JP5416330B2 - 金めっき液用亜硫酸金塩水溶液の製造方法 - Google Patents
金めっき液用亜硫酸金塩水溶液の製造方法 Download PDFInfo
- Publication number
- JP5416330B2 JP5416330B2 JP2005066456A JP2005066456A JP5416330B2 JP 5416330 B2 JP5416330 B2 JP 5416330B2 JP 2005066456 A JP2005066456 A JP 2005066456A JP 2005066456 A JP2005066456 A JP 2005066456A JP 5416330 B2 JP5416330 B2 JP 5416330B2
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- JP
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- Prior art keywords
- gold
- sulfite
- solution
- plating solution
- gold plating
- 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.)
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- 239000010931 gold Substances 0.000 title claims description 178
- 229910052737 gold Inorganic materials 0.000 title claims description 178
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims description 177
- 238000007747 plating Methods 0.000 title claims description 157
- 239000000243 solution Substances 0.000 title claims description 154
- SRCZENKQCOSNAI-UHFFFAOYSA-H gold(3+);trisulfite Chemical compound [Au+3].[Au+3].[O-]S([O-])=O.[O-]S([O-])=O.[O-]S([O-])=O SRCZENKQCOSNAI-UHFFFAOYSA-H 0.000 title claims description 84
- 239000007864 aqueous solution Substances 0.000 title claims description 79
- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 claims description 55
- WDZVNNYQBQRJRX-UHFFFAOYSA-K gold(iii) hydroxide Chemical compound O[Au](O)O WDZVNNYQBQRJRX-UHFFFAOYSA-K 0.000 claims description 55
- 239000002245 particle Substances 0.000 claims description 50
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- 239000003638 chemical reducing agent Substances 0.000 claims description 18
- 150000003839 salts Chemical class 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000008139 complexing agent Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 5
- 239000006172 buffering agent Substances 0.000 claims description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 claims 1
- ZWZLRIBPAZENFK-UHFFFAOYSA-J sodium;gold(3+);disulfite Chemical compound [Na+].[Au+3].[O-]S([O-])=O.[O-]S([O-])=O ZWZLRIBPAZENFK-UHFFFAOYSA-J 0.000 description 46
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 23
- -1 aliphatic saturated alcohol Chemical class 0.000 description 13
- 238000003756 stirring Methods 0.000 description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 8
- 229940001482 sodium sulfite Drugs 0.000 description 8
- 235000010265 sodium sulphite Nutrition 0.000 description 8
- 229940101006 anhydrous sodium sulfite Drugs 0.000 description 7
