CN1802452A - Electroless gold plating solution - Google Patents
Electroless gold plating solution Download PDFInfo
- Publication number
- CN1802452A CN1802452A CNA2004800160274A CN200480016027A CN1802452A CN 1802452 A CN1802452 A CN 1802452A CN A2004800160274 A CNA2004800160274 A CN A2004800160274A CN 200480016027 A CN200480016027 A CN 200480016027A CN 1802452 A CN1802452 A CN 1802452A
- Authority
- CN
- China
- Prior art keywords
- gold plating
- gold
- plating liquid
- compound
- chemical
- 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.)
- Granted
Links
- 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 29
- 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
- 125000001539 acetonyl group Chemical group [H]C([H])([H])C(=O)C([H])([H])* 0.000 claims abstract description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 5
- 125000002541 furyl group Chemical group 0.000 claims abstract description 5
- 125000001624 naphthyl group Chemical group 0.000 claims abstract description 5
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 5
- 125000004076 pyridyl group Chemical group 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
- 239000011734 sodium Chemical group 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 9
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 8
- 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
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 claims description 5
- UOULCEYHQNCFFH-UHFFFAOYSA-M sodium;hydroxymethanesulfonate Chemical compound [Na+].OCS([O-])(=O)=O UOULCEYHQNCFFH-UHFFFAOYSA-M 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 abstract description 16
- 238000005260 corrosion Methods 0.000 abstract description 16
- 239000002253 acid Substances 0.000 abstract description 7
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 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
- 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
- 125000001424 substituent group Chemical group 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
Abstract
An electroless gold plating solution with which a gold plating film free of pitting corrosion at its surface can be obtained, which gold plating film when soldered realizes satisfactory soldering strength. In particular, an electroless gold plating solution characterized by containing a water soluble compound of gold and further containing as a reducing agent a hydroxyalkylsulfonic acid of the following general formula or salt thereof and an amine compound. (wherein R represents any of hydrogen, carboxyl, substituted or unsubstituted phenyl, naphthyl, saturated or unsaturated alkyl, acetyl, acetonyl, pyridyl and furyl; X represents any of hydrogen, Na, K and NH4; and n is an integer of 0 to 4.
Description
Technical field
The present invention relates to plating technology and chemical gold plating liquid.
Background technology
Chemical gilding is applicable to joint, the circuit surface of electronic industry parts such as the circuit, IC encapsulation, ito substrate, IC-card of printed circuit board.
Carrying out on the substrate chemical nickel plating tunicle under the situation of displaced type chemical gilding that thickness is 0.05～0.1 μ m, particularly after the plating reaction has just begun, nickel is very fast with the replacement(metathesis)reaction of gold, the grain circle part of the precipitation particles in the heavy attack chemical nickel plating tunicle optionally, the erosion of precipitation particles is deeply carried out, formation defect part below gold-plated tunicle.Along with the difference of situation, defect part or continuously or concentrate, even cause the bad order (pitting corrosion takes place on the surface) of gold-plated tunicle.And then though the thickness of the golden tunicle of separating out is very thin, smaller or equal to 0.1 μ m, but because the erosive degree of depth is very dark, the fragilityization of the chemical nickel plating tunicle that such displaced type gold plating liquid causes and with the cohesiveness deficiency of gold-plated tunicle, so when endurance test, peel off, when welding, can not guarantee enough welding strengths.In the chemical gold plating liquid of such prior art, owing to exist pitting corrosion, welding strength deficiency to produce inferior goods on gold-plated tunicle surface, this becomes big problem in ball grid array (BGA) N-type semiconductorN encapsulation etc.
Open in the 2001-107259 communique the spy,, disclose the chemical gold plating liquid that contains hypophosphite or hydrazine and directly lock the shape alkylamine as the displaced type chemical gold plating liquid.The purpose of this displaced type chemical gold plating liquid is to reduce the reduction that the cohesive strength (shearing resistance) coarse, the welding assembly that reduces solder sphere etc. of substrate nickel surface is caused by thermal history.
In addition, open in the flat 6-280039 communique the spy and to disclose, in the chemical plating bath that contains nitrogenous compounds such as water-soluble gold compound, complexing agent, reductive agent and amine, add nonionogenic tenside and/or nonionic polymkeric substance as stablizer, can prevent the generation of plating expansion as much as possible.
Summary of the invention
The object of the present invention is to provide a kind of chemical gold plating liquid, it can obtain the gold-plated tunicle that the surface does not have pitting corrosion, can guarantee enough welding strengths when welding.
The present inventor furthers investigate in order to solve above-mentioned problem, found that by making chemical gold plating liquid contain specific hydroxy alkyl sulfonic acid or its salt and containing amine compound, can obtain the gold-plated tunicle that the surface does not have pitting corrosion, thereby finish the present invention.That is, the present invention is as described below.
