A CN108103540B CN 108103540 B CN108103540 B CN 108103540B CN 201810067046 A CN201810067046 A CN 201810067046A CN 108103540 B CN108103540 B CN 108103540B
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- China
- Prior art keywords
- acid
- organic
- tin
- salt
- agent
- Prior art date
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- 229910001128 Sn alloy Inorganic materials 0.000 title claims abstract description 35
- 238000009713 electroplating Methods 0.000 title claims abstract description 28
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 82
- 229920001661 Chitosan Polymers 0.000 claims abstract description 64
- 239000008139 complexing agent Substances 0.000 claims abstract description 56
- 239000002253 acid Substances 0.000 claims abstract description 52
- 239000003381 stabilizer Substances 0.000 claims abstract description 52
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 34
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 33
- 125000003396 thiol group Chemical group [H]S* 0.000 claims abstract description 32
- JIRRNZWTWJGJCT-UHFFFAOYSA-N carbamothioylthiourea Chemical compound NC(=S)NC(N)=S JIRRNZWTWJGJCT-UHFFFAOYSA-N 0.000 claims abstract description 31
- CVSVTCORWBXHQV-UHFFFAOYSA-N creatine Chemical compound NC(=[NH2+])N(C)CC([O-])=O CVSVTCORWBXHQV-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000007670 refining Methods 0.000 claims abstract description 18
- 150000003839 salts Chemical class 0.000 claims abstract description 18
- 238000005282 brightening Methods 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000001621 bismuth Chemical class 0.000 claims abstract description 4
- 150000001879 copper Chemical class 0.000 claims abstract description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 81
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims description 52
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 47
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 36
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical group C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 claims description 34
- DLLMHEDYJQACRM-UHFFFAOYSA-N 2-(carboxymethyldisulfanyl)acetic acid Chemical compound OC(=O)CSSCC(O)=O DLLMHEDYJQACRM-UHFFFAOYSA-N 0.000 claims description 32
- BDDLHHRCDSJVKV-UHFFFAOYSA-N 7028-40-2 Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O BDDLHHRCDSJVKV-UHFFFAOYSA-N 0.000 claims description 30
- KVBGVZZKJNLNJU-UHFFFAOYSA-N naphthalene-2-sulfonic acid Chemical compound C1=CC=CC2=CC(S(=O)(=O)O)=CC=C21 KVBGVZZKJNLNJU-UHFFFAOYSA-N 0.000 claims description 30
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 30
- 239000000956 alloy Substances 0.000 claims description 26
- 229950000244 sulfanilic acid Drugs 0.000 claims description 26
- 229910045601 alloy Inorganic materials 0.000 claims description 25
- 238000007747 plating Methods 0.000 claims description 24
- 239000010949 copper Substances 0.000 claims description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 22
- 229910052802 copper Inorganic materials 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- 229910052706 scandium Inorganic materials 0.000 claims description 19
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 19
- 229910052759 nickel Inorganic materials 0.000 claims description 18
- 229910052720 vanadium Inorganic materials 0.000 claims description 18
- 229910052748 manganese Inorganic materials 0.000 claims description 17
- 239000011572 manganese Substances 0.000 claims description 17
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 17
- UHGULLIUJBCTEF-UHFFFAOYSA-N 2-aminobenzothiazole Chemical compound C1=CC=C2SC(N)=NC2=C1 UHGULLIUJBCTEF-UHFFFAOYSA-N 0.000 claims description 16
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 16
- AICMYQIGFPHNCY-UHFFFAOYSA-J methanesulfonate;tin(4+) Chemical compound [Sn+4].CS([O-])(=O)=O.CS([O-])(=O)=O.CS([O-])(=O)=O.CS([O-])(=O)=O AICMYQIGFPHNCY-UHFFFAOYSA-J 0.000 claims description 16
- 229910052710 silicon Inorganic materials 0.000 claims description 16
- 239000010703 silicon Substances 0.000 claims description 16
- FNRAFDRAOOKVOR-UHFFFAOYSA-M silver;2-hydroxypropane-1-sulfonate Chemical compound [Ag+].CC(O)CS([O-])(=O)=O FNRAFDRAOOKVOR-UHFFFAOYSA-M 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 15
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 12
- KYBOCQHDFLVQIB-UHFFFAOYSA-N 2-(4-methyl-2-sulfanylidene-3h-1,3-thiazol-5-yl)acetic acid Chemical compound CC=1N=C(S)SC=1CC(O)=O KYBOCQHDFLVQIB-UHFFFAOYSA-N 0.000 claims description 11
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 claims description 9
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 claims description 8
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 8
- -1 silver p-cresol sulfonate Chemical compound 0.000 claims description 7
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 6
- ASOKPJOREAFHNY-UHFFFAOYSA-N 1-Hydroxybenzotriazole Chemical compound C1=CC=C2N(O)N=NC2=C1 ASOKPJOREAFHNY-UHFFFAOYSA-N 0.000 claims description 6
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 6
- YGHRJJRRZDOVPD-UHFFFAOYSA-N 3-methylbutanal Chemical compound CC(C)CC=O YGHRJJRRZDOVPD-UHFFFAOYSA-N 0.000 claims description 6
- MUDSDYNRBDKLGK-UHFFFAOYSA-N 4-methylquinoline Chemical compound C1=CC=C2C(C)=CC=NC2=C1 MUDSDYNRBDKLGK-UHFFFAOYSA-N 0.000 claims description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 6
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 6
- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 claims description 6
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 6
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 claims description 6