- 238000007796 conventional method Methods 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- 150000001735 carboxylic acids Chemical class 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 239000003446 ligand Substances 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 239000000872 buffer Substances 0.000 description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 3
- 235000015165 citric acid Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007772 electroless plating Methods 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 239000012088 reference solution Substances 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-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
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 2
- HTKFORQRBXIQHD-UHFFFAOYSA-N allylthiourea Chemical compound NC(=S)NCC=C HTKFORQRBXIQHD-UHFFFAOYSA-N 0.000 description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- ZETCGWYACBNPIH-UHFFFAOYSA-N azane;sulfurous acid Chemical compound N.OS(O)=O ZETCGWYACBNPIH-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 239000001630 malic acid Substances 0.000 description 2
- 235000011090 malic acid Nutrition 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- DJEHXEMURTVAOE-UHFFFAOYSA-M potassium bisulfite Chemical compound [K+].OS([O-])=O DJEHXEMURTVAOE-UHFFFAOYSA-M 0.000 description 2
- 235000010259 potassium hydrogen sulphite Nutrition 0.000 description 2
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 2
- 235000019252 potassium sulphite Nutrition 0.000 description 2
- 229940079827 sodium hydrogen sulfite Drugs 0.000 description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N thiocyanic acid Chemical compound SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- JAEZSIYNWDWMMN-UHFFFAOYSA-N 1,1,3-trimethylthiourea Chemical compound CNC(=S)N(C)C JAEZSIYNWDWMMN-UHFFFAOYSA-N 0.000 description 1
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
- JAJIPIAHCFBEPI-UHFFFAOYSA-N 9,10-dioxoanthracene-1-sulfonic acid Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)O JAJIPIAHCFBEPI-UHFFFAOYSA-N 0.000 description 1
- 239000004475 Arginine Substances 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- PDQAZBWRQCGBEV-UHFFFAOYSA-N Ethylenethiourea Chemical compound S=C1NCCN1 PDQAZBWRQCGBEV-UHFFFAOYSA-N 0.000 description 1
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 1
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- VLCDUOXHFNUCKK-UHFFFAOYSA-N N,N'-Dimethylthiourea Chemical compound CNC(=S)NC VLCDUOXHFNUCKK-UHFFFAOYSA-N 0.000 description 1
- FLVIGYVXZHLUHP-UHFFFAOYSA-N N,N'-diethylthiourea Chemical compound CCNC(=S)NCC FLVIGYVXZHLUHP-UHFFFAOYSA-N 0.000 description 1
