JP6449335B2 - 水性無電解ニッケルめっき浴、及びその使用方法 - Google Patents
水性無電解ニッケルめっき浴、及びその使用方法 Download PDFInfo
- Publication number
- JP6449335B2 JP6449335B2 JP2016570823A JP2016570823A JP6449335B2 JP 6449335 B2 JP6449335 B2 JP 6449335B2 JP 2016570823 A JP2016570823 A JP 2016570823A JP 2016570823 A JP2016570823 A JP 2016570823A JP 6449335 B2 JP6449335 B2 JP 6449335B2
- Authority
- JP
- Japan
- Prior art keywords
- electroless nickel
- acid
- plating solution
- nickel plating
- substrate
- 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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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims description 246
- 229910052759 nickel Inorganic materials 0.000 title claims description 116
- 238000007747 plating Methods 0.000 title claims description 99
- 238000000034 method Methods 0.000 title claims description 37
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 54
- 239000011574 phosphorus Substances 0.000 claims description 54
- 229910052698 phosphorus Inorganic materials 0.000 claims description 53
- 239000000758 substrate Substances 0.000 claims description 29
- 238000012360 testing method Methods 0.000 claims description 28
- 239000002244 precipitate Substances 0.000 claims description 26
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 24
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims description 19
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 19
- 229910001453 nickel ion Inorganic materials 0.000 claims description 17
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 17
- 239000003381 stabilizer Substances 0.000 claims description 17
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 claims description 16
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 16
- 239000003638 chemical reducing agent Substances 0.000 claims description 14
- 150000003464 sulfur compounds Chemical class 0.000 claims description 12
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 150000007513 acids Chemical class 0.000 claims description 10
- 229910052797 bismuth Inorganic materials 0.000 claims description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 150000001991 dicarboxylic acids Chemical class 0.000 claims description 9
- 150000002497 iodine compounds Chemical group 0.000 claims description 9
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000001384 succinic acid Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 claims description 6
- 229960003080 taurine Drugs 0.000 claims description 6
- 230000007306 turnover Effects 0.000 claims description 6
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 5
- 229940081974 saccharin Drugs 0.000 claims description 5
- 235000019204 saccharin Nutrition 0.000 claims description 5
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 claims description 5
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004310 lactic acid Substances 0.000 claims description 4
- 235000014655 lactic acid Nutrition 0.000 claims description 4
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 4
- 239000001230 potassium iodate Substances 0.000 claims description 4
- 235000006666 potassium iodate Nutrition 0.000 claims description 4
- 229940093930 potassium iodate Drugs 0.000 claims description 4
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-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
