JP5411561B2 - インジウム電気めっき組成物においてインジウムイオンを補充する方法 - Google Patents
インジウム電気めっき組成物においてインジウムイオンを補充する方法 Download PDFInfo
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- JP5411561B2 JP5411561B2 JP2009101970A JP2009101970A JP5411561B2 JP 5411561 B2 JP5411561 B2 JP 5411561B2 JP 2009101970 A JP2009101970 A JP 2009101970A JP 2009101970 A JP2009101970 A JP 2009101970A JP 5411561 B2 JP5411561 B2 JP 5411561B2
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- indium
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- metal
- acid
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- 229910052697 platinum Inorganic materials 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- 229940107700 pyruvic acid Drugs 0.000 description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 2
- 229960004889 salicylic acid Drugs 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 150000003536 tetrazoles Chemical class 0.000 description 2
- 229960002898 threonine Drugs 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229960004295 valine Drugs 0.000 description 2
- 239000004474 valine Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- RBNPOMFGQQGHHO-UHFFFAOYSA-N -2,3-Dihydroxypropanoic acid Natural products OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 description 1
- ODJKHOBNYXJHRG-UHFFFAOYSA-N 1,3-dimethylimidazole Chemical compound CN1[CH]N(C)C=C1 ODJKHOBNYXJHRG-UHFFFAOYSA-N 0.000 description 1
- RPNQVCXMPGHQPH-UHFFFAOYSA-N 1-(2-methylphenyl)-4,5-dihydroimidazole Chemical compound CC1=CC=CC=C1N1C=NCC1 RPNQVCXMPGHQPH-UHFFFAOYSA-N 0.000 description 1
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical class CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 1
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 1
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 description 1
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 description 1
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 1
- AEGRGDYHZFLAGY-UHFFFAOYSA-N 2-amino-1h-imidazol-5-ol Chemical compound NC1=NC=C(O)N1 AEGRGDYHZFLAGY-UHFFFAOYSA-N 0.000 description 1
- LTHNHFOGQMKPOV-UHFFFAOYSA-N 2-ethylhexan-1-amine Chemical compound CCCCC(CC)CN LTHNHFOGQMKPOV-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- BKCCAYLNRIRKDJ-UHFFFAOYSA-N 2-phenyl-4,5-dihydro-1h-imidazole Chemical compound N1CCN=C1C1=CC=CC=C1 BKCCAYLNRIRKDJ-UHFFFAOYSA-N 0.000 description 1
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 1
- BCSZNBYWPPFADT-UHFFFAOYSA-N 4-(1,2,4-triazol-4-ylmethyl)benzonitrile Chemical compound C1=CC(C#N)=CC=C1CN1C=NN=C1 BCSZNBYWPPFADT-UHFFFAOYSA-N 0.000 description 1
