CN100510174C - 化学镀金液 - Google Patents
化学镀金液 Download PDFInfo
- Publication number
- CN100510174C CN100510174C CNB2004800160274A CN200480016027A CN100510174C CN 100510174 C CN100510174 C CN 100510174C CN B2004800160274 A CNB2004800160274 A CN B2004800160274A CN 200480016027 A CN200480016027 A CN 200480016027A CN 100510174 C CN100510174 C CN 100510174C
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- CN
- China
- Prior art keywords
- gold plating
- gold
- plating liquid
- replace
- substituent
- 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.)
- Expired - Lifetime
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- 238000007747 plating Methods 0.000 title claims abstract description 69
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000010931 gold Substances 0.000 title claims abstract description 47
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 47
- -1 amine compound Chemical class 0.000 claims abstract description 30
- 150000003839 salts Chemical class 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 10
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 8
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 5
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 4
- 239000000126 substance Substances 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 34
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 10
- 239000011734 sodium Chemical group 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 9
- 150000002344 gold compounds Chemical class 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000002829 reductive effect Effects 0.000 claims description 6
- UOULCEYHQNCFFH-UHFFFAOYSA-M sodium;hydroxymethanesulfonate Chemical compound [Na+].OCS([O-])(=O)=O UOULCEYHQNCFFH-UHFFFAOYSA-M 0.000 claims description 3
- 125000001424 substituent group Chemical group 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 16
- 238000005260 corrosion Methods 0.000 abstract description 16
- 239000002253 acid Substances 0.000 abstract description 7
- 125000001539 acetonyl group Chemical group [H]C([H])([H])C(=O)C([H])([H])* 0.000 abstract description 4
- 125000002541 furyl group Chemical group 0.000 abstract description 4
- 125000001624 naphthyl group Chemical group 0.000 abstract description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 4
- 125000004076 pyridyl group Chemical group 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000005476 soldering Methods 0.000 abstract 1
- 125000004417 unsaturated alkyl group Chemical group 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 28
