JP6718509B2 - 水性媒体中における元素の電気化学的析出 - Google Patents
水性媒体中における元素の電気化学的析出 Download PDFInfo
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- JP6718509B2 JP6718509B2 JP2018532164A JP2018532164A JP6718509B2 JP 6718509 B2 JP6718509 B2 JP 6718509B2 JP 2018532164 A JP2018532164 A JP 2018532164A JP 2018532164 A JP2018532164 A JP 2018532164A JP 6718509 B2 JP6718509 B2 JP 6718509B2
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- ligand
- substituted
- metal
- unsubstituted
- aluminum
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- 238000004070 electrodeposition Methods 0.000 title claims description 22
- 239000012736 aqueous medium Substances 0.000 title description 14
- 229910052751 metal Inorganic materials 0.000 claims description 114
- 239000003446 ligand Substances 0.000 claims description 112
- 239000002184 metal Substances 0.000 claims description 97
- 238000000034 method Methods 0.000 claims description 92
- 229910052782 aluminium Inorganic materials 0.000 claims description 78
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 71
- -1 hexafluorosilicic acid Chemical compound 0.000 claims description 64
- 239000003792 electrolyte Substances 0.000 claims description 51
- 230000009467 reduction Effects 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 150000004696 coordination complex Chemical class 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 23
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 19
- 229910052760 oxygen Inorganic materials 0.000 claims description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 16
- JHRWWRDRBPCWTF-OLQVQODUSA-N captafol Chemical compound C1C=CC[C@H]2C(=O)N(SC(Cl)(Cl)C(Cl)Cl)C(=O)[C@H]21 JHRWWRDRBPCWTF-OLQVQODUSA-N 0.000 claims description 15
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 10
- 239000003125 aqueous solvent Substances 0.000 claims description 9
- 239000012298 atmosphere Substances 0.000 claims description 9
- 150000007942 carboxylates Chemical class 0.000 claims description 9
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 4
- 150000001414 amino alcohols Chemical class 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 150000002596 lactones Chemical class 0.000 claims description 3
- 125000005498 phthalate group Chemical class 0.000 claims description 3
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- 229920005862 polyol Polymers 0.000 claims description 3
- 125000005549 heteroarylene group Chemical group 0.000 claims description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 2
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 2
- 150000003462 sulfoxides Chemical class 0.000 claims description 2
- 125000001475 halogen functional group Chemical group 0.000 claims 4
- 230000007423 decrease Effects 0.000 claims 2
- 150000002739 metals Chemical group 0.000 description 28
- 125000004432 carbon atom Chemical group C* 0.000 description 22
- 239000000243 solution Substances 0.000 description 20
- 229910052739 hydrogen Inorganic materials 0.000 description 19