- AVKRFEZLHPIAJO-UHFFFAOYSA-N 5-ethyl-1h-imidazol-4-ol Chemical compound CCC=1NC=NC=1O AVKRFEZLHPIAJO-UHFFFAOYSA-N 0.000 description 1
- LPULCTXGGDJCTO-UHFFFAOYSA-N 6-methylheptan-1-amine Chemical compound CC(C)CCCCCN LPULCTXGGDJCTO-UHFFFAOYSA-N 0.000 description 1
- DZDVMKLYUKZMKK-UHFFFAOYSA-N 7-methyloctan-1-amine Chemical compound CC(C)CCCCCCN DZDVMKLYUKZMKK-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RBNPOMFGQQGHHO-UWTATZPHSA-N D-glyceric acid Chemical compound OC[C@@H](O)C(O)=O RBNPOMFGQQGHHO-UWTATZPHSA-N 0.000 description 1
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 1
- 208000032368 Device malfunction Diseases 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- WJYIASZWHGOTOU-UHFFFAOYSA-N Heptylamine Chemical compound CCCCCCCN WJYIASZWHGOTOU-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- KVQWOXMVXMDOHN-UHFFFAOYSA-N OCC(O)CO.[In] Chemical class OCC(O)CO.[In] KVQWOXMVXMDOHN-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical class [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229920002214 alkoxylated polymer Polymers 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- VUAQKPWIIMBHEK-UHFFFAOYSA-K bis(methylsulfonyloxy)indiganyl methanesulfonate Chemical compound [In+3].CS([O-])(=O)=O.CS([O-])(=O)=O.CS([O-])(=O)=O VUAQKPWIIMBHEK-UHFFFAOYSA-K 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
- 150000003842 bromide salts Chemical class 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- QDHFHIQKOVNCNC-UHFFFAOYSA-N butane-1-sulfonic acid Chemical compound CCCCS(O)(=O)=O QDHFHIQKOVNCNC-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940043264 dodecyl sulfate Drugs 0.000 description 1
- JZKFHQMONDVVNF-UHFFFAOYSA-N dodecyl sulfate;tris(2-hydroxyethyl)azanium Chemical compound OCCN(CCO)CCO.CCCCCCCCCCCCOS(O)(=O)=O JZKFHQMONDVVNF-UHFFFAOYSA-N 0.000 description 1
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical group 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- AMNSWIGOPDBSIE-UHFFFAOYSA-H indium(3+);tricarbonate Chemical compound [In+3].[In+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O AMNSWIGOPDBSIE-UHFFFAOYSA-H 0.000 description 1
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical class Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical class [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 229910000457 iridium oxide Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- FJDUDHYHRVPMJZ-UHFFFAOYSA-N nonan-1-amine Chemical compound CCCCCCCCCN FJDUDHYHRVPMJZ-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229940100684 pentylamine Drugs 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 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