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 6
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 claims description 6
- SUMDYPCJJOFFON-UHFFFAOYSA-N isethionic acid Chemical compound OCCS(O)(=O)=O SUMDYPCJJOFFON-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical compound OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 claims description 6
- ZFRKQXVRDFCRJG-UHFFFAOYSA-N skatole Chemical compound C1=CC=C2C(C)=CNC2=C1 ZFRKQXVRDFCRJG-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 5
- TWFSYIOOAAYYAL-UHFFFAOYSA-N 2,4,6-trichlorobenzaldehyde Chemical compound ClC1=CC(Cl)=C(C=O)C(Cl)=C1 TWFSYIOOAAYYAL-UHFFFAOYSA-N 0.000 claims description 4
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 claims description 4
- SRWILAKSARHZPR-UHFFFAOYSA-N 3-chlorobenzaldehyde Chemical compound ClC1=CC=CC(C=O)=C1 SRWILAKSARHZPR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- PZOUSPYUWWUPPK-UHFFFAOYSA-N indole Natural products CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 claims description 4
- RKJUIXBNRJVNHR-UHFFFAOYSA-N indolenine Natural products C1=CC=C2CC=NC2=C1 RKJUIXBNRJVNHR-UHFFFAOYSA-N 0.000 claims description 4
- JJVNINGBHGBWJH-UHFFFAOYSA-N ortho-vanillin Chemical compound COC1=CC=CC(C=O)=C1O JJVNINGBHGBWJH-UHFFFAOYSA-N 0.000 claims description 4
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 claims description 3
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 claims description 3
- XHANCLXYCNTZMM-UHFFFAOYSA-N 2,5-dimethyl-1,3-benzothiazole Chemical compound CC1=CC=C2SC(C)=NC2=C1 XHANCLXYCNTZMM-UHFFFAOYSA-N 0.000 claims description 3
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 claims description 3
- JWYUFVNJZUSCSM-UHFFFAOYSA-N 2-aminobenzimidazole Chemical compound C1=CC=C2NC(N)=NC2=C1 JWYUFVNJZUSCSM-UHFFFAOYSA-N 0.000 claims description 3
- AXZKCQSGDARVRL-UHFFFAOYSA-N 2-hydroxy-5-methylbenzenesulfonic acid Chemical compound CC1=CC=C(O)C(S(O)(=O)=O)=C1 AXZKCQSGDARVRL-UHFFFAOYSA-N 0.000 claims description 3
- XDJYNCLHESNUHA-UHFFFAOYSA-J 2-hydroxyethanesulfonate tin(4+) Chemical compound [Sn+4].OCCS([O-])(=O)=O.OCCS([O-])(=O)=O.OCCS([O-])(=O)=O.OCCS([O-])(=O)=O XDJYNCLHESNUHA-UHFFFAOYSA-J 0.000 claims description 3
- HVYYTJFWIYJPFE-UHFFFAOYSA-J 2-hydroxypropane-1-sulfonate tin(4+) Chemical compound [Sn+4].CC(O)CS([O-])(=O)=O.CC(O)CS([O-])(=O)=O.CC(O)CS([O-])(=O)=O.CC(O)CS([O-])(=O)=O HVYYTJFWIYJPFE-UHFFFAOYSA-J 0.000 claims description 3
- HSXUNHYXJWDLDK-UHFFFAOYSA-N 2-hydroxypropane-1-sulfonic acid Chemical compound CC(O)CS(O)(=O)=O HSXUNHYXJWDLDK-UHFFFAOYSA-N 0.000 claims description 3
- RYKLZUPYJFFNRR-UHFFFAOYSA-N 3-hydroxypiperidin-2-one Chemical compound OC1CCCNC1=O RYKLZUPYJFFNRR-UHFFFAOYSA-N 0.000 claims description 3
- WQPMYSHJKXVTME-UHFFFAOYSA-N 3-hydroxypropane-1-sulfonic acid Chemical compound OCCCS(O)(=O)=O WQPMYSHJKXVTME-UHFFFAOYSA-N 0.000 claims description 3
- GRIATXVEXOFBGO-UHFFFAOYSA-N 4-methyl-1,3-benzothiazol-2-amine Chemical compound CC1=CC=CC2=C1N=C(N)S2 GRIATXVEXOFBGO-UHFFFAOYSA-N 0.000 claims description 3
- BXRFQSNOROATLV-UHFFFAOYSA-N 4-nitrobenzaldehyde Chemical compound [O-][N+](=O)C1=CC=C(C=O)C=C1 BXRFQSNOROATLV-UHFFFAOYSA-N 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 3
- 244000060011 Cocos nucifera Species 0.000 claims description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- PVCJKHHOXFKFRP-UHFFFAOYSA-N N-acetylethanolamine Chemical compound CC(=O)NCCO PVCJKHHOXFKFRP-UHFFFAOYSA-N 0.000 claims description 3
- 229920002873 Polyethylenimine Polymers 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- PCSMJKASWLYICJ-UHFFFAOYSA-N Succinic aldehyde Chemical compound O=CCCC=O PCSMJKASWLYICJ-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- XJHABGPPCLHLLV-UHFFFAOYSA-N benzo[de]isoquinoline-1,3-dione Chemical compound C1=CC(C(=O)NC2=O)=C3C2=CC=CC3=C1 XJHABGPPCLHLLV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 229940117916 cinnamic aldehyde Drugs 0.000 claims description 3
- KJPRLNWUNMBNBZ-UHFFFAOYSA-N cinnamic aldehyde Natural products O=CC=CC1=CC=CC=C1 KJPRLNWUNMBNBZ-UHFFFAOYSA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000000174 gluconic acid Substances 0.000 claims description 3
- 235000012208 gluconic acid Nutrition 0.000 claims description 3
- 229940015043 glyoxal Drugs 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 3
- DOUHZFSGSXMPIE-UHFFFAOYSA-N hydroxidooxidosulfur(.) Chemical compound [O]SO DOUHZFSGSXMPIE-UHFFFAOYSA-N 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- KQJYDHWNYPRIRY-UHFFFAOYSA-N n-cyclohexylbenzamide Chemical compound C=1C=CC=CC=1C(=O)NC1CCCCC1 KQJYDHWNYPRIRY-UHFFFAOYSA-N 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 229940054441 o-phthalaldehyde Drugs 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- ZWLUXSQADUDCSB-UHFFFAOYSA-N phthalaldehyde Chemical compound O=CC1=CC=CC=C1C=O ZWLUXSQADUDCSB-UHFFFAOYSA-N 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 3
- 229940071536 silver acetate Drugs 0.000 claims description 3
- ULQFYBXXHIFWIQ-UHFFFAOYSA-M silver;2-hydroxyethanesulfonate Chemical compound [Ag+].OCCS([O-])(=O)=O ULQFYBXXHIFWIQ-UHFFFAOYSA-M 0.000 claims description 3
- GURNTNKIRDSILY-UHFFFAOYSA-M silver;ethanesulfonate Chemical compound [Ag+].CCS([O-])(=O)=O GURNTNKIRDSILY-UHFFFAOYSA-M 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- BATOPAZDIZEVQF-UHFFFAOYSA-N sorbic aldehyde Natural products CC=CC=CC=O BATOPAZDIZEVQF-UHFFFAOYSA-N 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 claims description 3
- BATOPAZDIZEVQF-MQQKCMAXSA-N (E,E)-2,4-hexadienal Chemical compound C\C=C\C=C\C=O BATOPAZDIZEVQF-MQQKCMAXSA-N 0.000 claims 1