- 229910052759 nickel Inorganic materials 0.000 description 14
- 238000003466 welding Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 229910052783 alkali metal Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical class NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 4
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000002431 hydrogen Chemical group 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 239000008139 complexing agent Substances 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-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
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- XKUKSGPZAADMRA-UHFFFAOYSA-N glycyl-glycyl-glycine Chemical compound NCC(=O)NCC(=O)NCC(O)=O XKUKSGPZAADMRA-UHFFFAOYSA-N 0.000 description 2
- YMAWOPBAYDPSLA-UHFFFAOYSA-N glycylglycine Chemical compound [NH3+]CC(=O)NCC([O-])=O YMAWOPBAYDPSLA-UHFFFAOYSA-N 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 1
- TYFSYONDMQEGJK-UHFFFAOYSA-N 2-(2,2-dihydroxyethylamino)acetic acid Chemical compound OC(O)CNCC(O)=O TYFSYONDMQEGJK-UHFFFAOYSA-N 0.000 description 1
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- XLJGIXLDEYIALO-UHFFFAOYSA-N 2-(carboxymethylamino)-4-hydroxybutanoic acid Chemical compound OCCC(C(O)=O)NCC(O)=O XLJGIXLDEYIALO-UHFFFAOYSA-N 0.000 description 1
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- 108010008488 Glycylglycine Proteins 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000002648 azanetriyl group Chemical group *N(*)* 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- IFQUWYZCAGRUJN-UHFFFAOYSA-N ethylenediaminediacetic acid Chemical compound OC(=O)CNCCNCC(O)=O IFQUWYZCAGRUJN-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 108010067216 glycyl-glycyl-glycine Proteins 0.000 description 1
- 229940043257 glycylglycine Drugs 0.000 description 1
- JCDVTZPJEWWGHU-UHFFFAOYSA-N gold sulfurous acid Chemical compound [Au].S(O)(O)=O JCDVTZPJEWWGHU-UHFFFAOYSA-N 0.000 description 1
- MXZVHYUSLJAVOE-UHFFFAOYSA-N gold(3+);tricyanide Chemical compound [Au+3].N#[C-].N#[C-].N#[C-] MXZVHYUSLJAVOE-UHFFFAOYSA-N 0.000 description 1
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 description 1
- TVGIYTJTDDLBJP-UHFFFAOYSA-N gold;thiocyanic acid Chemical compound [Au].SC#N TVGIYTJTDDLBJP-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- SYECJBOWSGTPLU-UHFFFAOYSA-N hexane-1,1-diamine Chemical compound CCCCCC(N)N SYECJBOWSGTPLU-UHFFFAOYSA-N 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- RTWNYYOXLSILQN-UHFFFAOYSA-N methanediamine Chemical compound NCN RTWNYYOXLSILQN-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229940045641 monobasic sodium phosphate Drugs 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 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
