JP5877928B2 - 半光沢ニッケルまたはニッケル合金を堆積するためのニッケルまたはニッケル合金の直流電気めっき浴、電気めっきのための方法、およびそのための浴および化合物の使用 - Google Patents
半光沢ニッケルまたはニッケル合金を堆積するためのニッケルまたはニッケル合金の直流電気めっき浴、電気めっきのための方法、およびそのための浴および化合物の使用 Download PDFInfo
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- JP5877928B2 JP5877928B2 JP2015220989A JP2015220989A JP5877928B2 JP 5877928 B2 JP5877928 B2 JP 5877928B2 JP 2015220989 A JP2015220989 A JP 2015220989A JP 2015220989 A JP2015220989 A JP 2015220989A JP 5877928 B2 JP5877928 B2 JP 5877928B2
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- Prior art keywords
- nickel
- bath
- semi
- bright
- nickel alloy
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- 150000001875 compounds Chemical class 0.000 title claims description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title description 196
- 229910052759 nickel Inorganic materials 0.000 title description 97
- 229910000990 Ni alloy Inorganic materials 0.000 title description 52
- 238000009713 electroplating Methods 0.000 title description 37
- 238000000151 deposition Methods 0.000 title description 17
- 238000000034 method Methods 0.000 title description 14
- 238000000576 coating method Methods 0.000 description 46
- 239000011248 coating agent Substances 0.000 description 33
- 239000000654 additive Substances 0.000 description 25
- 229930195733 hydrocarbon Natural products 0.000 description 23
- 238000002474 experimental method Methods 0.000 description 22
- 239000004215 Carbon black (E152) Substances 0.000 description 21
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N coumarin Chemical compound C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 18
- 239000000758 substrate Substances 0.000 description 17
- 230000000996 additive effect Effects 0.000 description 14
- 238000007747 plating Methods 0.000 description 13
- 235000001671 coumarin Nutrition 0.000 description 11
- 125000004122 cyclic group Chemical group 0.000 description 11
- 150000002430 hydrocarbons Chemical class 0.000 description 11
- 229960000956 coumarin Drugs 0.000 description 9
- 125000003118 aryl group Chemical group 0.000 description 8
- 150000002815 nickel Chemical class 0.000 description 8
- -1 polypropylene Polymers 0.000 description 7
- RJPRZHQPROLZRW-UHFFFAOYSA-N 2-hydroxy-3-pyridin-1-ium-1-ylpropane-1-sulfonate Chemical compound [O-]S(=O)(=O)CC(O)C[N+]1=CC=CC=C1 RJPRZHQPROLZRW-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 125000006615 aromatic heterocyclic group Chemical group 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000011541 reaction mixture Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 125000001424 substituent group Chemical group 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 150000001721 carbon Chemical group 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 241000080590 Niso Species 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007857 degradation product Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 239000000080 wetting agent Substances 0.000 description 3
- 229910001369 Brass Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-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
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 2
- 239000010953 base metal 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
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000010951 brass Substances 0.000 description 2