- JTNFLOSMZURXJM-UHFFFAOYSA-N NS(S)(=O)=O Chemical compound NS(S)(=O)=O JTNFLOSMZURXJM-UHFFFAOYSA-N 0.000 claims 1
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 abstract description 10
- BPMFZUMJYQTVII-UHFFFAOYSA-N guanidinoacetic acid Chemical compound NC(=N)NCC(O)=O BPMFZUMJYQTVII-UHFFFAOYSA-N 0.000 abstract description 6
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 abstract description 3
- VLCDUOXHFNUCKK-UHFFFAOYSA-N N,N'-Dimethylthiourea Chemical compound CNC(=S)NC VLCDUOXHFNUCKK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052718 tin Inorganic materials 0.000 description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 28
- 239000004094 surface-active agent Substances 0.000 description 28
- 239000000243 solution Substances 0.000 description 27
- 239000010410 layer Substances 0.000 description 16
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- 229920000056 polyoxyethylene ether Polymers 0.000 description 16
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 15
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 15
- 229910052742 iron Inorganic materials 0.000 description 14
- HUMNYLRZRPPJDN-KWCOIAHCSA-N benzaldehyde Chemical group O=[11CH]C1=CC=CC=C1 HUMNYLRZRPPJDN-KWCOIAHCSA-N 0.000 description 13
- 239000002994 raw material Substances 0.000 description 13
- 238000003466 welding Methods 0.000 description 13
- 229910000881 Cu alloy Inorganic materials 0.000 description 12
- 239000003973 paint Substances 0.000 description 12
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- 230000000052 comparative effect Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 7
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- YODZTKMDCQEPHD-UHFFFAOYSA-N thiodiglycol Chemical compound OCCSCCO YODZTKMDCQEPHD-UHFFFAOYSA-N 0.000 description 4
- WJUAJNWYBNSKAO-UHFFFAOYSA-N 2-[2-(carboxymethylsulfanyl)butan-2-ylsulfanyl]acetic acid Chemical compound OC(=O)CSC(C)(CC)SCC(O)=O WJUAJNWYBNSKAO-UHFFFAOYSA-N 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- AMNPXXIGUOKIPP-UHFFFAOYSA-N [4-(carbamothioylamino)phenyl]thiourea Chemical compound NC(=S)NC1=CC=C(NC(N)=S)C=C1 AMNPXXIGUOKIPP-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
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- 229910052804 chromium Inorganic materials 0.000 description 2
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- 238000002425 crystallisation Methods 0.000 description 2
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- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- BRWIZMBXBAOCCF-UHFFFAOYSA-N hydrazinecarbothioamide Chemical compound NNC(N)=S BRWIZMBXBAOCCF-UHFFFAOYSA-N 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
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- 229920001223 polyethylene glycol Polymers 0.000 description 2
- DUIOPKIIICUYRZ-UHFFFAOYSA-N semicarbazide Chemical compound NNC(N)=O DUIOPKIIICUYRZ-UHFFFAOYSA-N 0.000 description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 2
- 235000019345 sodium thiosulphate Nutrition 0.000 description 2
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- 229950006389 thiodiglycol Drugs 0.000 description 2
- RSPCKAHMRANGJZ-UHFFFAOYSA-N thiohydroxylamine Chemical compound SN RSPCKAHMRANGJZ-UHFFFAOYSA-N 0.000 description 2
- 238000005491 wire drawing Methods 0.000 description 2
- 239000012991 xanthate Substances 0.000 description 2
- YHZQOKUDQQISEW-UHFFFAOYSA-N 4-Cumylphenol Natural products C1=CC(C(C)C)=CC=C1C1=CC=C(O)C=C1 YHZQOKUDQQISEW-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- GUTKPTLYNQSWGI-UHFFFAOYSA-N [Cu].[Sn].[Sn] Chemical compound [Cu].[Sn].[Sn] GUTKPTLYNQSWGI-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- QBDSZLJBMIMQRS-UHFFFAOYSA-N p-Cumylphenol Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=CC=C1 QBDSZLJBMIMQRS-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/60—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of tin
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
Abstract
The invention provides a tin alloy electroplating solution, which comprises organic mixed acid, organic tin salt, organic metal salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; wherein, calculated by weight portion, 1000 portions of deionized water, 600 portions of organic mixed acid 100, 40 to 100 portions of organic tin salt, 1 to 8 portions of organic metal salt, 50 to 160 portions of complexing agent, 30 to 70 portions of reducing agent, 20 to 100 portions of stabilizing agent, 5 to 20 portions of refiner and 3 to 15 portions of brightener; the organic metal salt comprises one of organic silver salt, organic copper salt and organic bismuth salt; the complexing agent comprises one or more of thiourea, 1, 3-dimethylthiourea, 2, 4-dithiobiuret, 2,4, 6-trithiotriurea, 2-dithiopyridine, 2-dithioaniline, tetramethylguanidine, guanidinoacetic acid, N-methyl guanidinoacetic acid and sulfhydryl chitosan.
Description
Technical Field
The invention relates to the technical field of electroplating, in particular to tin alloy electroplating solution.
Background
In recent years, for example, in the automobile field, electrification has rapidly advanced, and the number of circuits of electric equipment has increased, and therefore, downsizing and increase in the number of pins of connectors used have become remarkable. If the connector is multi-needled, even if the insertion force per needle is small, a large force is required for the entire connector when inserting the connector, and there is a possibility that productivity is lowered. Therefore, an attempt was made to reduce the insertion force of each needle by reducing the friction coefficient of the tin-plated copper alloy material.