- 238000007747 plating Methods 0.000 description 1
- 229920001281 polyalkylene Polymers 0.000 description 1
- 229920001521 polyalkylene glycol ether Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- PBMFSQRYOILNGV-UHFFFAOYSA-N pyridazine Chemical compound C1=CC=NN=C1 PBMFSQRYOILNGV-UHFFFAOYSA-N 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
- ABVVEAHYODGCLZ-UHFFFAOYSA-N tridecan-1-amine Chemical compound CCCCCCCCCCCCCN ABVVEAHYODGCLZ-UHFFFAOYSA-N 0.000 description 1
- QFKMMXYLAPZKIB-UHFFFAOYSA-N undecan-1-amine Chemical compound CCCCCCCCCCCN QFKMMXYLAPZKIB-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/16—Regeneration of process solutions
- C25D21/18—Regeneration of process solutions of electrolytes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
-
- 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
- C25D3/54—Electroplating: Baths therefor from solutions of metals not provided for in groups C25D3/04 - C25D3/50
Description
Cobleyらへの米国特許第6,911,068号は不溶性陽極と共に使用されうる電気めっき組成物を開示する。この特許は添加剤の分解を抑制することが認められた1種以上の不飽和有機化合物を導入することにより様々な金属電気めっき組成物における添加剤分解の課題に取り組む。
1)脂肪族鎖アミン;
2)少なくとも2つの反応性窒素部位を有する非置換複素環式窒素化合物;および
3)少なくとも2つの反応性窒素部位を有し、アルキル基、アリール基、ニトロ基、ハロゲンおよびアミノ基から選択される1〜2の置換基を有する置換複素環式窒素化合物;
が挙げられるが、これらに限定されない。
次の実施例は本発明をさらに説明するが、本発明の範囲を限定することを意図するものではない。
次の水性インジウム組成物が製造された:
インジウム組成物のS.G.は、0.5、1、1.5および2のMTOで測定された。図1に示されるように、インジウムの電気めっき中に、S.G.は増加し続けた。S.G.の増加によりインジウム組成物は濁り、これは電気めっき組成物中でその溶解度限界に到達したインジウムイオンとスルファートアニオンの蓄積により引き起こされたと考えられた。このインジウムイオンとスルファートアニオンの蓄積は、硫酸インジウムを用いたインジウムイオンの周期的な補充のためであった。結果的に得られたインジウム堆積物は粗い表面を有していた。インジウム堆積物は均一ではなく、堆積物の縁に沿って孔が存在していた。
次の水性インジウム電気めっき組成物が製造された:
インジウム組成物のS.G.は、0.5、1、1.5、2、2.5および3のMTOで測定された。インジウムイオンが硫酸インジウムで補充された実施例Iのインジウム電気めっき組成物のS.G.と比較して、図2に示されるようにインジウムの電気めっき中にS.G.はゆっくりと増加した。S.G.はMTO=0で1.165からMTO=3で1.18までしか増加しなかった。電気めっき中のインジウム組成物の濁りは観察されなかった。インジウム堆積物は滑らかかつ艶消しであり、インジウム堆積物の縁上に観察可能な孔はなかった。インジウム堆積物は銅板の表面にわたって均一であった。よって、酢酸インジウムを用いたインジウムイオンの補充は、インジウムイオンが硫酸インジウムで補充されたインジウム組成物と比較して、インジウム組成物の電気めっき性能を向上させた。
次の水性インジウム電気めっき組成物が製造された:
インジウム組成物のS.G.は、3、6、7および9のMTOで測定された。インジウムイオンが硫酸インジウムで補充された実施例Iのインジウム電気めっき組成物のS.G.と比較して、図3に示されるようにインジウムの電気めっき中にS.G.はゆっくりと増加した。S.G.はMTO=0で1.09からMTO=6で1.10超までしか増加しせず、次いでMTO=9で1.09超まで減少した。電気めっき中のインジウム組成物の濁りは観察されなかった。インジウム堆積物は滑らかかつ艶消しであり、インジウム堆積物の縁上に観察可能な孔はなかった。インジウム堆積物は銅板の表面にわたって均一であった。よって、酢酸インジウムを用いたインジウムイオンの補充は、インジウムイオンが硫酸インジウムで補充されたインジウム組成物と比較して、インジウム組成物の電気めっき性能を向上させた。