- RNFNDJAIBTYOQL-UHFFFAOYSA-N chloral hydrate Chemical compound OC(O)C(Cl)(Cl)Cl RNFNDJAIBTYOQL-UHFFFAOYSA-N 0.000 description 2
- 229960002327 chloral hydrate Drugs 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 150000004775 coumarins Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 2
- 229960004889 salicylic acid Drugs 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 125000004434 sulfur atom Chemical group 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- ORTVZLZNOYNASJ-UPHRSURJSA-N (z)-but-2-ene-1,4-diol Chemical compound OC\C=C/CO ORTVZLZNOYNASJ-UPHRSURJSA-N 0.000 description 1
- SOSQXPIKTBUEKF-UHFFFAOYSA-N 1,4-dihexoxy-1,4-dioxobutane-2-sulfonic acid Chemical compound CCCCCCOC(=O)CC(S(O)(=O)=O)C(=O)OCCCCCC SOSQXPIKTBUEKF-UHFFFAOYSA-N 0.000 description 1
- CBCQTCPKFYFJEU-UHFFFAOYSA-N 1,4-dioxo-1,4-dipentoxybutane-2-sulfonic acid Chemical compound CCCCCOC(=O)CC(S(O)(=O)=O)C(=O)OCCCCC CBCQTCPKFYFJEU-UHFFFAOYSA-N 0.000 description 1
- MHGOKSLTIUHUBF-UHFFFAOYSA-N 2-ethylhexyl sulfate Chemical compound CCCCC(CC)COS(O)(=O)=O MHGOKSLTIUHUBF-UHFFFAOYSA-N 0.000 description 1
- GOLORTLGFDVFDW-UHFFFAOYSA-N 3-(1h-benzimidazol-2-yl)-7-(diethylamino)chromen-2-one Chemical compound C1=CC=C2NC(C3=CC4=CC=C(C=C4OC3=O)N(CC)CC)=NC2=C1 GOLORTLGFDVFDW-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WRUAHXANJKHFIL-UHFFFAOYSA-N benzene-1,3-disulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC(S(O)(=O)=O)=C1 WRUAHXANJKHFIL-UHFFFAOYSA-N 0.000 description 1
- RWDJJOUSDATHMI-UHFFFAOYSA-N benzenesulfinic acid;sodium Chemical compound [Na].OS(=O)C1=CC=CC=C1 RWDJJOUSDATHMI-UHFFFAOYSA-N 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- RZMWTGFSAMRLQH-UHFFFAOYSA-L disodium;2,2-dihexyl-3-sulfobutanedioate Chemical compound [Na+].[Na+].CCCCCCC(C([O-])=O)(C(C([O-])=O)S(O)(=O)=O)CCCCCC RZMWTGFSAMRLQH-UHFFFAOYSA-L 0.000 description 1
- UYMKPFRHYYNDTL-UHFFFAOYSA-N ethenamine Chemical compound NC=C UYMKPFRHYYNDTL-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- ZBGWAJQUDSCDPB-UHFFFAOYSA-N n-(benzenesulfonyl)benzamide Chemical compound C=1C=CC=CC=1C(=O)NS(=O)(=O)C1=CC=CC=C1 ZBGWAJQUDSCDPB-UHFFFAOYSA-N 0.000 description 1
- OVQABVAKPIYHIG-UHFFFAOYSA-N n-(benzenesulfonyl)benzenesulfonamide Chemical compound C=1C=CC=CC=1S(=O)(=O)NS(=O)(=O)C1=CC=CC=C1 OVQABVAKPIYHIG-UHFFFAOYSA-N 0.000 description 1
- SGCKSDJIMSBTFY-UHFFFAOYSA-N n-sulfonylformamide Chemical class O=CN=S(=O)=O SGCKSDJIMSBTFY-UHFFFAOYSA-N 0.000 description 1
- ZPBSAMLXSQCSOX-UHFFFAOYSA-N naphthalene-1,3,6-trisulfonic acid Chemical compound OS(=O)(=O)C1=CC(S(O)(=O)=O)=CC2=CC(S(=O)(=O)O)=CC=C21 ZPBSAMLXSQCSOX-UHFFFAOYSA-N 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- NCYVXEGFNDZQCU-UHFFFAOYSA-N nikethamide Chemical compound CCN(CC)C(=O)C1=CC=CN=C1 NCYVXEGFNDZQCU-UHFFFAOYSA-N 0.000 description 1
- 229960003226 nikethamide Drugs 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- TVDSBUOJIPERQY-UHFFFAOYSA-N prop-2-yn-1-ol Chemical compound OCC#C TVDSBUOJIPERQY-UHFFFAOYSA-N 0.000 description 1
- UVTAMWNTYFEONL-UHFFFAOYSA-N pyridin-3-yl(pyrrolidin-1-yl)methanone Chemical compound C=1C=CN=CC=1C(=O)N1CCCC1 UVTAMWNTYFEONL-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 description 1
- 229940081974 saccharin Drugs 0.000 description 1
- 235000019204 saccharin Nutrition 0.000 description 1
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- DIKJULDDNQFCJG-UHFFFAOYSA-M sodium;prop-2-ene-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC=C DIKJULDDNQFCJG-UHFFFAOYSA-M 0.000 description 1