A tin-plated copper alloy terminal material is widely used as a terminal material by performing copper plating and tin plating on a base material made of a copper alloy and then performing a reflow process to form a Cu — Sn alloy layer on a lower layer of an Sn-based surface layer of a surface layer.
The tin-copper-tin alloy has larger tin content, is easy to polish, has high reflectivity after polishing, and has hardness between nickel and chromium; the oxidation resistance in air is strong, and the corrosion resistance of the plating layer is increased along with the increase of the tin content in the plating layer.
For terminal tin-plated products with small volume and high precision, tin whiskers are easy to appear after tin plating is finished, most of the tin whiskers are as high as more than 100 micrometers, and the problems that two adjacent pins are easy to generate short circuit and the like in subsequent use are easily caused.
Therefore, aiming at the problems, the invention provides the tin alloy electroplating solution, which solves the problems of high welding temperature, coarse crystallization and easy tin whisker growth of tin electroplating alloy, effectively reduces the tin whiskers on a tinned product, ensures that the surface of a plated layer has good flatness, no crack and stable chemical property, and improves the safety and stability of the product in subsequent use.
Disclosure of Invention
In order to solve the above problems, the present invention provides a tin alloy plating solution, which comprises an organic mixed acid, an organic tin salt, an organic metal salt, a complexing agent, a reducing agent, a stabilizer, a refiner, a brightener, and deionized water; wherein, calculated by weight portion, 1000 portions of deionized water, 600 portions of organic mixed acid 100, 40 to 100 portions of organic tin salt, 1 to 8 portions of organic metal salt, 50 to 160 portions of complexing agent, 30 to 70 portions of reducing agent, 20 to 100 portions of stabilizing agent, 5 to 20 portions of refiner and 3 to 15 portions of brightener; the organic metal salt comprises one of organic silver salt, organic copper salt and organic bismuth salt; the complexing agent comprises one or more of thiourea, 1, 3-dimethylthiourea, 2, 4-dithiobiuret, 2,4, 6-trithiotriurea, 2-dithiopyridine, 2-dithioaniline, tetramethylguanidine, guanidinoacetic acid, N-methyl guanidinoacetic acid and sulfhydryl chitosan.
In one embodiment, the organic mixed acid is two or more of methanesulfonic acid, ethanesulfonic acid, 2-hydroxyethanesulfonic acid, 2-hydroxypropanesulfonic acid, 3-hydroxypropanesulfonic acid, citric acid, tartaric acid, lactic acid, gluconic acid, p-cresolsulfonic acid, sulfanilic acid, sulfosalicylic acid, oxalic acid.
In one embodiment, the organotin salt includes one or more of tin methanesulfonate, tin 2-hydroxyethanesulfonate, tin 2-hydroxypropanesulfonate.
In one embodiment, the organic silver salt comprises one or more of silver methanesulfonate, silver 2-hydroxyethanesulfonate, silver 2-hydroxypropanesulfonate, silver p-cresolsulfonate, silver acetate, silver ethanesulfonate, and silver sulfinate.
In one embodiment, the stabilizer comprises one or more of sodium thiosulfate, potassium thiosulfate, thiourea, xanthates, 2, 4-dithiobiuret, semicarbazide, thiosemicarbazide, 1, 4-phenylene bis (thiourea), thiodiglycol, β -thiodiglycol, dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid, [ (1-methylpropylidene) dithio ] diacetic acid, dithiodiglycolic acid.
In one embodiment, the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid, dithioglycolic acid; the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: (0.1-0.3): (0.5-2).
In one embodiment, the refining agent comprises one or more of sodium chloride, copper chloride, potassium chloride, ammonium chloride, bismuth nitrate, ethylene glycol, crotonic acid, acrylamide, crotonamide, crotonaldehyde, acetylethanolamine, 1, 8-naphthalimide, N-cyclohexylbenzamide, N-dimethylformamide, urea, sulfanylamide, acetamide, formamide, coconut diethanolamide, 2-mercaptobenzothiazole, dibenzothiazyl disulfide, 2-mercaptobenzimidazole, 2, 5-dimethylbenzothiazole, 2-amino-4-methylbenzothiazole, 2-aminobenzothiazole, 2-aminobenzimidazole, 3-methylindole, 4-methylquinoline.
In one embodiment, the brightener includes one or more of α -picolinic acid, benzaldehyde, 2,4, 6-trichlorobenzaldehyde, β -naphthalenesulfonic acid, m-chlorobenzaldehyde, p-nitrobenzaldehyde, salicylaldehyde, o-phthalaldehyde, formaldehyde, acetoacetal, acetaldehyde, butyraldehyde, isobutyraldehyde, propionaldehyde, n-valeraldehyde, acrolein, crotonaldehyde, glyoxal, isovaleraldehyde, hexanal, succinaldehyde, 2, 4-hexadienealdehyde, cinnamaldehyde, acetylacetone, imidazole, 2-vinylpyridine, indole, quinoline, ethanolamine, o-vanillin, polyvinyl alcohol, polyethyleneimine.
In one embodiment, the tin alloy plating solution is applied to an alloy terminal of a circuit board connector material.
In one embodiment, the circuit board connector material alloy terminals are made of, by weight percent, iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The above-described and other features, aspects, and advantages of the present application will become more apparent with reference to the following detailed description.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
"Polymer" means a polymeric compound prepared by polymerizing monomers of the same or different types. The generic term "polymer" embraces the terms "homopolymer", "copolymer", "terpolymer" and "interpolymer".
"interpolymer" means a polymer prepared by polymerizing at least two different monomers. The generic term "interpolymer" includes the term "copolymer" (which is generally used to refer to polymers prepared from two different monomers) and the term "terpolymer" (which is generally used to refer to polymers prepared from three different monomers). It also includes polymers made by polymerizing more monomers. "blend" means a polymer formed by two or more polymers being mixed together by physical or chemical means.