- 239000001257 hydrogen Substances 0.000 description 19
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 16
- 238000007747 plating Methods 0.000 description 15
- 125000000623 heterocyclic group Chemical group 0.000 description 14
- 125000000217 alkyl group Chemical group 0.000 description 13
- 150000001768 cations Chemical class 0.000 description 13
- 239000010410 layer Substances 0.000 description 13
- 125000003118 aryl group Chemical group 0.000 description 12
- 238000000576 coating method Methods 0.000 description 12
- 241000894007 species Species 0.000 description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- 125000005843 halogen group Chemical group 0.000 description 10
- 125000005842 heteroatom Chemical group 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- 125000001424 substituent group Chemical group 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 125000003545 alkoxy group Chemical group 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000011651 chromium Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 230000002829 reductive effect Effects 0.000 description 8
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 125000002252 acyl group Chemical group 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 239000010955 niobium Substances 0.000 description 7
- 239000011135 tin Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 125000001072 heteroaryl group Chemical group 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- DTQVDTLACAAQTR-UHFFFAOYSA-M Trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-M 0.000 description 5
- 125000003710 aryl alkyl group Chemical group 0.000 description 5
- 125000004104 aryloxy group Chemical group 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002659 electrodeposit Substances 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 229910052758 niobium Inorganic materials 0.000 description 5
- 239000010948 rhodium Substances 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- 229910052718 tin Inorganic materials 0.000 description 5
- 229910052720 vanadium Inorganic materials 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000000872 buffer Substances 0.000 description 4
- 150000001721 carbon Chemical class 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 125000000753 cycloalkyl group Chemical group 0.000 description 4
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 description 4
- VILAVOFMIJHSJA-UHFFFAOYSA-N dicarbon monoxide Chemical group [C]=C=O VILAVOFMIJHSJA-UHFFFAOYSA-N 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 4
- 229910021397 glassy carbon Inorganic materials 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000002608 ionic liquid Substances 0.000 description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 125000005466 alkylenyl group Chemical group 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 125000004446 heteroarylalkyl group Chemical group 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 229910052741 iridium Inorganic materials 0.000 description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 2