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 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
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 150000003476 thallium compounds Chemical class 0.000 description 1
- UCGZDNYYMDPSRK-UHFFFAOYSA-L trisodium;gold;hydroxy-oxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [Na+].[Na+].[Na+].[Au].OS([S-])(=O)=O.OS([S-])(=O)=O UCGZDNYYMDPSRK-UHFFFAOYSA-L 0.000 description 1
Images
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
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/24—Reinforcing the conductive pattern
- H05K3/244—Finish plating of conductors, especially of copper conductors, e.g. for pads or lands
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
本发明的目的在于提供一种化学镀金液，其可以得到表面没有孔腐蚀的镀金被膜，在焊接时可以确保足够的焊接强度。本发明提供一种化学镀金液，其特征在于，含有水溶性金化合物、下述通式所示的羟基烷基磺酸或其盐作为还原剂、和胺化合物，(上式中，R表示氢、羧基、或可以有取代基的苯基、萘基、饱和或不饱和的烷基、乙酰基、丙酮基、吡啶基和呋喃基中的任一种，X表示氢、Na、K和NH4中的任一种，n是0～4的整数)。
Description
技术领域
本发明涉及镀敷技术和化学镀金液。
背景技术
化学镀金适用于印制布线板的电路、IC封装、ITO基板、IC卡等电子工业部件的接头、电路表面。
在基底化学镀镍被膜上进行厚度为0.05～0.1μm的置换型化学镀金的情况下，特别是在镀敷反应刚开始后，镍与金的置换反应很快，选择性地强力攻击化学镀镍被膜中的析出粒子的粒界部分，析出粒子的侵蚀深入进行，在镀金被膜的下面形成缺陷部分。随着情况的不同，缺陷部分或者连续或者集中，甚至引起镀金被膜的外观不良(表面发生孔腐蚀)。进而虽然析出的金被膜的膜厚很薄、小于等于0.1μm，但是由于侵蚀的深度很深，这样的置换型镀金液引起的化学镀镍被膜的脆弱化以及与镀金被膜的粘结性不足，所以在耐久性试验时发生剥离，在焊接时不能确保足够的焊接强度。在这样现有技术的化学镀金液中，由于在镀金被膜表面存在孔腐蚀、焊接强度不足而产生劣质品，这在球状矩阵排列(BGA)型半导体封装等中成为了大问题。
在特开2001-107259号公报中，作为置换型化学镀金液，公开了含有次磷酸盐或肼、和直锁状烷基胺的化学镀金液。该置换型化学镀金液的目的在于减少基底镍表面的粗糙、减少焊接球等的焊接部件的粘结强度(剪切强度)由热经历引起的降低。
另外，在特开平6-280039号公报中公开了，在含有水溶性金化合物、络合剂、还原剂和胺等含氮化合物的化学镀浴中添加非离子表面活性剂和/或非离子性聚合物作为稳定剂，可以尽可能地防止镀敷扩展的发生。
发明内容
本发明的目的在于提供一种化学镀金液，其可以得到表面没有孔腐蚀的镀金被膜，在进行焊接时可以确保足够的焊接强度。
本发明者为了解决上述课题进行了深入研究，结果发现通过使化学镀金液含有特定的羟基烷基磺酸或其盐、并含有胺化合物，可以得到表面没有孔腐蚀的镀金被膜，从而完成了本发明。即，本发明如下所述。
(1)一种化学镀金液，其特征在于，含有水溶性金化合物，含有下述通式所示的羟基烷基磺酸或其盐作为还原剂、和胺化合物，
(上式中，R表示氢、羧基、或可以有取代基的苯基、萘基、饱和或不饱和的烷基、乙酰基、丙酮基、吡啶基和呋喃基中的任一种，X表示氢、Na、K和NH4中的任一种，n是0～4的整数)。
(2)如上述(1)所述的化学镀金液，其特征在于，还含有磷酸系化合物。
(3)如上述(1)或(2)所述的化学镀金液，其特征在于，上述通式所示的还原剂为羟基甲磺酸钠(HOCH2SO3Na)。
(4)如上述(1)～(3)的任一项所述的化学镀金液，其特征在于，上述胺化合物为三亚乙基四胺(H2N(CH2)2NH(CH2)2NH(CH2)2NH2)。
(5)一种镀金物，其特征在于，是使用上述(1)～(4)的任一项所述的化学镀金液制作的。
附图说明
图1是实施例1的镀金被膜表面的SEM照片。
图2是比较例1的镀金被膜表面的SEM照片。
图3是比较例2的镀金被膜表面的SEM照片。
具体实施方式
下面，对本发明的化学镀金液进行详细说明。
本发明的镀金液，成为金源的金化合物只要是水溶性即可，没有特别的限定，其最大的特征在于，含有特定的羟基烷基磺酸或其盐、和胺化合物。