The invention provides a tin alloy electroplating solution, which comprises organic mixed acid, organic tin salt, organic metal salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; wherein, calculated by weight portion, 1000 portions of deionized water, 600 portions of organic mixed acid 100, 40 to 100 portions of organic tin salt, 1 to 8 portions of organic metal salt, 50 to 160 portions of complexing agent, 30 to 70 portions of reducing agent, 20 to 100 portions of stabilizing agent, 5 to 20 portions of refiner and 3 to 15 portions of brightener; the organic metal salt comprises one of organic silver salt, organic copper salt and organic bismuth salt; the complexing agent comprises one or more of thiourea, 1, 3-dimethylthiourea, 2, 4-dithiobiuret, 2,4, 6-trithiotriurea, 2-dithiopyridine, 2-dithioaniline, tetramethylguanidine, guanidinoacetic acid, N-methyl guanidinoacetic acid and sulfhydryl chitosan.
Preferably, the cleaning agent comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic metal salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner and 8 parts of brightener.
In one embodiment, the organometallic salt is an organic silver salt.
In one embodiment, the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid, mercaptochitosan.
In one embodiment, the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan in the complexing agent is 1: (0.1-0.5): (0.3-1.2); preferably, the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid and the mercapto chitosan is 1: 0.24: 0.72.
in one embodiment, the raw materials for preparing the mercaptochitosan comprise 2-mercapto-4-methyl-5-thiazoleacetic acid (CAS: 31090-12-7) and chitosan.
The preparation method of the mercapto chitosan comprises the following steps:
adding chitosan, 1-hydroxybenzotriazole and distilled water into a reactor, uniformly stirring, adding 2-mercapto-4-methyl-5-thiazoleacetic acid and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, reacting the pH of a reaction solution to 5 by using 1mol/L sodium hydroxide, reacting for 4h at room temperature, adding absolute ethyl alcohol, filtering, drying at 60 ℃ under reduced pressure for 10h, grinding, and storing at 5 ℃ at low temperature; the weight ratio of the chitosan to the 1-hydroxybenzotriazole to the distilled water is 1: 0.7: 30, of a nitrogen-containing gas; the weight ratio of the chitosan to the 2-mercapto-4-methyl-5-thiazoleacetic acid is 1: 3.6; the molar ratio of the 2-mercapto-4-methyl-5-thiazoleacetic acid to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 1: 1.05; the weight ratio of the chitosan to the absolute ethyl alcohol is 1: 10.
the chitosan has the characteristics of stronger complexing and adsorbing capacity, good mechanical property, stable chemical property and high fixing efficiency, the adhesion of the chitosan molecules after being connected with sulfydryl is further enhanced, the chitosan molecules can be effectively adsorbed to the surface of an electrode, the stability of the sulfydryl chitosan is good, and the service life of the sulfydryl chitosan is long. The sulfhydryl group is easy to oxidize to form a disulfide bond, thereby forming a network structure and having obvious adsorption effect.
The introduction of sulfhydryl groups imparts new biological properties to chitosan: when the content of sulfydryl is increased, the contact time between the mucous membrane and the thiolated chitosan is prolonged, and when the pH value is increased, the activity of sulfydryl is enhanced, and a plurality of disulfide bonds are formed inside the thiolated chitosan molecules.
According to the invention, the sulfhydryl chitosan is obtained by reacting chitosan with 2-sulfydryl-4-methyl-5-thiazoleacetic acid, has a network structure, and can form a flexible nickel plating layer which ensures the hardness and flexibility required by a plating layer while ensuring the stability of a plating solution; in addition, a higher plating layer formation speed can be provided, and the plating layer has excellent corrosion resistance and wear resistance even if the number of uses of the plating solution is increased.
In one embodiment, the organic mixed acid is two or more of methanesulfonic acid, ethanesulfonic acid, 2-hydroxyethanesulfonic acid, 2-hydroxypropanesulfonic acid, 3-hydroxypropanesulfonic acid, citric acid, tartaric acid, lactic acid, gluconic acid, p-cresolsulfonic acid, sulfanilic acid, sulfosalicylic acid, oxalic acid; preferably, the organic mixed acid is citric acid and sulfanilic acid.
In one embodiment, the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2.
in one embodiment, the organotin salt comprises one or more of tin methanesulfonate, tin 2-hydroxyethanesulfonate, tin 2-hydroxypropanesulfonate; preferably, the organotin salt is tin methanesulfonate.
In one embodiment, the organic silver salt comprises one or more of silver methanesulfonate, silver 2-hydroxyethanesulfonate, silver 2-hydroxypropanesulfonate, silver p-cresolsulfonate, silver acetate, silver ethanesulfonate, silver sulfinate; preferably, the organic silver salt is silver 2-hydroxypropanesulfonate.
In one embodiment, the stabilizer comprises one or more of sodium thiosulfate, potassium thiosulfate, thiourea, xanthates, 2, 4-dithiobiuret, semicarbazide, thiosemicarbazide, 1, 4-phenylenebis (thiourea), thiodiglycol, β -thiodiglycol, dibenzothiazothiofide, (ethane dithio subunit tetra) tetraacetic acid (CAS:10003-69-7), [ (1-methylpropylidene) dithio ] diacetic acid (CAS:4265-61-6), dithioglycolic acid (CAS: 505-73-7).
In one embodiment, the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid, dithioglycolic acid; the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: (0.1-0.3): (0.5-2); preferably, the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid, the dithioglycolic acid is 1: 0.15: 1.2.
in one embodiment, the refining agent comprises one or more of sodium chloride, copper chloride, potassium chloride, ammonium chloride, bismuth nitrate, ethylene glycol, crotonic acid, acrylamide, crotonamide, crotonaldehyde, acetylethanolamine, 1, 8-naphthalimide, N-cyclohexylbenzamide, N-dimethylformamide, urea, sulfanylamide, acetamide, formamide, coconut diethanolamide, 2-mercaptobenzothiazole, dibenzothiazyl disulfide, 2-mercaptobenzimidazole, 2, 5-dimethylbenzothiazole, 2-amino-4-methylbenzothiazole, 2-aminobenzothiazole, 2-aminobenzimidazole, 3-methylindole, 4-methylquinoline; preferably, the refiner is 2-aminobenzothiazole.