- 239000005695 Ammonium acetate Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 229940118662 aluminum carbonate Drugs 0.000 description 2
- 235000019257 ammonium acetate Nutrition 0.000 description 2
- 229940043376 ammonium acetate Drugs 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 125000002102 aryl alkyloxo group Chemical group 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 150000001540 azides Chemical class 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 125000005265 dialkylamine group Chemical group 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 125000005553 heteroaryloxy group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000011133 lead Substances 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 125000001624 naphthyl group Chemical group 0.000 description 2
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 125000003367 polycyclic group Chemical group 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 description 2
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
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- 230000003139 buffering effect Effects 0.000 description 1
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical compound CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 description 1
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- 125000005587 carbonate group Chemical group 0.000 description 1
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- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
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- 150000002081 enamines Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910021482 group 13 metal Inorganic materials 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 125000005252 haloacyl group Chemical group 0.000 description 1
- 125000004404 heteroalkyl group Chemical group 0.000 description 1
- 125000004415 heterocyclylalkyl group Chemical group 0.000 description 1
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- 230000036571 hydration Effects 0.000 description 1
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- 150000002431 hydrogen Chemical group 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
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- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
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- 238000003760 magnetic stirring Methods 0.000 description 1
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- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 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 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- 125000002950 monocyclic group Chemical group 0.000 description 1
- 125000002757 morpholinyl group Chemical group 0.000 description 1
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 125000006574 non-aromatic ring group Chemical group 0.000 description 1