電気めっき組成物において酒石酸インジウムがインジウムイオンを補充するのに使用されることを除いて、上記実施例IIに記載された方法が繰り返される。インジウム電気めっき組成物のS.G.は、電気めっきサイクル中に実質的に同じにとどまっているか、またはゆっくり変化することが予想される。電気めっき中に組成物が濁るとは考えられない。インジウム堆積物は艶消しかつ滑らかな表面外観を有し、かつ均一な厚さを有するものと予想される。さらに、インジウム堆積物の縁上に孔は認められないと予想される。
エピハロヒドリンコポリマーが当該技術分野において公知の従来法により製造される1,2,3−トリアゾール−エピクロロヒドリンコポリマーであることを除いて、上記実施例IIに記載された方法が繰り返される。メタンスルホン酸インジウムが初期組成物中のインジウムイオン源である。電気めっき中にシュウ酸インジウムでインジウムイオンが補充される。インジウム電気めっき組成物のS.G.は、電気めっきサイクル中に実質的に同じにとどまっているか、またはゆっくり変化することが予想される。電気めっき中に組成物が濁るとは考えられない。インジウム堆積物は艶消しかつ滑らかな表面外観を有し、かつ均一な厚さを有するものと予想される。さらに、インジウム堆積物の縁上に孔は認められないと予想される。
エピハロヒドリンコポリマーが当該技術分野において公知の従来法により製造されるピリダジン−エピブロモヒドリンコポリマーであることを除いて、上記実施例IIに記載された方法が繰り返される。初期のインジウムイオン源はスルファミン酸インジウムからで、60g/Lの濃度であり、メタンスルホン酸が60g/Lのスルファミン酸で置き換えられる。電気めっき中にシュウ酸インジウムでインジウムイオンが補充される。インジウム電気めっき組成物のS.G.は、電気めっきサイクル中に実質的に同じにとどまっているか、またはゆっくり変化することが予想される。電気めっき中に組成物が濁るとは考えられない。インジウム堆積物は艶消しかつ滑らかな表面外観を有し、かつ均一な厚さを有するものと予想される。さらに、インジウム堆積物の縁上に孔は認められないと予想される。
エピハロヒドリンコポリマーが当該技術分野において公知の従来法により製造される2−メチルイミダゾール−エピブロモヒドリンコポリマーであることを除いて、上記実施例IIに記載された方法が繰り返される。インジウム組成物中にインジウムイオンを補充するために酢酸インジウムが使用される。インジウム電気めっき組成物のS.G.は、電気めっきサイクル中に実質的に同じにとどまっているか、またはゆっくり変化することが予想される。電気めっき中に組成物が濁るとは考えられない。インジウム堆積物は艶消しかつ滑らかな表面外観を有し、かつ均一な厚さを有するものと予想される。さらに、インジウム堆積物の縁上に孔は認められないと予想される。
インジウム電気めっき組成物が2重量%の硫酸スズをさらに含むことを除いて、上記実施例IIの方法が繰り返される。電流密度は30秒にわたり10A/dm2に維持され、インジウム/スズ金属合金が銅板の上に堆積される。インジウムイオンを補充するためにシュウ酸インジウムが使用される。インジウム電気めっき組成物のS.G.は、電気めっきサイクル中に実質的に同じにとどまっているか、またはゆっくり変化することが予想される。電気めっき中に組成物が濁るとは考えられない。インジウム堆積物は艶消しかつ滑らかな表面外観を有し、かつ均一な厚さを有するものと予想される。さらに、インジウム堆積物の縁上に孔は認められないと予想される。
インジウム電気めっき組成物が2重量%の硫酸亜鉛をさらに含むことを除いて、上記実施例IIの方法が繰り返される。電流密度は20分にわたり10A/dm2に維持され、インジウム/亜鉛金属合金が銅板の上に堆積される。酢酸インジウムでインジウムイオンが補充される。インジウム電気めっき組成物のS.G.は、電気めっきサイクル中に実質的に同じにとどまっているか、またはゆっくり変化することが予想される。電気めっき中に組成物が濁るとは考えられない。インジウム堆積物は艶消しかつ滑らかな表面外観を有し、かつ均一な厚さを有するものと予想される。さらに、インジウム堆積物の縁上に孔は認められないと予想される。
インジウム電気めっき組成物が1重量%の硫酸銅・5水和物をさらに含むことを除いて、上記実施例IIの方法が繰り返される。電流密度は40分にわたり5A/dm2に維持され、インジウム/銅金属合金が銅板の上に堆積される。インジウム電気めっき組成物のS.G.は、電気めっきサイクル中に実質的に同じにとどまっているか、またはゆっくり変化することが予想される。電気めっき中に組成物が濁るとは考えられない。インジウム堆積物は艶消しかつ滑らかな表面外観を有し、かつ均一な厚さを有するものと予想される。さらに、インジウム堆積物の縁上に孔は認められないと予想される。
Claims (7)
- a)1種以上のインジウムイオン源を含む組成物を提供し;
b)インジウム金属を基体上に電気めっきし;および
c)電気めっき中に、酢酸インジウム、ギ酸インジウムおよびシュウ酸インジウムの1種以上でインジウムイオンを組成物に補充すること;
を含む方法。 - 組成物が1種以上の合金形成金属をさらに含む、請求項1に記載の方法。
- 組成物が1種以上のエピハロヒドリンコポリマーをさらに含む、請求項1に記載の方法。
- 1以上の可溶性陽極を含む装置を用いて、インジウムが基体上に電気めっきされる、請求項1に記載の方法。
- 1以上の不溶性陽極を含む装置を用いて、インジウムが基体上に電気めっきされる、請求項1に記載の方法。
- 1以上の不溶性陽極がシールド付き不溶性陽極である、請求項5に記載の方法。
- 組成物の比重が1〜1.2の範囲である、請求項1に記載の方法。
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