The refiner can refine grains, so that the grain refinement size reaches 5-50 nm, a fine-grain coating is finally obtained, and the brightness of the coating is improved.
In one embodiment, the brightener includes one or more of α -picolinic acid, benzaldehyde, 2,4, 6-trichlorobenzaldehyde, β -naphthalenesulfonic acid, m-chlorobenzaldehyde, p-nitrobenzaldehyde, salicylaldehyde, o-phthalaldehyde, formaldehyde, acetoacetal, acetaldehyde, butyraldehyde, isobutyraldehyde, propionaldehyde, n-valeraldehyde, acrolein, crotonaldehyde, glyoxal, isovaleraldehyde, hexanal, succinaldehyde, 2, 4-hexadienealdehyde, cinnamaldehyde, acetylacetone, imidazole, 2-vinylpyridine, indole, quinoline, ethanolamine, o-vanillin, polyvinyl alcohol, polyethyleneimine; preferably, the brightener comprises one or more of alpha-picolinic acid, benzaldehyde, 2,4, 6-trichlorobenzaldehyde, beta-naphthalenesulfonic acid, m-chlorobenzaldehyde, imidazole, 2-vinylpyridine, indole, quinoline, ethanolamine, o-vanillin, polyvinyl alcohol; most preferably, the brightener is benzaldehyde, beta-naphthalene sulfonic acid.
In one embodiment, the weight ratio of the benzaldehyde to the beta-naphthalenesulfonic acid in the brightener is 1: 0.3.
in one embodiment, the tin alloy electroplating bath further comprises 3-10 parts of a surfactant; the surfactant comprises one or more of polyethylene glycol (molecular weight 400-; preferably, the surfactant is one or more of polyethylene glycol (molecular weight 400-1500), nonylphenol polyoxyethylene ether (8-12EO), fatty alcohol polyoxyethylene ether, nonylphenol polyoxypropylene ether (5-12EO), polyoxyethylene-polyoxypropylene (EO-PO, EO, PO number ratio EO: PO ═ 2-4: 3) copolymer, 4-cumylphenol polyoxyethylene ether (7-11 EO); more preferably, the surfactant is nonylphenol polyoxyethylene ether (10 EO).
In one embodiment, the tin alloy plating solution is applied to an alloy terminal of a circuit board connector material.
In one embodiment, the circuit board connector material alloy terminals are made of, by weight percent, iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The production method of the alloy terminal of the circuit board connector material comprises the following steps of: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and the balance copper are smelted, formed by primary drawing, heat treated, drawn by rough drawing, heat treated by middle drawing (degaussing), drawn by fine drawing, cut to the required specification by a punch press, or smelted, formed by primary drawing, heat treated, tinned, drawn by rough drawing, heat treated by middle drawing (degaussing), drawn by fine drawing, and cut to the required specification by a punch press. In the drawing process after the first heat treatment, the inner hole of the die used for drawing the wire is square, flat or circular, and the final finished alloy wire is a square alloy wire or a flat alloy wire or a circular alloy wire determined by the shape of the inner hole of the die of the wire drawing according to different shapes of the inner hole of the die of the wire drawing, and is cut into a square terminal, a flat terminal or a circular terminal by a punch with a corresponding type. And during the second heat treatment, controlling the temperature at 1050-.
Scandium (Sc) having an atomic number of 21 belongs to a 3d type transition group metal, has a period equivalent to Ti, V, Cr, Mn, and an equivalent group to La, Ce, Pr, Nd, and therefore has the advantageous effects of both rare earth elements and transition group elements in a copper alloy. The trace scandium added into the copper alloy can obviously refine grains and inhibit recrystallization, and obviously improve the strength corrosion resistance and the welding performance while maintaining the excellent conductivity of the copper alloy.
Sc has strong metamorphic effect, can refine grains in a friction welding seam melting zone, and obviously reduce welding crack tendency. Meanwhile, Sc can effectively inhibit recrystallization of a heat affected zone, the subgrain structure of the matrix is directly transited to an as-cast zone of the weld joint, so that the weld joint transition zone or the heat affected zone which should have the recrystallized structure does not have the recrystallized structure, and as-cast grains in the weld joint are refined along with the increase of Sc content.
Vanadium is a transition metal, has a BCC structure at normal temperature and normal pressure, has a lattice structure which undergoes phase change under different pressures, and can be added into the copper alloy in a trace amount, so that crystal grains can be obviously refined, recrystallization can be inhibited, and the strength corrosion resistance and the welding performance of the copper alloy can be further obviously improved while the excellent conductivity of the copper alloy is maintained.
The preparation process of the electroplating solution comprises the following steps:
adding deionized water into the electroplating bath, adding required amounts of organic mixed acid mixed solution, organic tin salt and organic silver salt, mixing, stirring uniformly, standing for 1h, sequentially adding complexing agent, reducing agent, stabilizing agent and refiner according to required amounts, mixing, stirring uniformly, standing for 0.5h, adding required amount of brightener, and stirring uniformly for later use; in order to obtain better electroplating effect, the pH environment of the electroplating solution is 4.5-6.5.
Tin whiskers are an elongated tin single crystal grown from the surface of a tin layer or tin alloy layer. Tin whiskers are generally in a linear, curved, kinky or annular structure, have high current loading capacity and seriously damage electronic components.
There are two indispensable conditions for the production of tin whiskers: firstly, the tin layer needs continuous compressive stress to maintain the driving force; secondly, the compressive stress continuously generated in the tin layer is maintained in dynamic balance through the growth of tin whiskers.
According to the invention, the electrode potential of copper is reduced by using a complex formed by a complexing agent and tin divalent ions, the copper is replaced by tin through a replacement reaction, and after the surface of the copper is completely covered by the tin, the tin is deposited on the surface of the copper through autocatalytic reduction, so that a tin-plated layer is continuously thickened; meanwhile, organic mixed acid, organic silver salt, dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithio glycolic acid are added to effectively overcome the tin whisker generated on the tin coating. The stabilizer is added, so that the tin plating solution can be prevented from generating precipitation, and the surface oxidation of the tin plating layer can be prevented. In addition, Ag and Sn are co-plated, so that the aim of alloying and retarding the growth of tin whisker is further fulfilled.