因此，本发明的镀金液是在水系溶剂中至少溶解有水溶性金化合物、特定的羟基烷基磺酸或其盐、和胺化合物的物质，作为溶剂，优选为水。
作为水溶性金化合物，优选使用氰化金、亚硫酸金、硫代硫酸金、硫氰酸金、氯金酸或其盐，如钠盐、钾盐、铵盐等。本发明的化学镀金液中的这些金化合物以镀敷液中的金浓度计，优选含有0.1～100g/L，更优选含有0.5～20g/L。如果金浓度小于0.1g/L，则金的置换速度显著变慢，如果超过100g/L，则效果饱和，没有优势。
作为还原剂，使用下述通式所示的羟基烷基磺酸或其盐。
(上式中，R表示氢、羧基、或可以有取代基的苯基、萘基、饱和或不饱和的烷基、乙酰基、丙酮基、吡啶基和呋喃基中的任一种，X表示氢、Na、K和NH4中的任一种，n是0～4的整数。)
上式中，作为R中的苯基、萘基、饱和或不饱和的烷基、乙酰基、丙酮基、吡啶基和呋喃基的取代基，可以列举出，卤素、烷氧基、硝基、羟基、磺酸基或其盐、苯基、乙酰基等。作为卤素，优选为氯，作为烷氧基，优选为低级烷氧基、例如甲氧基。另外，作为磺酸基的盐，可以列举出碱金属盐等，优选为钠盐。
作为饱和或者不饱和的烷基，优选为碳原子数为1～4的烷基。
另外，上式中，作为X优选为钠。
作为上述通式所示的羟基烷基磺酸或其盐的具体例，可以列举出以下化合物，优选使用No.1和2的化合物。
1 HO—CH2—SO3Na
2 HO—CH2—CH2—SO3Na
上述羟基烷基磺酸或其盐，在镀敷液中优选含有0.1～20g/L，更优选含有0.5～10g/L。如果含有量小于0.1g/L，则金析出速度变慢，另外，如果超过20g/L，则因为引起镀浴分解的可能性提高，所以不优选。
作为胺化合物，可以是二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺等1分子中有伯胺和仲胺的化合物；甲胺、乙胺、丙胺、丁胺、戊胺、己胺等的单胺化合物；亚甲基二胺、1，2-乙二胺、丙邻二胺、亚丁基二胺、戊二胺、己二胺等的二胺化合物。
另外，还可以列举出在上述化合物中进一步结合有苯环等芳香环的芳香族胺、直接结合有氨基的苯胺等芳香族胺化合物。另外，为了提高对水的溶解性，也可以使用在上述化合物中结合有羟基、羧基、磺酸基等高极性取代基的化合物、形成了盐酸盐等盐的化合物。
胺化合物在镀敷液中，优选含有0.1～30g/L，更优选含有0.5～20g/L。如果含有量小于0.1g/L，则镍表面的粒界发生侵蚀，有时引起镀金被膜的外观不良。另外，如果含有量超过30g/L，则因为引起镀浴分解的可能性提高，所以不优选。
另外，本发明的化学镀金液，根据需要，可以添加磷酸系化合物作为pH缓冲剂。
作为磷酸系化合物，可以列举出，磷酸、焦磷酸、或它们的碱金属盐、碱土类金属盐、铵盐、磷酸二氢碱金属盐、磷酸二氢碱土类金属盐、磷酸二氢铵、磷酸氢二碱金属盐、磷酸氢二碱土类金属盐、磷酸氢二铵等。镀敷液中的磷酸系化合物的浓度优选为0.1～200g/L，更优选为1～100g/L。
另外，本发明的镀金液还可以含有氨基羧酸化合物作为络合剂，作为氨基羧酸化合物，可以列举出，乙二胺四乙酸(EDTA)、羟基乙基乙二胺三乙酸、二羟基乙基乙二胺二乙酸、丙二胺四乙酸、二亚乙基三胺五乙酸、三亚乙基四胺六乙酸、甘氨酸、甘氨酰甘氨酸、甘氨酰甘氨酰甘氨酸、二羟基乙基甘氨酸、亚氨基二乙酸、羟基乙基亚氨基二乙酸、次氮基三乙酸、次氮基三丙酸、或其碱金属盐、碱土类金属盐、铵盐等。镀敷液中的氨基羧酸化合物的浓度优选为0.1～200g/L，更优选为1～100g/L。如果氨基羧酸化合物的浓度小于0.1g/L，则作为络合剂的效果不足，即使超过200g/L，效果饱和，没有优势。
在本发明的镀金液中，还可以添加用于使金络合物稳定化、提高镀浴稳定性的氰化钾、氰化钠等的氰化化合物。如果氰化化合物的添加量过多，则腐蚀基底镍被膜，很容易发生孔腐蚀，因此，优选在0.01～5g/L的范围内添加。
进而，作为反应促进剂，添加铊化合物、铅化合物也是有效的。作为它们的添加量，以金属计，优选为0.01～50mg/L。如果反应促进剂的添加量过多，则引起镀浴分解。
从金的析出速度、镀膜的外观和镀浴稳定性的观点出发，本发明的镀金液的pH值优选为5～9，特别优选6～8。
对于pH的调整，可以使用氢氧化钾、氢氧化钠、氨等的碱性化合物、硫酸、磷酸等的酸性化合物。
另外，从镀浴的稳定性和金的析出速度的观点出发，本发明的镀金液优选在镀浴温度为60～90℃使用。
在使用本发明的镀金液进行镀敷时，将印制布线板等的被镀敷材料浸渍在镀浴中。被镀敷材料优选为基底进行过镀镍等之后的材料，如果使用本发明的镀金液进行镀敷，则在得到的镀金被膜的表面看不见孔腐蚀，与基底镀镍被膜的粘结性好，在进行焊接时能确保足够的焊接强度。
实施例
用如下所示的实施例和比较例，对本发明优选的实施方式进行说明。实施例1～2和比较例1～2
调制表1所示的各组成的镀金液浴。作为被镀敷材料，使用镀铜印制布线板，如下所示进行直至化学镀金为止的工序，用表1记载的条件进行化学镀金。
酸性脱脂工序(日矿メタルプレ—ティング制KG-512)45℃、5分钟
→热水洗涤50～60℃、1分钟
→水洗
→软蚀刻(过硫酸钠80g/L，硫酸20ml/L)
→水洗
→酸洗涤(硫酸30ml/L)
→水洗
→活化(日矿メタルプレ—ティング制KG-522)25℃，3分钟
→水洗
→酸浸渍(硫酸30ml/L)
→水洗
→化学镀镍(日矿メタルプレ—ティング制KG-530)85℃，3分钟
→水洗
→化学镀金
对得到的镀膜进行如下评价。用SEM放大3000倍观察有无孔腐蚀。图1～3分别显示实施例1和比较例1～2的镀金被膜的SEM照片。照片中以黑点的形式观察到孔腐蚀。在实施例1的镀金被膜上没有看到该黑点即孔腐蚀，但是在比较例1和2的镀金被膜中看到了孔腐蚀。另外，实施例2的镀金被膜也与实施例1同样，没有看见孔腐蚀。
另外，通过进行20分钟的镀敷后，使用セイコ—电子工业(株)制荧光X射线膜厚度计SFT-3200，测定镀膜厚度，来求出析出速度。