(1) a kind of chemical gold plating liquid is characterized in that, contains water-soluble gold compound, contains the hydroxy alkyl sulfonic acid shown in the following general formula or its salt as reductive agent and amine compound,
(in the following formula, R represents hydrogen, carboxyl, maybe in substituent phenyl, naphthyl, saturated or undersaturated alkyl, ethanoyl, acetonyl, pyridyl and the furyl any can be arranged, and X represents hydrogen, Na, K and NH
4In any, n is 0～4 integer).
(2) as above-mentioned (1) described chemical gold plating liquid, it is characterized in that, also contain the phosphoric acid based compound.
As above-mentioned (1) or (2) described chemical gold plating liquid, it is characterized in that (3) reductive agent shown in the above-mentioned general formula is sodium hydroxymethane sulfonate (HOCH
2SO
3Na).
As each described chemical gold plating liquid of above-mentioned (1)～(3), it is characterized in that (4) above-mentioned amine compound is Triethylenetetramine (TETA) (H
2N (CH
2)
2NH (CH
2)
2NH (CH
2)
2NH
2).
(5) a kind of ormolu is characterized in that, is to use the described chemical gold plating liquid of each of above-mentioned (1)～(4) to make.
Description of drawings
Fig. 1 is the SEM photo on the gold-plated tunicle surface of embodiment 1.
Fig. 2 is the SEM photo on the gold-plated tunicle surface of comparative example 1.
Fig. 3 is the SEM photo on the gold-plated tunicle surface of comparative example 2.
Embodiment
Below, chemical gold plating liquid of the present invention is elaborated.
Gold plating liquid of the present invention, the gold compound that becomes Jin Yuan is so long as water-soluble getting final product, and there is no particular limitation, and its maximum is characterised in that, contains specific hydroxy alkyl sulfonic acid or its salt and amine compound.
Therefore, gold plating liquid of the present invention is to be dissolved with water-soluble gold compound, specific hydroxy alkyl sulfonic acid or the material of its salt and amine compound in water solvent at least, as solvent, is preferably water.
As water-soluble gold compound, preferably use gold tricyanide, sulfurous acid gold, gold aurothiosulfate, thiocyanic acid gold, hydrochloro-auric acid or its salt, as sodium salt, sylvite, ammonium salt etc.These gold compounds in the chemical gold plating liquid of the present invention preferably contain 0.1～100g/L in the gold concentration in the plating solution, more preferably contain 0.5～20g/L.If gold concentration is less than 0.1g/L, then Jin replacing velocity is significantly slack-off, if surpass 100g/L, then effect is saturated, does not have advantage.
As reductive agent, use the hydroxy alkyl sulfonic acid shown in the following general formula or its salt.
(in the following formula, R represents hydrogen, carboxyl, maybe in substituent phenyl, naphthyl, saturated or undersaturated alkyl, ethanoyl, acetonyl, pyridyl and the furyl any can be arranged, and X represents hydrogen, Na, K and NH
4In any, n is 0～4 integer.)
In the following formula, the substituting group as the phenyl among the R, naphthyl, saturated or undersaturated alkyl, ethanoyl, acetonyl, pyridyl and furyl can list, halogen, alkoxyl group, nitro, hydroxyl, sulfonic group or its salt, phenyl, ethanoyl etc.As halogen, be preferably chlorine, as alkoxyl group, be preferably lower alkoxy, for example methoxyl group.In addition,, can list an alkali metal salt etc., be preferably sodium salt as sulfonic salt.
As saturated or undersaturated alkyl, be preferably carbonatoms and be 1～4 alkyl.
In addition, in the following formula, be preferably sodium as X.
As the hydroxy alkyl sulfonic acid shown in the above-mentioned general formula or the concrete example of its salt, can list following compound, preferably use the compound of No.1 and 2.
1 HO-CH
2-SO
3Na
2 HO-CH
2-CH
2-SO
3Na
Above-mentioned hydroxy alkyl sulfonic acid or its salt preferably contain 0.1～20g/L in plating solution, more preferably contain 0.5～10g/L.If amount is less than 0.1g/L, then golden speed of separating out is slack-off, in addition, if surpass 20g/L, then because causing the possibility that plating bath is decomposed improves, so not preferred.
As amine compound, can be the compound that primary amine and secondary amine are arranged in 1 molecules such as diethylenetriamine, Triethylenetetramine (TETA), tetren, penten; The monoamine compound of methylamine, ethamine, propylamine, butylamine, amylamine, hexylamine etc.; The diamine compound of methylene diamine, 1, propylene diamine, butylene diamine, pentamethylene diamine, hexanediamine etc.