- KQJQICVXLJTWQD-UHFFFAOYSA-N N-Methylthiourea Chemical compound CNC(N)=S KQJQICVXLJTWQD-UHFFFAOYSA-N 0.000 description 1
- IPCRBOOJBPETMF-UHFFFAOYSA-N N-acetylthiourea Chemical compound CC(=O)NC(N)=S IPCRBOOJBPETMF-UHFFFAOYSA-N 0.000 description 1
- XGEGHDBEHXKFPX-UHFFFAOYSA-N N-methylthiourea Natural products CNC(N)=O XGEGHDBEHXKFPX-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- WYNAWAKUKHILJH-UHFFFAOYSA-L S(=O)([O-])[O-].[Au+3].[Na+].[Au+3] Chemical compound S(=O)([O-])[O-].[Au+3].[Na+].[Au+3] WYNAWAKUKHILJH-UHFFFAOYSA-L 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 description 1
- 229940072107 ascorbate Drugs 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- GABPAXJCPQEORA-UHFFFAOYSA-K azanium;gold(3+);disulfite Chemical compound [NH4+].[Au+3].[O-]S([O-])=O.[O-]S([O-])=O GABPAXJCPQEORA-UHFFFAOYSA-K 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- VYGAQHDGEYQIJU-UHFFFAOYSA-N butanedioic acid;phthalic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)C1=CC=CC=C1C(O)=O VYGAQHDGEYQIJU-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- HUQOFZLCQISTTJ-UHFFFAOYSA-N diethylaminoboron Chemical compound CCN([B])CC HUQOFZLCQISTTJ-UHFFFAOYSA-N 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 229940042400 direct acting antivirals phosphonic acid derivative Drugs 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 229940093915 gynecological organic acid Drugs 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- BRWIZMBXBAOCCF-UHFFFAOYSA-N hydrazinecarbothioamide Chemical compound NNC(N)=S BRWIZMBXBAOCCF-UHFFFAOYSA-N 0.000 description 1
- 150000002429 hydrazines Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 1
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical compound NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 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
- PHFFANVCGVJLOM-UHFFFAOYSA-N n-diethylboranylethanamine Chemical compound CCNB(CC)CC PHFFANVCGVJLOM-UHFFFAOYSA-N 0.000 description 1
- BORTXUKGEOWSPS-UHFFFAOYSA-N n-dimethylboranylmethanamine Chemical compound CNB(C)C BORTXUKGEOWSPS-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 150000003007 phosphonic acid derivatives Chemical class 0.000 description 1
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- RRDWZGMHSCBIGX-UHFFFAOYSA-J potassium;gold(3+);disulfite Chemical compound [K+].[Au+3].[O-]S([O-])=O.[O-]S([O-])=O RRDWZGMHSCBIGX-UHFFFAOYSA-J 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- ZNZJJSYHZBXQSM-UHFFFAOYSA-N propane-2,2-diamine Chemical compound CC(C)(N)N ZNZJJSYHZBXQSM-UHFFFAOYSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- KZVLNAGYSAKYMG-UHFFFAOYSA-N pyridine-2-sulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=N1 KZVLNAGYSAKYMG-UHFFFAOYSA-N 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- PODWXQQNRWNDGD-UHFFFAOYSA-L sodium thiosulfate pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[O-]S([S-])(=O)=O PODWXQQNRWNDGD-UHFFFAOYSA-L 0.000 description 1