- 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
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 3
- ZRDJERPXCFOFCP-UHFFFAOYSA-N azane;iodic acid Chemical compound [NH4+].[O-]I(=O)=O ZRDJERPXCFOFCP-UHFFFAOYSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- NALMPLUMOWIVJC-UHFFFAOYSA-N n,n,4-trimethylbenzeneamine oxide Chemical compound CC1=CC=C([N+](C)(C)[O-])C=C1 NALMPLUMOWIVJC-UHFFFAOYSA-N 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000011697 sodium iodate Substances 0.000 claims description 3
- 235000015281 sodium iodate Nutrition 0.000 claims description 3
- 229940032753 sodium iodate Drugs 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims 2
- 235000015165 citric acid Nutrition 0.000 claims 2
- 239000001630 malic acid Substances 0.000 claims 2
- 235000011090 malic acid Nutrition 0.000 claims 2
- 238000002845 discoloration Methods 0.000 claims 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical group [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 15
- 230000035882 stress Effects 0.000 description 10
- 229910001096 P alloy Inorganic materials 0.000 description 9
- -1 but not limited to Substances 0.000 description 9
- 229910052793 cadmium Inorganic materials 0.000 description 7
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 238000000151 deposition Methods 0.000 description 7
- 230000008021 deposition Effects 0.000 description 6
- 229910000990 Ni alloy Inorganic materials 0.000 description 5
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000013522 chelant Substances 0.000 description 4
- 239000002738 chelating agent Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- GQZXNSPRSGFJLY-UHFFFAOYSA-N hydroxyphosphanone Chemical compound OP=O GQZXNSPRSGFJLY-UHFFFAOYSA-N 0.000 description 4
- 229940005631 hypophosphite ion Drugs 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000008139 complexing agent Substances 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 239000000383 hazardous chemical Substances 0.000 description 2
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical compound [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M thiocyanate group Chemical group [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- PAPULADQENAUOG-UHFFFAOYSA-N 2h-benzotriazole;1,3-thiazolidine-2-thione Chemical compound S=C1NCCS1.C1=CC=CC2=NNN=C21 PAPULADQENAUOG-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910000521 B alloy Inorganic materials 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- FLVIGYVXZHLUHP-UHFFFAOYSA-N N,N'-diethylthiourea Chemical compound CCNC(=S)NCC FLVIGYVXZHLUHP-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- IOEJYZSZYUROLN-UHFFFAOYSA-M Sodium diethyldithiocarbamate Chemical compound [Na+].CCN(CC)C([S-])=S IOEJYZSZYUROLN-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910001439 antimony ion Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 229910001451 bismuth ion Inorganic materials 0.000 description 1
- QDWJUBJKEHXSMT-UHFFFAOYSA-N boranylidynenickel Chemical compound [Ni]#B QDWJUBJKEHXSMT-UHFFFAOYSA-N 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- 229960002433 cysteine Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- ZBKFYXZXZJPWNQ-UHFFFAOYSA-N isothiocyanate group Chemical group [N-]=C=S ZBKFYXZXZJPWNQ-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical compound C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 1