- 239000012457 nonaqueous media Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 125000002971 oxazolyl group Chemical group 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 125000001792 phenanthrenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C=CC12)* 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 125000004193 piperazinyl group Chemical group 0.000 description 1
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- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
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- 125000001725 pyrenyl group Chemical group 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 125000000714 pyrimidinyl group Chemical group 0.000 description 1
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- 125000000719 pyrrolidinyl group Chemical group 0.000 description 1
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- 230000000717 retained effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 125000006413 ring segment Chemical group 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 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
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 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
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000003107 substituted aryl group Chemical group 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 125000000565 sulfonamide group Chemical group 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 125000001174 sulfone group Chemical group 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 125000003375 sulfoxide group Chemical group 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 125000003718 tetrahydrofuranyl group Chemical group 0.000 description 1
- 125000003831 tetrazolyl group Chemical group 0.000 description 1
- WROMPOXWARCANT-UHFFFAOYSA-N tfa trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F.OC(=O)C(F)(F)F WROMPOXWARCANT-UHFFFAOYSA-N 0.000 description 1
- 239000012720 thermal barrier coating Substances 0.000 description 1
- 125000001544 thienyl group Chemical group 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 125000004306 triazinyl group Chemical group 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- 125000004044 trifluoroacetyl group Chemical group FC(C(=O)*)(F)F 0.000 description 1
- 125000003960 triphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C3=CC=CC=C3C12)* 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 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
- C25D3/42—Electroplating: Baths therefor from solutions of light metals
- C25D3/44—Aluminium
-
- 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
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Description
商業的に重要な周期表上の元素の多くは、水溶液から電着することは容易でない。なぜなら、その還元電位が水の電気化学窓よりもはるかに大きくなりうる(例えば、水分解に起因して水素ガスを放出させるほどの過電圧となる)からである。本明細書に記載の種々の実施形態により提供するアプローチによれば、金属類の還元電位を、水溶液からの電着用に修正可能なように「チューニング」する。一実施形態において、金属類の還元電位は、例えば、水素ガスを発生することなく金属類を水溶液から電着できるように金属類の還元電位を変更する配位子(リガンド)を選択することによりチューニングする。他の実施形態において、当該配位子の選択は、金属中心の還元電位に熱力学的な影響を及ぼすように行い、水素発生過電圧の発生よりも前に金属中心の還元が起こるようにする。