- LDHXNOAOCJXPAH-UHFFFAOYSA-M sodium;prop-2-yne-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC#C LDHXNOAOCJXPAH-UHFFFAOYSA-M 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- LMYRWZFENFIFIT-UHFFFAOYSA-N toluene-4-sulfonamide Chemical compound CC1=CC=C(S(N)(=O)=O)C=C1 LMYRWZFENFIFIT-UHFFFAOYSA-N 0.000 description 1
- NJPKYOIXTSGVAN-UHFFFAOYSA-K trisodium;naphthalene-1,3,6-trisulfonate Chemical compound [Na+].[Na+].[Na+].[O-]S(=O)(=O)C1=CC(S([O-])(=O)=O)=CC2=CC(S(=O)(=O)[O-])=CC=C21 NJPKYOIXTSGVAN-UHFFFAOYSA-K 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 230000003442 weekly effect Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/81—Amides; Imides
- C07D213/82—Amides; Imides in position 3
-
- 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
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/72—Nitrogen atoms
- C07D213/74—Amino or imino radicals substituted by hydrocarbon or substituted hydrocarbon radicals
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/16—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms acylated on ring nitrogen atoms
- C07D295/18—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms acylated on ring nitrogen atoms by radicals derived from carboxylic acids, or sulfur or nitrogen analogues thereof
- C07D295/182—Radicals derived from carboxylic acids
- C07D295/192—Radicals derived from carboxylic acids from aromatic carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
- C07D401/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
- C07D401/06—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings linked by a carbon chain containing only aliphatic carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D413/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and oxygen atoms as the only ring hetero atoms
- C07D413/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and oxygen atoms as the only ring hetero atoms containing two hetero rings
- C07D413/06—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and oxygen atoms as the only ring hetero atoms containing two hetero rings linked by a carbon chain containing only aliphatic carbon atoms
-
- 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
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
- C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
- C25D3/18—Heterocyclic compounds
-
- 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
-
- 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
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- Electroplating And Plating Baths Therefor (AREA)
- Pyridine Compounds (AREA)
Description
従って、先行技術を鑑み、本発明の課題は、公知の先行技術のニッケル電気めっき浴の上述の欠点を示さない、半光沢ニッケルまたはニッケル合金のコーティングを基材上に堆積するための修正されたニッケルまたはニッケル合金の直流電気めっき浴を提供することであった。
これらの課題、および明示的に述べられていないが本願において前置きとして議論される文脈から直ちに導出可能もしくは認識可能であるさらなる課題は、請求項1の全ての特徴を有する直流浴によって解決される。本発明の直流浴の適切な変更物は、独立請求項2〜12において保護される。さらに、請求項13は、前記の半光沢ニッケルまたはニッケル合金のコーティングを導電性加工物上に堆積するための方法を含む一方で、請求項14は、前記の方法を実施することによって光沢ニッケルまたはニッケル合金のコーティングを堆積するための、前記の半光沢ニッケルまたはニッケル合金の直流電気めっき浴の使用を含む。請求項15は、式(II)、(III)および(IV)を有する化合物についての絶対的な化学化合物の保護を含む。
R1はSO3 -基で置換されたC1〜C18炭化水素成分、カルボキシル基で置換されたC1〜C18炭化水素成分、少なくとも1つの芳香族および/または複素環式芳香族基で置換されたC1〜C18炭化水素成分であり、
R2はNR3R4成分、OR5成分、または環式NR6成分であり、その際
R3、R4、R5は、水素またはC1〜C18炭化水素成分、または少なくとも1つの芳香族および/または複素環式芳香族基で置換されたC1〜C18炭化水素成分であり、その際、R3、R4およびR5は同一または異なり、
R6はC3〜C8炭化水素成分、または少なくとも1つの炭素原子がヘテロ原子によって置換されているC3〜C8炭化水素成分であり、且つ、
nは1〜3である]