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- YTQVHRVITVLIRD-UHFFFAOYSA-L thallium sulfate Chemical compound [Tl+].[Tl+].[O-]S([O-])(=O)=O YTQVHRVITVLIRD-UHFFFAOYSA-L 0.000 description 1
- 229940119523 thallium sulfate Drugs 0.000 description 1
- 229910000374 thallium(I) sulfate Inorganic materials 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Chemically Coating (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Description
パーティクル増加率[%]=100×(N2−N1)/N1 で定義される。
金50gを王水100mLに溶解した後、40質量%の水酸化ナトリウム水溶液を用いてpH8に中和し、水酸化金を沈殿させた。炉別後、水で洗浄して得られた水酸化金を以下の全ての製造例で用いた。
<亜硫酸金ナトリウム水溶液(1)の調製>
50gの金から得られた上記水酸化金を、水900mLの水中に攪拌しながら分散させ、液温を60℃以上65℃以下に制御しながら、無水亜硫酸ナトリウム粉末195gを、2時間かけて少しずつ添加し反応させた。その後、水酸化金が完全に溶解してから更に1時間、同一温度で攪拌を続けた後、90℃以上95℃以下に昇温して、2時間攪拌させた。最後に全量が1Lとなるように水を加えて調節し、金濃度50g/Lの亜硫酸金ナトリウム水溶液(1)を得た。
<亜硫酸金ナトリウム水溶液(2)の調製>
50gの金から得られた上記水酸化金を、水900mLの水中に攪拌しながら分散させ、液温を50℃以上55℃以下に制御しながら、無水亜硫酸ナトリウム粉末195gを30分かけて添加し反応させた。その後、水酸化金が完全に溶解してから更に2時間、同一温度で攪拌を続けた後、80℃以上85℃以下に昇温して、2時間攪拌させた。最後に全量が1Lとなるように水を加えて調節し、金濃度50g/Lの亜硫酸金ナトリウム水溶液(2)を得た。
<亜硫酸金ナトリウム水溶液(3)の調製>
特開平3−146419号公報の実施例に準じて、50gの金から得られた水酸化金に、900mLの水と水酸化ナトリウムを加えて80℃に加熱し、水酸化金を完全に溶解させて均一な水酸化金溶液とした。そこに、無水亜硫酸ナトリウム粉末195gを2時間かけて、攪拌しながらゆっくり加えて反応させた。添加を終えてからも、更に2時間攪拌を続けた。最後に全量が1Lとなるように水を加えて調節し、金濃度50g/Lの亜硫酸金ナトリウム水溶液(3)を得た。
<亜硫酸金ナトリウム水溶液(4)の調製>
50gの金から得られた上記水酸化金を、水900mLの水中に攪拌しながら分散させ、液温を75℃以上80℃以下に制御しながら、無水亜硫酸ナトリウム粉末195gを30分かけて添加し反応させた。その後、水酸化金が溶解してから更に2時間攪拌させてから、90℃以上95℃以下に昇温して、2時間攪拌させた。最後に全量が1Lとなるように水を加えて調節し、金濃度50g/Lの亜硫酸金ナトリウム水溶液(4)を得た。
<亜硫酸金ナトリウム水溶液(5)の調製>
50gの金から得られた上記水酸化金を、水900mLの水中に攪拌しながら分散させ、液温を50℃から75℃まで、1.5時間かけてゆっくり昇温させながら、無水亜硫酸ナトリウム粉末195gをゆっくり加えて反応させた。この時70℃以上になった時点でも未溶解の水酸化金が存在していた。その後、水酸化金が完全に溶解したら、90℃以上95℃以下に昇温して、2時間攪拌させた。最後に全量が1Lとなるように水を加えて調節し、金濃度50g/Lの亜硫酸金ナトリウム水溶液(5)を得た。
<亜硫酸金ナトリウム水溶液(6)の調製>
50gの金から得られた上記水酸化金を、水900mLの水中に攪拌しながら分散させ、液温を60℃以上65℃以下に制御しながら、亜硫酸ナトリウム195gを加えて反応させた。その後、水酸化金が完全に溶解してから、75℃以上77℃以下に昇温して、2時間攪拌させた。最後に全量が1Lとなるように水を加えて調節し、金濃度50g/Lの亜硫酸金ナトリウム水溶液(6)を得た。
亜硫酸金ナトリウム水溶液を、孔径0.1μmのメンブランフィルターを使い濾過し、自動式液中微粒子計測器KL−20(リオン株式会社製)を用い、溶液10ml中の大きさ2μm以上のパーティクル数を計測し、その値をN1とした。その後、20℃で24時間静置保管後、同様にKL−20を用い、溶液10ml中の大きさ2μm以上のパーティクル数を計測して、その値をN2とした。下記式で表される値を求め、「パーティクル増加率」と定義した。
パーティクル増加率[%]=100×(N2−N1)/N1
<無電解金めっき液のめっきランニング安定性評価>
上記亜硫酸金ナトリウム水溶液(1)ないし(6)を金源として、それぞれ以下の組成の無電解金めっき液を調製した。それぞれ、番号を対応させて、無電解金めっき液(1)ないし(6)とする。これら無電解金めっき液のpHは、全て7.0であった。