According to the invention, through using the scandium-containing copper alloy and the vanadium-containing copper alloy, the copper alloys are mutually diffused and are subjected to dynamic recrystallization to achieve metallurgical bonding, so that the strength of the terminal is obviously improved, and the welding performance and the corrosion resistance of the terminal are greatly improved; in addition, the electrode potential of copper is reduced by a complex formed by a complexing agent and tin divalent ions, organic mixed acid, organic silver salt, dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithio glycolic acid are added to effectively overcome the problem that tin whiskers are generated on a tin coating, and Ag and Sn are co-plated to further achieve alloying and slow down the growth of tin whiskers.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the raw materials used are commercially available from national chemical reagents, unless otherwise specified.
Example 1
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.24: 0.72, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.15: 1.2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan comprises the following steps:
adding chitosan, 1-hydroxybenzotriazole and distilled water into a reactor, uniformly stirring, adding 2-mercapto-4-methyl-5-thiazoleacetic acid and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, reacting the pH of a reaction solution to 5 by using 1mol/L sodium hydroxide, reacting for 4h at room temperature, adding absolute ethyl alcohol, filtering, drying at 60 ℃ under reduced pressure for 10h, grinding, and storing at 5 ℃ at low temperature; the weight ratio of the chitosan to the 1-hydroxybenzotriazole to the distilled water is 1: 0.7: 30, of a nitrogen-containing gas; the weight ratio of the chitosan to the 2-mercapto-4-methyl-5-thiazoleacetic acid is 1: 3.6; the molar ratio of the 2-mercapto-4-methyl-5-thiazoleacetic acid to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 1: 1.05; the weight ratio of the chitosan to the absolute ethyl alcohol is 1: 10.
example 2
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.5: 0.3, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.15: 1.2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Example 3
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.1: 1.2, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.15: 1.2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Example 4
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.24: 0.72, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid (CAS: 31090-12-7) and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.1: 2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Example 5
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.24: 0.72, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid (CAS: 31090-12-7) and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.3: 0.5; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Comparative example 1
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
wherein the complexing agent is 2, 4-dithiobiuret or N-methylguanidinoacetic acid, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid is 1: 0.24, the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.15: 1.2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
Comparative example 2
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is sulfhydryl chitosan, and the preparation raw materials of the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid (CAS: 31090-12-7) and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.15: 1.2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Comparative example 3
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.24: 0.72, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid (CAS: 31090-12-7) and chitosan; the organic mixed acid is citric acid; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.15: 1.2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Comparative example 4
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.24: 0.72, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid (CAS: 31090-12-7) and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide sulfur; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Comparative example 5
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.24: 0.72, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid (CAS: 31090-12-7) and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is (ethane dithio subunit tetra) tetraacetic acid; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Comparative example 6
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.24: 0.72, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid (CAS: 31090-12-7) and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide and dithiodiglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the dithiodiglycolic acid is 1: 1.2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
Comparative example 7
The tin alloy electroplating solution comprises organic mixed acid, organic tin salt, organic silver salt, a complexing agent, a reducing agent, a stabilizing agent, a refining agent, a brightening agent and deionized water; the water-soluble paint comprises, by weight, 1000 parts of deionized water, 350 parts of organic mixed acid, 80 parts of organic tin salt, 2 parts of organic silver salt, 100 parts of complexing agent, 45 parts of reducing agent, 60 parts of stabilizing agent, 10 parts of refiner, 8 parts of brightener and 6 parts of surfactant;
the complexing agent is 2, 4-dithiobiuret, N-methylguanidinoacetic acid and mercaptochitosan, and the weight ratio of the 2, 4-dithiobiuret to the N-methylguanidinoacetic acid to the mercaptochitosan is 1: 0.24: 0.72, the raw materials for preparing the sulfhydryl chitosan comprise 2-sulfhydryl-4-methyl-5-thiazole acetic acid (CAS: 31090-12-7) and chitosan; the organic mixed acid is citric acid and sulfanilic acid, and the weight ratio of the citric acid to the sulfanilic acid is 1: 1.2; the organic tin salt is tin methane sulfonate; the organic silver salt is silver 2-hydroxypropanesulfonate; the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid and dithioglycolic acid, and the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: 0.15: 1.2; the refiner is 2-aminobenzothiazole; the brightener is benzaldehyde and beta-naphthalene sulfonic acid, and the weight ratio of the benzaldehyde to the beta-naphthalene sulfonic acid is 1: 0.3; the surfactant is nonylphenol polyoxyethylene ether (10 EO);
the circuit board connector material alloy terminal is composed of iron: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2% scandium 0.0035% and the balance copper.
The preparation method of the mercapto chitosan is the same as that of example 1.
And (3) performance testing:
1. an accelerating test method of JEDEC201 is adopted in a tin whisker growth experiment under the temperature circulation condition, and the parameters are as follows: -55 ℃ (+ 0/-10 ℃) to +85 ℃ (+ 10/-0 ℃), atmospheric environment, and tin whisker growth is observed after every 500 cycles in the course of 3 cycles/h experiment; in total, 1500 cycles were performed, and the growth state of tin whiskers was observed three times.
2. Test of welding Performance
Welding the two samples, wherein the welding area is 5 x 5mm, stretching the welded samples by using an HY-1080 type universal stretching machine, and the pull force is greater than 1000N, so that the welding performance is good; the pulling force is larger than 800N and smaller than 1000N, and the welding performance is general; the pulling force is less than 800N, and the welding performance is poor.
3. Test of Corrosion resistance
And (3) taking the area of the prepared sample as 10mm by 10mm to perform an acid salt spray test, testing for 24h, and observing the number of rust points.