- NRZRRZAVMCAKEP-UHFFFAOYSA-N naphthionic acid Chemical compound C1=CC=C2C(N)=CC=C(S(O)(=O)=O)C2=C1 NRZRRZAVMCAKEP-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229940053662 nickel sulfate Drugs 0.000 description 1
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 description 1
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 239000012811 non-conductive material Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 229910001380 potassium hypophosphite Inorganic materials 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- IAAKNVCARVEIFS-UHFFFAOYSA-M sodium;4-hydroxynaphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(O)=CC=C(S([O-])(=O)=O)C2=C1 IAAKNVCARVEIFS-UHFFFAOYSA-M 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229950000244 sulfanilic acid Drugs 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- UIERGBJEBXXIGO-UHFFFAOYSA-N thiamine mononitrate Chemical compound [O-][N+]([O-])=O.CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N UIERGBJEBXXIGO-UHFFFAOYSA-N 0.000 description 1
- 125000001391 thioamide group Chemical group 0.000 description 1
- 125000005300 thiocarboxy group Chemical group C(=S)(O)* 0.000 description 1
- UVZICZIVKIMRNE-UHFFFAOYSA-N thiodiacetic acid Chemical compound OC(=O)CSCC(O)=O UVZICZIVKIMRNE-UHFFFAOYSA-N 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 125000005323 thioketone group Chemical group 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
Description
a)ニッケルイオン源と;
b)還元剤と;
c)1種以上の錯化剤と;を含む。
a)ニッケルイオン源と;
b)次亜リン酸塩を含む還元剤と;
c)以下、
i)1種以上のジカルボン酸;及び
ii)1種以上のα−ヒドロキシカルボン酸;を含むキレート系と;
を含み、無電解ニッケルめっき液の寿命に亘り、約12%のリン含有量を維持するニッケル析出物を生成することを特徴とする無電解ニッケルめっき液に関する。
a)ニッケルイオン源と;
b)次亜リン酸塩を含む還元剤と;
c)以下、
i)1種以上のジカルボン酸;及び
ii)1種以上のα−ヒドロキシカルボン酸;を含むキレート系と;
を含む無電解ニッケルリンめっき液と、前記基材上に約12%のリン含有量を有するニッケルリン析出物を提供するための期間接触させる工程を含み;
前記無電解ニッケルめっき液が、前記無電解ニッケルめっき液の寿命に亘り、約12%のリン含有量を維持するニッケル析出物を生成することを特徴とする方法に関する。
a)ニッケルイオン源と;
b)次亜リン酸塩を含む還元剤と;
c)以下、
i)1種以上のジカルボン酸;及び
ii)1種以上のα−ヒドロキシカルボン酸;を含むキレート系と;
を含み、無電解ニッケルめっき液の寿命に亘り、約12%のリン含有量を維持するニッケル析出物を生成することを特徴とする無電解ニッケルめっき液に関する。
a)約30g/L〜約40g/L、より好ましくは約33g/L〜約36g/Lの次亜リン酸塩と;
b)約30g/L〜約40g/L、より好ましくは約33g/L〜約36g/Lの乳酸と;
c)約3g/L〜約6g/L、より好ましくは約4g/L〜約5g/Lのコハク酸と;
d)約25g/L〜約35g/L、より好ましくは約28g/L〜約31g/Lのマロン酸と;を含む。
a)ニッケルイオン源と;
b)次亜リン酸塩を含む還元剤と;
c)以下、
i)1種以上のジカルボン酸;及び
ii)1種以上のα−ヒドロキシカルボン酸;を含むキレート系と;
を含む無電解ニッケルリンめっき液と、前記基材上に約12%のリン含有量を有するニッケルリン析出物を提供するための期間接触させる工程を含み;
前記無電解ニッケルめっき液が、前記無電解ニッケルめっき液の寿命に亘り、約12%のリン含有量を維持するニッケル析出物を生成することを特徴とする方法に関する。
以下を含むキレート系を調製した。
34g/L 乳酸
4.1g/L コハク酸
30g/L マロン酸
6.5g/L 硫酸ニッケル
20g/L 次亜リン酸ナトリウム
Claims (34)
- a)ニッケルイオン源と;
b)次亜リン酸塩を含む還元剤と;
c)以下、
i)1種以上のジカルボン酸;及び
ii)1種以上のα−ヒドロキシカルボン酸;を含むキレート系と;
d)ビスマス及びタウリンを含む光沢剤と;
を含み、無電解ニッケルめっき液の寿命に亘り、約12%のリン含有量を維持するニッケル析出物を生成することを特徴とする無電解ニッケルめっき液。 - a)ニッケルイオン源と;
b)30g/L〜40g/Lの次亜リン酸塩を含む還元剤と;
c1)30g/L〜40g/Lの乳酸と;
c2)3g/L〜6g/Lのコハク酸と;
c3)25g/L〜35g/Lのマロン酸と;
d)ビスマスを含む光沢剤と;
を含み、無電解ニッケルめっき液の寿命に亘り、約12%のリン含有量を維持するニッケル析出物を生成することを特徴とする無電解ニッケルめっき液。 - 前記1種以上のジカルボン酸が、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、及びピメリン酸からなる群から選択され、前記1種以上のα−ヒドロキシカルボン酸が、グリコール酸、乳酸、リンゴ酸、クエン酸、及び酒石酸からなる群から選択される請求項1に記載の無電解ニッケルめっき液。
- b)30g/L〜40g/Lの次亜リン酸塩と;
c1)30g/L〜40g/Lの乳酸と;
c2)3g/L〜6g/Lのコハク酸と;
c3)25g/L〜35g/Lのマロン酸と;
を含む請求項2又は3のいずれかに記載の無電解ニッケルめっき液。 - b)33g/L〜36g/Lの次亜リン酸塩と;