上記亜硫酸金ナトリウム水溶液 金換算で2.5g/L
チオ硫酸ナトリウム5水塩 50g/L
無水亜硫酸ナトリウム 25g/L
塩化アンモニウム 5g/L
硼酸 20g/L
アスコルビン酸ナトリウム 5g/L
<無電解金めっき液のめっきランニング安定性評価>
上記亜硫酸金水溶液(1)と(3)を金源として用いて、それぞれ番号を対応させて、下記の組成で、電解金めっき液(1)と(3)を調製した。これら電解金めっき液のpHは、全て7.5であった。
上記亜硫酸金溶液 金換算で10g/L
無水亜硫酸ナトリウム 20g/L
無水燐酸水素二ナトリウム 20g/L
硫酸タリウム タリウム換算で10ppm
金濃度50g/Lの上記亜硫酸金ナトリウム水溶液(1)を水で希釈して、金濃度、2.5g/L、5g/L、10g/L、25g/Lの亜硫酸金ナトリウム水溶液を調製した。それらをこの順に亜硫酸金ナトリウム水溶液(7)(8)(9)(10)とする。
上記亜硫酸金ナトリウム水溶液(7)及び(11)に、それぞれ還元剤であるチオ尿素を5g/L配合して、参考液(1)及び(2)を調製した。それらの液のパーティクル増加率を表5に示す。
以 上
Claims (11)
- 亜硫酸金塩及び亜硫酸塩を含有し、20℃で24時間静置保管することによって測定したパーティクル増加率が20%以下である金めっき液用亜硫酸金塩水溶液の製造方法であって、該亜硫酸金塩を、水酸化金を水中に懸濁させた状態で亜硫酸塩を添加して水酸化金と反応させる工程を含む方法により得ることを特徴とする金めっき液用亜硫酸金塩水溶液の製造方法。
- 亜硫酸金塩を金換算で1〜200g/L及び亜硫酸塩を前記亜硫酸金塩の2〜20倍モル含有する請求項1記載の金めっき液用亜硫酸金塩水溶液の製造方法。
- 水酸化金を金換算で10〜200g/L、かつ亜硫酸塩を前記水酸化金の2.5〜25倍モル用いる方法により得られるものである請求項1又は請求項2記載の金めっき液用亜硫酸金塩水溶液の製造方法。
- 亜硫酸塩を添加して水酸化金と反応させる工程において、前記水酸化金が溶解するまでは、液温70℃以下に制御して反応を行う請求項1ないし請求項3の何れかの請求項記載の金めっき液用亜硫酸金塩水溶液の製造方法。
- 亜硫酸塩を添加して水酸化金と反応させる工程において、前記水酸化金が溶解するまでは、液温70℃以下に制御して反応を行い、水酸化金が溶解した後に、液温80℃以上で反応を行う請求項1ないし請求項4の何れかの請求項記載の金めっき液用亜硫酸金塩水溶液の製造方法。
- 請求項1ないし請求項5の何れかの請求項記載の製造方法で製造された金めっき液用亜硫酸金塩水溶液に、少なくとも更に、還元剤及び/又は緩衝剤を含有させることを特徴とする無電解金めっき液の製造方法。
- 更に、錯化剤を含有させる請求項6記載の無電解金めっき液の製造方法。
- 請求項1ないし請求項5の何れかの請求項記載の製造方法で製造された金めっき液用亜硫酸金塩水溶液に、少なくとも更に、電導塩及び/又は結晶調整剤を含有させることを特徴とする電解金めっき液の製造方法。
- 更に、錯化剤を含有させる請求項8記載の電解金めっき液の製造方法。
- 請求項1ないし請求項5の何れかの請求項記載の製造方法で製造された金めっき液用亜硫酸金塩水溶液を用いて無電解金めっき液を製造して金めっき皮膜を製造することを特徴とする金めっき皮膜の製造方法。
- 請求項1ないし請求項5の何れかの請求項記載の製造方法で製造された金めっき液用亜硫酸金塩水溶液を用いて電解金めっき液を製造して金めっき皮膜を製造することを特徴とする金めっき皮膜の製造方法。
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US7981202B2 (en) * | 2007-02-28 | 2011-07-19 | Kojima Chemicals Co., Ltd. | Electroless pure palladium plating solution |
JP5312842B2 (ja) * | 2008-05-22 | 2013-10-09 | 関東化学株式会社 | 電解合金めっき液及びそれを用いるめっき方法 |
JP5175156B2 (ja) * | 2008-09-30 | 2013-04-03 | 松田産業株式会社 | パラジウム合金めっき液およびめっき方法 |
JP6299750B2 (ja) * | 2013-04-04 | 2018-03-28 | 日立化成株式会社 | 生体物質捕獲用のフィルター |
CN106637314B (zh) * | 2016-12-15 | 2018-08-31 | 广东光华科技股份有限公司 | 一种无氰镀金用的亚硫酸金钠溶液的制备方法 |
JP6773079B2 (ja) * | 2018-06-11 | 2020-10-21 | 日進化成株式会社 | ノンシアン系電解金めっき液 |
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JPH09287077A (ja) * | 1996-04-19 | 1997-11-04 | Hitachi Chem Co Ltd | 無電解金めっき液 |
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JPH1121672A (ja) * | 1997-07-04 | 1999-01-26 | Hitachi Ltd | 無電解金めっき液及び金めっき方法 |
JP3677617B2 (ja) * | 1999-06-08 | 2005-08-03 | 小島化学薬品株式会社 | 無電解金めっき液 |
JP2003013278A (ja) * | 2001-06-26 | 2003-01-15 | Japan Pure Chemical Co Ltd | 金めっき液 |
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