を有する少なくとも1つの化合物を含むことを特徴とする前記電気めっき浴を提供する。
本発明の課題、特徴および利点はまた、以下の説明を以下の表と関連付けて読むことによって明らかになる:
表1は、本発明の実施態様による半光沢ニッケルのコーティングについての実験を示す。
本願において使用される場合、「ニッケルまたはニッケル合金の直流電気めっき浴」との用語は、本発明による半光沢ニッケルまたはニッケル合金のコーティングの堆積について適用される場合、ニッケルの直流浴に関し、それはいわゆる「ワット電解浴」に基づき、一般に以下の組成を有する:
240〜550g/lの硫酸ニッケル(NiSO4・7H2OまたはNiSO4・6H2O)、
30〜150g/lの塩化ニッケル(NiCl2・6H2O)、および
30〜55g/lのホウ酸(H3BO3)。
R1が、SO3 -基で置換されたC1〜C8、好ましくはC1〜C4炭化水素成分、カルボキシル基で置換されたC1〜C8、好ましくはC1〜C4炭化水素成分、または少なくとも1つの芳香族および/または複素環式芳香族基で置換されたC1〜C8、好ましくはC1〜C4炭化水素成分であり、
R2が、NR3R4成分、OR5成分、または環式NR6成分であり、その際、
R3、R4、R5が、水素またはC1〜C18炭化水素成分、または少なくとも1つの芳香族および/または複素環式芳香族基で置換されたC1〜C18炭化水素成分であり、その際、R3、R4およびR5は同一または異なり、
R6が、C4〜C8炭化水素成分、または少なくとも1つの炭素原子がヘテロ原子によって置換されているC3〜C8炭化水素成分であり、且つ、
nが1または2である、
一般式(I)を有する少なくとも1つの化合物を含む。
R1が、SO3 -基で置換されたC1〜C8、好ましくはC1〜C4炭化水素成分、カルボキシル基で置換されたC1〜C8、好ましくはC1〜C4炭化水素成分、または少なくとも1つの芳香族および/または複素環式芳香族基で置換されたC1〜C8、好ましくはC1〜C4炭化水素成分であり、
R2が、NR3R4成分、OR5成分、または環式NR6成分であり、その際、
R3、R4、R5が、水素またはC1〜C8、好ましくはC1〜C4炭化水素成分、または少なくとも1つの芳香族および/または複素環式芳香族基で置換されたC1〜C8、好ましくはC1〜C4炭化水素成分であり、その際、R3、R4およびR5は同一または異なり、
R6が、C4またはC5炭化水素成分、または少なくとも1つの炭素原子が硫黄原子または酸素原子によって置換されているC4〜C5炭化水素成分であり、且つ、
nが1である、
一般式(I)を有する少なくとも1つの化合物を含む。
R1がn−エチル−SO3 -、n−プロピル−SO3 -、n−ブチル−SO3 -、ベンジル、CH2−COOHまたはそれらの塩、好ましくはナトリウム塩CH2−COONa成分であり、
R2がNH2、N(エチル)2、O(エチル)、OH成分、または環式NR6成分であり、その際、
R6がC4またはC5炭化水素成分、または少なくとも1つの炭素原子が硫黄原子または酸素原子によって置換されているC4〜C5炭化水素成分であり、且つ、
nが1である、
一般式(I)を有する少なくとも1つの化合物を含む。
i) 加工物を、本発明による半光沢ニッケルまたはニッケル合金の電気めっき浴と接触させる段階、
ii) 少なくとも1つのアノードを、半光沢ニッケルまたはニッケル合金の電気めっき浴と接触させる段階、
iii) 前記加工物と少なくとも1つのアノードとにわたって電圧を印加する段階、および
iv) 半光沢ニッケルまたはニッケル合金のコーティングを加工物上に電着させる段階
を含む前記方法によっても解決される。
3−(3−(ジエチルカルバモイル)ピリジニウム−1−イル)プロパン−1−スルホネート(II)
10g(0.0555mol)のニコチン酸ジエチルアミド(99%)を50mlのエタノール中で溶解する。引き続き、6.78g(0.0555mol)の1,3−プロパンスルトンを添加する。その後、反応混合物を還流下で48時間の間、78℃で加熱する。
10g(0.056747mol)の3−(ピロリジン−1−カルボニル)ピリジンを50mlのエタノール中で溶解する。引き続き、6.93g(0.056747mol)の1,3−プロパンスルトンを添加する。その後、反応混合物を還流下で48時間の間、78℃で加熱する。
10g(0.05206mol)の3−(モルホリン−1−カルボニル)ピリジンを50mlのエタノール中で溶解する。引き続き、6.36g(0.05206mol)の1,3−プロパンスルトンを添加する。その後、反応混合物を還流下で48時間の間、78℃で加熱する。
280g/lの硫酸ニッケル(NiSO4・7H2O)、
35g/lの塩化ニッケル(NiCl2・6H2O)、
35g/lのホウ酸(H3BO3)、および
50mg/lのジヘキシルスルホコハク酸ナトリウム。
i) 熱い浸漬洗浄剤によって脱脂し、
ii) 電解脱脂し、
iii) 濯ぎ、
iv) 10体積%の硫酸を用いて酸浸漬する。
+++ 非常に良い
++ 良い
+ 普通
− 悪い。
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EP13167074.7A EP2801640A1 (en) | 2013-05-08 | 2013-05-08 | Galvanic nickel or nickel alloy electroplating bath for depositing a semi-bright nickel or nickel alloy |
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DE102014207778B3 (de) | 2014-04-25 | 2015-05-21 | Kiesow Dr. Brinkmann GmbH & Co. KG | Verwendung einer Mischung zur Verwendung in einem galvanischen Bad oder eines galvanischen Bades zur Herstellung einer Glanznickelschicht sowie Verfahren zur Herstellung eines Artikels mit einer Glanznickelschicht |
CN105112949A (zh) * | 2015-07-31 | 2015-12-02 | 广东欧珀移动通信有限公司 | 一种改善铝合金镀件光泽度的方法及铝合金镀件、电子装置 |
TWI707061B (zh) * | 2015-11-27 | 2020-10-11 | 德商德國艾托特克公司 | 鈀之電鍍浴組合物及無電電鍍方法 |
WO2017199835A1 (ja) * | 2016-05-18 | 2017-11-23 | 日本高純度化学株式会社 | 電解ニッケル(合金)めっき液 |
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JP2020524746A (ja) * | 2017-06-23 | 2020-08-20 | アトテック ドイチェランド ゲーエムベーハー | 基材上に装飾ニッケルコーティングを堆積させるためのニッケル電気メッキ浴 |
EP3456870A1 (en) * | 2017-09-13 | 2019-03-20 | ATOTECH Deutschland GmbH | A bath and method for filling a vertical interconnect access or trench of a work piece with nickel or a nickel alloy |
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