本明細書に記載の電着法を用いて電着することができる金属類は限定されない。電子求引性アプローチは、少なくとも、2族、4族、5族、7族、及び13族の金属に適用可能である。本明細書に記載の方法に有用な金属類としては、一般に、ポーリングの電気陰性度が1.9未満(例えば、約1.3〜約1.6、約1.7〜約1.9、及び約1.6〜約1.9)の金属類が挙げられる。一般に、そのような金属類は、水中において高効率でめっきすることはほぼ不可能だろうと考えられ、又は、そのような金属類では水素脆性が問題となりうる。
本明細書に記載の種々の実施形態の金属錯体は、金属中心及び当該金属中心と会合する配位子を含む。いくつかの実施形態において、金属中心と会合する配位子のうち少なくとも1個が、電子求引性配位子である。
(M1LaLb)p(M2LaLb)d
式中、M1及びM2は、それぞれ、独立して金属中心を表し、Lは電子求引性配位子であり、pは0〜5であり、dは0〜5であり、aは1〜8(例えば、1〜4、0.5〜1.5、2〜8、2〜6、及び4〜6)であり、bは1〜8(例えば、1〜4、0.5〜1.5、2〜8、2〜6、及び4〜6)である。本明細書において検討する金属錯体は、したがって、金属種を1つ以上含む金属錯体であり、さらに、p及びdがそれぞれ5である場合には、異なる金属種を10まで含むこともできる。加えて、金属錯体は、それぞれ、金属中心の周囲に同一又は異なる配位子を有することができる。したがって、例えば、異なる2つの金属錯体(例えばpが1、dが1である場合)を有することができ、第1の金属錯体はCr(SO3R1)a、第2の金属錯体はMo(SO3R1)aとなる。金属錯体をこのように組み合わせて使用することにより、CrMo合金を基板表面上に電着することができる。
が挙げられ、
式中、波線は、例えば、−C(O)O−部分への結合点を表す。
本明細書に記載の方法の種々の実施形態は、実質的水性媒体中に溶解した金属錯体の電気化学的還元を介して、少なくとも1種の金属を電着することを含む。
本明細書に記載の各実施形態は、少なくとも1種の金属を導電性基板の表面上に電着する方法に関するものである。
いくつかの実施形態において、本明細書に記載の各方法を用いて、少なくとも1種(例えば、少なくとも2種)の金属の少なくとも1つの層(例えば少なくとも2層)を基板表面に電着することができる。いくつかの実施形態において、各層は、1種以上の異なる金属を含む。他の実施形態において、少なくとも2層が電着されている場合、第1の層は、第2の層とは異なる少なくとも1種の金属を含む。
炭酸アルミニウム(Al2(CO3)3、アルファ・エイサー社製);塩化アルミニウム(AlCl3、無水、≧98.0%,TCI);ビス(トリフルオロメタン)スルホンアミド(Tf2NH、≧95.0%、シグマ−アルドリッチ製);メタンスルホン酸(MsOH、99%、アクロスオーガニック製);p−トルエンスルホン酸(TsOH、水和物monohydrate、98.5+%、アルファ・エイサー社製);トリフルオロメタンスルホン酸(TfOH、99%,オークウッドケミカル製);トリフルオロ酢酸(TFA、99%、アルファ・エイサー社製);ポリビニルアルコール(PVA,平均Mw13000−23000、98%加水分解、シグマ−アルドリッチ製);酢酸アンモニウム(CH3CO2NH4、97%、アルファ・エイサー社製);水酸化アンモニウム溶液(NH4OH、ACS試薬、シグマ−アルドリッチ製);及びクエン酸(97%、アルファ・エイサー社製)を、さらに精製することなく使用した。
Al2(CO3)3(138g、0.59mol、1当量)をH2O(600mL)中に混合したものに、HTf2N水溶液(6当量、995g、3.54モルを300mLのH2O中に加えたもの)を、室温で磁気撹拌しながら一部ずつ添加した。混濁した混合物は泡状となり、温かくなった。2時間後、混合物を60℃で一晩加熱し、透明な淡黄色液体を得た。混合物を室温まで冷却した後、追加のH2Oを添加して、混合物の全体積を1.2Lにした。
2mLのアルミニウム錯体水溶液を調製するため、Al2(CO3)3(0.23g、1mmol)とH2O(0.5mL)との混合物を室温で撹拌した。有機酸(6mmol又は12mmol;Alに対して3又は6当量、表1参照)をゆっくりと混合物に加え、濁った水性混合物を得た。さらに1時間撹拌した後、混合物を約60℃に一晩加熱し、透明な液体を得た。混合物を室温まで冷却した後、H2Oを添加して、溶液を一定のモル濃度(0.5M又は1M、表1参照)に調製した。
アルミニウムめっき試験1
アルミニウムめっきプロセスの一実施例では、0.3MのAl(Tf2N)3水溶液を、1Mの酢酸アンモニウムの追加の電解質とともに使用した。0.5重量%のPVAの添加剤を添加した。この溶液100mLを用い、0.5Aで30分間ハルセルめっきを行い、高電流密度端に粉末状析出物を生じさせ、低電流密度端にはめっきを生じさせず、40A/dm2〜150A/dm2の間の平滑な反射性の金属コーティングを生じさせた。このめっき溶液を緩衝してpHを4.8〜5.0の間とし、温度を40℃とした。この溶液には、電気分解後(post electrolysis)、かなりの暗色の沈殿物(precipitate)及び大量の泡立ちが生じていた。当該走査型電子顕微鏡(SEM)及びエネルギー分散型X線(EDX)分光分析により、平滑な反射性アルミニウムの暗色の金属析出物が見られた。例えば図5を参照されたい。
アルミニウムめっきプロセスのさらなる実施例では、0.3MのAl(Tf2N)3水溶液を、1Mクエン酸からNH4OHで滴定した1Mクエン酸アンモニウムの追加の電解質とともに使用した。0.5重量%のPVAの添加剤を添加した。この溶液100mLを用い、0.5Aで30分間ハルセルめっきを行い、高電流密度端により厚く(40A/dm2超)さらに暗色の析出物を生じさせ、低電流密度端ではめっきを生じさせなかった(40A/dm2未満)。このコーティングは、高電流密度端で最も厚く、光沢があり金属質であった。めっき溶液を緩衝してpHを2.8〜3.2の間とし、温度を40℃とした。この溶液は、電気分解後(post electrolysis)、淡暗色の沈殿物を生じていたが、この場合に泡立ちは見られなかった。SEM及びEDX分析により、高電流密度から低電流密度への明確な析出勾配を有する、平滑な反射性アルミニウムの暗色の金属析出物が見られる。
アルミニウム対配位子比が1:1の0.5MのAl(OMs)及び1Mクエン酸アンモニウムの10mL試験アリコートを使用して、20AWGの銅ワイヤを10μmを超える厚さに良好に(successfully)めっきした。本手法では、陰極基体として銅線(20AWG、長さ6mm)とアルミニウムの対向/参照電極を備えた2電極システムを使用した。クロノポテンシオメトリーを−20mA(−120mA・cm−2)で3時間行った(図5)。初めから終わりまで、浴温度を54℃に制御し維持した。