c1)33g/L〜36g/Lの乳酸と;
c2)4g/L〜5g/Lのコハク酸と;
c3)28g/L〜31g/Lのマロン酸と;
を含む請求項4に記載の無電解ニッケルめっき液。 - pHが5.2〜6.2である請求項1又は2に記載の無電解ニッケルめっき液。
- pHが5.6〜5.7である請求項6に記載の無電解ニッケルめっき液。
- 安定化剤を含み、前記安定化剤が、ヨウ素酸カリウム、ヨウ素酸ナトリウム、ヨウ素酸アンモニウム、及びこれらの1以上の組合せからなる群から選択されるヨウ素化合物である請求項1又は2に記載の無電解ニッケルめっき液。
- 前記安定化剤が鉛又はアンチモンを含んでいない請求項8に記載の無電解ニッケルめっき液。
- 硫黄化合物を更に含む請求項8に記載の無電解ニッケルめっき液。
- 前記硫黄化合物がサッカリンである請求項10に記載の無電解ニッケルめっき液。
- 前記光沢剤が、2mg/L〜4mg/Lのビスマス、及び0.5mg/L〜3.0mg/Lのタウリンを含む請求項1に記載の無電解ニッケルめっき液。
- 約12%のリン含有量を有する無電解ニッケルリン析出物を基材上に製造する方法であって、前記基材を、
a)ニッケルイオン源と;
b)次亜リン酸塩を含む還元剤と;
c)以下、
i)1種以上のジカルボン酸;及び
ii)1種以上のα−ヒドロキシカルボン酸;を含むキレート系と;
d)ビスマス及びタウリンを含む光沢剤と;
を含む無電解ニッケルリンめっき液と、前記基材上に約12%のリン含有量を有するニッケルリン析出物を提供するための期間接触させる工程を含み;
前記無電解ニッケルめっき液が、前記無電解ニッケルめっき液の寿命に亘り、約12%のリン含有量を維持するニッケル析出物を生成することを特徴とする方法。 - 約12%のリン含有量を有する無電解ニッケルリン析出物を基材上に製造する方法であって、前記基材を、
a)ニッケルイオン源と;
b)30g/L〜40g/Lの次亜リン酸塩を含む還元剤と;
c1)30g/L〜40g/Lの乳酸と;
c2)3g/L〜6g/Lのコハク酸と;
c3)25g/L〜35g/Lのマロン酸と;
d)ビスマスを含む光沢剤と;
を含む無電解ニッケルリンめっき液と、前記基材上に約12%のリン含有量を有するニッケルリン析出物を提供するための期間接触させる工程を含み;
前記無電解ニッケルめっき液が、前記無電解ニッケルめっき液の寿命に亘り、約12%のリン含有量を維持するニッケル析出物を生成することを特徴とする方法。 - 前記無電解ニッケルめっき液の寿命が少なくとも3メタルターンオーバーを含む請求項13又は14に記載の方法。
- 前記無電解ニッケルめっき液の寿命が少なくとも5メタルターンオーバーを含む請求項15に記載の方法。
- 前記1種以上のジカルボン酸が、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、及びピメリン酸からなる群から選択され、前記1種以上のα−ヒドロキシカルボン酸が、グリコール酸、乳酸、リンゴ酸、クエン酸、及び酒石酸からなる群から選択される請求項13に記載の方法。
- 前記めっき液が、
b)30g/L〜40g/Lの次亜リン酸塩と;
c1)30g/L〜40g/Lの乳酸と;
c2)3g/L〜6g/Lのコハク酸と;
c3)25g/L〜35g/Lのマロン酸と;
を含む請求項14又は17のいずれかに記載の方法。 - 前記めっき液が、
b)33g/L〜36g/Lの次亜リン酸塩と;
c1)33g/L〜36g/Lの乳酸と;
c2)4g/L〜5g/Lのコハク酸と;
c3)28g/L〜31g/Lのマロン酸と;
を含む請求項18に記載の方法。 - 前記無電解ニッケルめっき液のpHが5.2〜6.2である請求項13又は14に記載の方法。
- 前記無電解ニッケルめっき液のpHが5.6〜5.7である請求項20に記載の方法。
- 前記無電解ニッケルめっき液が安定化剤を含み、前記安定化剤が、ヨウ素酸カリウム、ヨウ素酸ナトリウム、ヨウ素酸アンモニウム、及びこれらの1以上の組合せからなる群から選択されるヨウ素化合物である請求項13又は14に記載の方法。
- 前記安定化剤が鉛又はアンチモンを含んでいない請求項22に記載の方法。
- 硫黄化合物を更に含む請求項22に記載の方法。
- 前記硫黄化合物がサッカリンである請求項24に記載の方法。
- 前記光沢剤が、2mg/L〜4mg/Lのビスマス、及び0.5mg/L〜3.0mg/Lのタウリンを含む請求項13に記載の方法。
- 前記基材上の前記無電解ニッケル液のめっき速度が、少なくとも0.5ミル/時間である請求項13又は14に記載の方法。
- 前記基材上の前記無電解ニッケル液のめっき速度が、少なくとも0.9ミル/時間である請求項27に記載の方法。
- 前記無電解ニッケル析出物が、標準的な硝酸試験を合格でき、前記標準的な硝酸試験が、無電解ニッケルコーティング基材を濃硝酸溶液に30秒間浸漬する工程を含み、前記無電解ニッケルコーティング基材が、前記基材の変色が観察されない場合に前記硝酸試験を合格となる請求項13又は14に記載の方法。
- 前記無電解ニッケルめっき液を、補充液で補充する工程を更に含む請求項13又は14に記載の方法。
- 前記補充液がチオ尿素を含む請求項30に記載の方法。
- 前記補充液が、0.2mg/L/MTO〜2.0mg/L/MTOのチオ尿素を含む請求項31に記載の方法。
- 前記無電解ニッケル析出物の引張応力が、15,000PSI未満である請求項30に記載の方法。
- 前記無電解ニッケル析出物の引張応力が、2500PSI未満である請求項33に記載の方法。
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US14/293,216 US11685999B2 (en) | 2014-06-02 | 2014-06-02 | Aqueous electroless nickel plating bath and method of using the same |
PCT/US2015/032375 WO2015187402A1 (en) | 2014-06-02 | 2015-05-26 | Aqueous electroless nickel plating bath and method of using the same |
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KR (2) | KR102234060B1 (ja) |
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ES2929860T3 (es) | 2022-12-02 |
KR20160148012A (ko) | 2016-12-23 |
EP3149223B1 (en) | 2022-10-26 |
US20150345027A1 (en) | 2015-12-03 |
KR102234060B1 (ko) | 2021-04-01 |
JP2017516920A (ja) | 2017-06-22 |
US11685999B2 (en) | 2023-06-27 |
WO2015187402A8 (en) | 2016-07-14 |
EP3149223A4 (en) | 2018-02-28 |
CN106661733A (zh) | 2017-05-10 |
WO2015187402A1 (en) | 2015-12-10 |
EP3149223A1 (en) | 2017-04-05 |
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