Table 1 results of performance testing
The data show that the tin alloy electroplating solution provided by the invention solves the problems of high welding temperature, coarse crystallization and easy tin whisker growth of tin electroplating alloy, effectively reduces the tin whiskers on a tinned product, ensures that the surface of a plated layer has good flatness, no crack and stable chemical property, and improves the safety and stability of the product in subsequent use.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (8)
1. The tin alloy electroplating solution is characterized by comprising organic mixed acid, organic tin salt, organic metal salt, complexing agent, reducing agent, stabilizing agent, refining agent, brightening agent and deionized water; wherein, calculated by weight portion, 1000 portions of deionized water, 600 portions of organic mixed acid 100, 40 to 100 portions of organic tin salt, 1 to 8 portions of organic metal salt, 50 to 160 portions of complexing agent, 30 to 70 portions of reducing agent, 20 to 100 portions of stabilizing agent, 5 to 20 portions of refiner and 3 to 15 portions of brightener; the organic metal salt comprises one of organic silver salt, organic copper salt and organic bismuth salt; the complexing agent is 2, 4-dithiobiuret, N-methyl guanidinoacetic acid and sulfydryl chitosan, and the weight ratio of the complexing agent to the complexing agent is 1: (0.1-0.5): (0.3 to 1.2); the stabilizer is dibenzothiazyl disulfide, (ethane dithio subunit tetra) tetraacetic acid, dithioglycolic acid; the weight ratio of the dibenzothiazyl disulfide to the (ethane dithio subunit tetra) tetraacetic acid and the dithioglycolic acid is 1: (0.1-0.3): (0.5-2);
the preparation method of the mercapto chitosan comprises the following steps:
adding chitosan, 1-hydroxybenzotriazole and distilled water into a reactor, uniformly stirring, adding 2-mercapto-4-methyl-5-thiazoleacetic acid and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, reacting the pH of a reaction solution to 5 by using 1mol/L sodium hydroxide, reacting for 4h at room temperature, adding absolute ethyl alcohol, filtering, drying at 60 ℃ under reduced pressure for 10h, grinding, and storing at 5 ℃ at low temperature; the weight ratio of the chitosan to the 1-hydroxybenzotriazole to the distilled water is 1: 0.7: 30, of a nitrogen-containing gas; the weight ratio of the chitosan to the 2-mercapto-4-methyl-5-thiazoleacetic acid is 1: 3.6; the molar ratio of the 2-mercapto-4-methyl-5-thiazoleacetic acid to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 1: 1.05; the weight ratio of the chitosan to the absolute ethyl alcohol is 1: 10.
2. the tin alloy plating solution as recited in claim 1, wherein the organic mixed acid is two or more of methanesulfonic acid, ethanesulfonic acid, 2-hydroxyethanesulfonic acid, 2-hydroxypropanesulfonic acid, 3-hydroxypropanesulfonic acid, citric acid, tartaric acid, lactic acid, gluconic acid, p-cresol sulfonic acid, sulfanilic acid, sulfosalicylic acid, and oxalic acid.
3. The tin alloy plating solution of claim 1, wherein the organotin salt comprises one or more of tin methanesulfonate, tin 2-hydroxyethanesulfonate, and tin 2-hydroxypropanesulfonate.
4. The tin alloy plating solution of claim 1, wherein the organic silver salt comprises one or more of silver methanesulfonate, silver 2-hydroxyethanesulfonate, silver 2-hydroxypropanesulfonate, silver p-cresol sulfonate, silver acetate, silver ethanesulfonate, and silver sulfinate.
5. The tin alloy plating solution as recited in claim 1, wherein the refining agent comprises one or more of sodium chloride, copper chloride, potassium chloride, ammonium chloride, bismuth nitrate, ethylene glycol, crotonic acid, acrylamide, crotonamide, crotonaldehyde, acetylethanolamine, 1, 8-naphthalimide, N-cyclohexylbenzamide, N-dimethylformamide, urea, sulfanylsulfonamide, acetamide, formamide, coconut diethanolamide, 2-mercaptobenzothiazole, dibenzothiazyl disulfide, 2-mercaptobenzimidazole, 2, 5-dimethylbenzothiazole, 2-amino-4-methylbenzothiazole, 2-aminobenzothiazole, 2-aminobenzimidazole, 3-methylindole, and 4-methylquinoline.
6. The tin alloy plating solution as set forth in claim 1, wherein the brightener includes one or more of α -picolinic acid, benzaldehyde, 2,4, 6-trichlorobenzaldehyde, β -naphthalenesulfonic acid, m-chlorobenzaldehyde, p-nitrobenzaldehyde, salicylaldehyde, o-phthalaldehyde, formaldehyde, acetoacetal, acetaldehyde, butyraldehyde, isobutyraldehyde, propionaldehyde, n-valeraldehyde, acrolein, crotonaldehyde, glyoxal, isovaleraldehyde, hexanal, succinaldehyde, 2, 4-hexadienal, cinnamaldehyde, acetylacetone, imidazole, 2-vinylpyridine, indole, quinoline, ethanolamine, o-vanillin, polyvinyl alcohol, and polyethyleneimine.
7. The tin alloy plating solution as set forth in claim 1, wherein the tin alloy plating solution is applied to an alloy terminal of a circuit board connector member.
8. The tin alloy plating solution as set forth in claim 7, wherein said circuit board connector material alloy terminals are composed of, by weight: 8.5%, manganese: 15%, silicon: 0.07%, nickel: 0.2%, scandium 0.0035%, vanadium: 0.0023% and balance copper.
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| CN109183096B (en) * | 2018-11-08 | 2021-04-23 | 杭州云会五金电镀有限公司 | Surface electroplating liquid for alloy and electroplating process |
| CN109594107A (en) * | 2018-11-13 | 2019-04-09 | 南通赛可特电子有限公司 | A kind of electrotinning additive and preparation method thereof |
| CN109972180B (en) * | 2019-04-12 | 2020-12-18 | 博敏电子股份有限公司 | New use of 2, 2' -dithiodipyridine, electroplating hole-filling additive using the same and electroplating method using the additive |
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| CN112359380A (en) * | 2020-10-23 | 2021-02-12 | 珠海鑫通化工有限公司 | Electroplating solution for chemical tinning of passive component |
| CN113604846A (en) * | 2021-03-29 | 2021-11-05 | 宁波德洲精密电子有限公司 | Surface treatment process for integrated circuit lead frame |
| CN116695204B (en) * | 2023-08-08 | 2023-11-03 | 宁波德洲精密电子有限公司 | IC frame tinning processing method |
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