评价结果如表1所示。
表1
化学镀金液的组成及其特性
| 实施例1 | 实施例2 | 比较例1 | 比较例2 | |
| 孔腐蚀 | ○ | ○ | × | △ |
| 析出速度(μm/20min) | 0.12 | 0.10 | 0.081 | 0.055 |
| 氰化金钾(g/L) | 2 | 2 | 2 | 2 |
| EDTA(g/L) | 10 | 10 | 0 | 10 |
| 三亚乙基四胺(g/L) | 10 | 10 | 0 | 10 |
| 磷酸二氢钠·2水合物(g/L) | 34 | 34 | 34 | 34 |
| 羟基甲磺酸钠(g/L) | 2 | - | 2 | 0 |
| 羟基乙磺酸钠(g/L) | - | 2 | - | - |
| pH | 7.0 | 7.0 | 7.0 | 7.0 |
| 镀浴温度(℃) | 88 | 88 | 88 | 88 |
用氢氧化钾来调整pH
下面，对实施例1和比较例1中得到的镀膜，进行焊接粘结强度的试验。
焊接粘结强度，使用Pb/Sn＝37/63、0.4mmΦ(SPARKLE BALLS千住金属制)作为焊接球，使用RMA型(NH-100VK-1アサヒ化学研究所制)作为焊剂，如下进行加热式碰撞拉伸试验(heat bump pull test)。试验进行12次，表2示出其中除去了异常值的最大值、最小值和平均值。
测定设备：粘结试验机4000系列(デイジ社制)
加热条件：设定温度 270℃
加热时间 5秒
冷却结束 50℃
试验速度 300μm/秒
回流炉：远红外线式回流焊接装置(RF-330日本パルス技术研究所制)
回流条件：峰温度 230℃
表2
| 实施例1 | 比较例1 | |
| 最大值 | 1462 | 1377 |
| 最小值 | 1181 | 976 |
| 平均值 | 1321 | 1185 |
单位：gf
由表2的结果可知，实施例1中得到的被膜的焊接粘结强度高于比较例1得到的被膜的焊接粘结强度。可以认为这是因为实施例1的被膜没有孔腐蚀，镍向镀金层的扩散少，镍表面很难形成磷含有率高的层，或者是由于没有孔腐蚀，镍表面很难氧化，提高了焊接粘结强度。
工业可利用性
如果使用本发明的化学镀金液，则可以得到表面没有孔腐蚀的镀金被膜。进而，如果将本发明的化学镀金液用于印制布线板的电路、IC封装、IT0基板、IC卡等电子工业部件的接头和电路表面上，则可以提高与基底的化学镀镍被膜的粘结性，在焊接时能够确保足够的焊接强度。
Claims (5)
1.一种化学镀金液，其特征在于，含有水溶性金化合物，含有下述通式所示的羟基烷基磺酸或其盐作为还原剂、并含有胺化合物，
上式中，R表示氢、羧基、未取代或具有取代基的苯基、未取代或具有取代基的萘基、未取代或具有取代基的饱和或不饱和的烷基、未取代或具有取代基的乙酰基、未取代或具有取代基的丙酮基、未取代或具有取代基的吡啶基和未取代或具有取代基的呋喃基中的任一种，X表示氢、Na、K和NH4中的任一种，n是0～4的整数。
2.如权利要求1所述的化学镀金液，其特征在于，还含有磷酸系化合物。
3.如权利要求1或2所述的化学镀金液，其特征在于，上述通式所示的还原剂为羟基甲磺酸钠HOCH2SO3Na。
4.如权利要求1或2所述的化学镀金液，其特征在于，上述胺化合物为三亚乙基四胺H2N(CH2)2NH(CH2)2NH(CH2)2NH2。
5.如权利要求3所述的化学镀金液，其特征在于，上述胺化合物为三亚乙基四胺H2N(CH2)2NH(CH2)2NH(CH2)2NH2。
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| JP416315/2003 | 2003-12-15 | ||
| PCT/JP2004/004656 WO2004111287A1 (ja) | 2003-06-10 | 2004-03-31 | 無電解金めっき液 |
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| JP5526459B2 (ja) * | 2006-12-06 | 2014-06-18 | 上村工業株式会社 | 無電解金めっき浴及び無電解金めっき方法 |
| JP4941650B2 (ja) * | 2007-01-11 | 2012-05-30 | 上村工業株式会社 | 無電解金めっき浴のめっき能維持管理方法 |
| JP5013077B2 (ja) * | 2007-04-16 | 2012-08-29 | 上村工業株式会社 | 無電解金めっき方法及び電子部品 |
| JP6619563B2 (ja) * | 2015-04-30 | 2019-12-11 | 日本高純度化学株式会社 | 無電解金めっき液、アルデヒド−アミン付加体補給液及びそれらを用いて形成した金皮膜 |
| CN105543816A (zh) * | 2016-02-01 | 2016-05-04 | 哈尔滨工业大学（威海） | 一种化学镀金液 |
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| JPWO2004111287A1 (ja) | 2006-07-20 |
| WO2004111287A2 (ja) | 2004-12-23 |
| JP4638818B2 (ja) | 2011-02-23 |
| TW200500496A (en) | 2005-01-01 |
| KR100749992B1 (ko) | 2007-08-16 |
| WO2004111287A3 (ja) | 2005-03-03 |
| CN1802452A (zh) | 2006-07-12 |
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