種々の配位子構造を有する様々なアルミニウム塩が開発されている(表2参照)。配位子は、二座配位子である可能性が高いTf2Nを除き、一般に単座配位と考えられている。各配位子は、本来、程度の差はあっても、電子求引性であると考えられている。特定の理論に縛られることは望まないが、この電子求引性は、電子求引性が最も強い置換基を有するアルミニウム(又は本明細書に記載の他の任意の金属)の還元電位を、負の電位がより低い方向にシフトさせる傾向があると考えられる。図2は、その酸のpKaから推定される各置換基の比較電子求引性を示す。一般に、より強い酸は、脱プロトン化した形態の酸をより安定化することができ、各pKaを低下させる。
Claims (25)
- 酸素含有雰囲気下で、0.5気圧(50.66kPa)〜5気圧(506.62kPa)において、10℃〜70℃の温度で、少なくとも1種の反応性金属を導電性基板の表面に電着する方法であって、水性溶媒中に溶解した金属錯体の電気化学的還元を介して前記少なくとも1種の反応性金属を電着することを含み、前記金属錯体は、金属中心及び配位子(リガンド)を含み、
前記反応性金属は、アルミニウムであり、
前記配位子は、スルホン酸配位子及びスルホンイミド配位子の少なくとも1つである、方法。 - 前記少なくとも1つのスルホン酸配位子は、式SO3R1で表される配位子であり、式中、R1は、ハロ;置換又は非置換C6−C18−アリール;置換又は非置換C1−C6−アルキル、置換又は非置換C6−C18−アリール−C1−C6−アルキルである、請求項1に記載の方法。
- 前記少なくとも1つのスルホンイミド配位子は、式N(SO2R1)で表される配位子
であり、式中、R1は、ハロ;置換又は非置換C6−C18−アリール;置換又は非置換C1−C6−アルキル;置換又は非置換C6−C18−アリール−C1−C6−アルキルである、請求項1に記載の方法。 - 前記少なくとも1つのスルホン酸配位子は、以下の式:
- 前記少なくとも1つのスルホンイミド配位子は、以下の式:
- 前記金属錯体は、式Al(SO3R1)n及びAl[N(SO3R1)2]nで表される金属錯体の少なくとも一方であり、式Al(SO3R1)n中、R1はハロ;置換又は非置換C6−C18−アリール;置換又は非置換C1−C6−アルキル;置換又は非置換C6−C18−アリール−又は置換又は非置換C1−C6−アルキルであり、nは2〜8の整数であり、及び、式Al[N(SO3R1)2]n中、R1は、ハロ;置換又は非置換C6−C18−アリール;置換又は非置換C1−C6−アルキル;置換又は非置換C6−C18−アリール−C1−C6−アルキルであり、nは1〜4の整数である、請求項1に記載の方法。
- 前記水性溶媒は電解質を含む、請求項1に記載の方法。
- 前記電解質は、ハロゲン化物電解質、過塩素酸電解質、アミドスルホン酸電解質、ヘキサフルオロケイ酸電解質、テトラフルオロホウ酸電解質、メタンスルホン酸電解質、及びカルボン酸塩電解質のうちの少なくとも1つを含む、請求項7に記載の方法。
- 前記電解質は、式R3CO2 −で表される化合物のうち少なくとも1つを含み、式中、R3は置換又は非置換C6−C18−アリール;又は置換又は非置換C1−C6−アルキルである、請求項8に記載の方法。
- 前記電解質は、ポリカルボン酸塩電解質、及びラクトンのうち少なくとも1つを含む、請求項8に記載の方法。
- 前記水性溶媒を緩衝して、pHを1〜7とする、請求項1に記載の方法。
- 前記水性溶媒は、水混和性有機溶媒を含む、請求項1に記載の方法。
- 前記水混和性有機溶媒は、C1−C6−アルカノール、C2−C10−ポリオール、(ポリ)アルキレングリコールエーテル、C2−C10−カルボン酸、C2−C10−ケトン、C2−C10−アルデヒド、ピロリドン、C2−C10−ニトリル、フタル酸塩、C2−C10−ジアルキルアミン、C2−C10−ジアルキルホルムアミド、C2−C10−ジアルキルスルホキシド、C4−C10−ヘテロシクロアルカン、アミノアルコール、及びC4−C10−ヘテロアリーレンのうちの少なくとも1つを含む、請求項12に記載の方法。
- 前記C1−C6−アルカノールは、エタノールを含む、請求項13に記載の方法。
- 前記電着することは、前記少なくとも1種の反応性金属の少なくとも1層を基板の表面上に電着することを含む、請求項1に記載の方法。
- 前記電着することは、前記少なくとも1種の反応性金属の少なくとも2層を基板の表面上に電着することを含む、請求項1に記載の方法。
- 酸素含有雰囲気下で、0.5気圧(50.66kPa)〜5気圧(506.62kPa)において、10℃〜70℃の温度で、アルミニウムを導電性基板の表面に電着する方法であって、水性溶媒中に溶解したアルミニウム錯体の電気化学的還元を介して前記アルミニウムを電着することを含む方法であって、前記アルミニウム錯体は、アルミニウム中心及び配位子(リガンド)を含み、少なくとも1つの配位子は電子求引性配位子であり、前記配位子は、それぞれ、電子求引性であり、アルミニウム錯体中のアルミニウムの還元電位を減少して、水分解により水素ガスを発生させる過電圧を下回るようにするか、前記配位子は、スルホン酸配位子及びスルホンイミド配位子の少なくとも1つである、方法。
- 酸素含有雰囲気下で、0.5気圧(50.66kPa)〜5気圧(506.62kPa)において、10℃〜70℃の温度で、少なくとも1種の反応性金属を導電性基板の表面に電着する方法であって、水性溶媒中に溶解した金属錯体の電気化学的還元を介して前記少なくとも1種の反応性金属を電着することを含む方法であって、
前記反応性金属は、アルミニウムであり、
前記金属錯体は金属中心及び配位子を含み、
前記配位子の少なくとも1つは電子求引性配位子であり、各配位子はそれぞれ電子求引性であり、金属錯体中の金属の還元電位を減少して、水分解により水素ガスを発生させる過電圧を下回るようにする、方法。 - 酸素含有雰囲気下で、0.5気圧(50.66kPa)〜5気圧(506.62kPa)において、10℃〜70℃の温度で、少なくとも1種の反応性金属を導電性基板の表面に電着する方法であって、少なくとも50%水溶性である溶媒中に溶解した金属錯体の電気化学的還元を介して前記少なくとも1種の反応性金属を電着することを含む方法であって、
前記金属錯体は、金属中心及び配位子を含み、
前記反応性金属は、アルミニウムであり、
前記配位子は、スルホン酸配位子及びスルホンイミド配位子の少なくとも1つである、方法。 - 前記溶媒は少なくとも60%水溶性である、請求項19に記載の方法。
- 前記溶媒は少なくとも70%水溶性である、請求項20に記載の方法。
- 前記溶媒は少なくとも80%水溶性である、請求項21に記載の方法。
- 前記溶媒は少なくとも90%水溶性である、請求項22に記載の方法。
- 前記溶媒は少なくとも99%水溶性である、請求項23に記載の方法。
- 前記水性溶媒は水からなる、請求項1に記載の方法。
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