In addition, can also list in above-claimed cpd further combined with the aromatic amine that aromatic nucleus such as phenyl ring is arranged, directly be combined with amino aromatic amines compounds such as aniline.In addition, in order to improve solvability, also can use the compound that in above-claimed cpd, is combined with hydroxyl, carboxyl, the contour polar substituent of sulfonic group, the compound that has formed salt such as hydrochloride to water.
Amine compound preferably contains 0.1～30g/L in plating solution, more preferably contain 0.5～20g/L.If amount is less than 0.1g/L, then the grain circle of nickel surface corrodes, and causes the bad order of gold-plated tunicle sometimes.In addition, if amount surpasses 30g/L, then because causing the possibility that plating bath is decomposed improves, so not preferred.
In addition, chemical gold plating liquid of the present invention as required, can add the phosphoric acid based compound as the pH buffer reagent.
As the phosphoric acid based compound, can list phosphoric acid, tetra-sodium or their an alkali metal salt, alkali earth metal salt, ammonium salt, biphosphate an alkali metal salt, biphosphate alkali earth metal salt, primary ammonium phosphate, phosphoric acid hydrogen two an alkali metal salts, phosphoric acid hydrogen two alkali earth metal salts, Secondary ammonium phosphate etc.The concentration of the phosphoric acid based compound in the plating solution is preferably 0.1～200g/L, more preferably 1～100g/L.
In addition, gold plating liquid of the present invention can also contain amino carboxylic acid compounds as complexing agent, as amino carboxylic acid compounds, can list ethylenediamine tetraacetic acid (EDTA) (EDTA), Oxyethylethylenediaminetriacetic acid, the dihydroxy ethyl ethylenediamine-N,N'-diacetic acid(EDDA), trimethylenedinitrilo-tertraacetic acid, diethylene triaminepentaacetic acid(DTPA), triethylenetetraaminehexaacetic acid, glycine, glycylglycine, the glycyl glycylglycine, dihydroxyethylglycin, iminodiethanoic acid, the hydroxyethyl iminodiethanoic acid, nitrilotriacetic acid(NTA), nitrilo three propionic acid, or its an alkali metal salt, alkali earth metal salt, ammonium salt etc.The concentration of the amino carboxylic acid compounds in the plating solution is preferably 0.1～200g/L, more preferably 1～100g/L.If the concentration of amino carboxylic acid compounds is less than 0.1g/L, then as the effect deficiency of complexing agent, even surpass 200g/L, effect is saturated, does not have advantage.
In gold plating liquid of the present invention, can also add the cyaniding compound that is used to make gold complex stabilization, the potassium cyanide that improves plating bath stability, sodium cyanide etc.If the addition of cyaniding compound is too much, then corrode the substrate nickel flashing, be easy to take place pitting corrosion, therefore, preferably in the scope of 0.01～5g/L, add.
And then as reaction promotor, interpolation thallium compound, lead compound also are effective.As their addition,, be preferably 0.01～50mg/L in metal.If the addition of reaction promotor is too much, then cause the plating bath decomposition.
From the speed of separating out of gold, the outward appearance of plated film and the viewpoint of plating bath stability, the pH value of gold plating liquid of the present invention is preferably 5～9, and preferred especially 6～8.
For the adjustment of pH, can use the acidic cpd of the basic cpd, sulfuric acid, phosphoric acid etc. of potassium hydroxide, sodium hydroxide, ammonia etc.
In addition, from the stability of plating bath and the viewpoint of the speed of separating out of gold, gold plating liquid of the present invention is 60～90 ℃ of uses in the plating bath temperature preferably.
When using gold plating liquid of the present invention to carry out plating, with being immersed in the plating bath of printed circuit board etc. by plating material.Be preferably substrate by plating material and carried out materials afterwards such as nickel plating, if use gold plating liquid of the present invention to carry out plating, then cannot see pitting corrosion on the surface of the gold-plated tunicle that obtains, good with the cohesiveness of substrate nickel plating tunicle, when welding, can guarantee enough welding strengths.
Embodiment
With embodiment as follows and comparative example, the preferred embodiment of the present invention is described.
Embodiment 1～2 and comparative example 1～2
The gold-plated bath of liquid that shown in the modulometer 1 each formed.As by plating material, use the copper facing printed circuit board, operation of carrying out till chemical gilding as follows is carried out chemical gilding with the condition of table 1 record.
Acid degreasing process (day ore deposit メ Le プ レ one テ イ Application グ system KG-512) 45 ℃, 5 minutes
→ hot wash 50～60 ℃, 1 minute
→ washing
→ soft etching (Sodium Persulfate 80g/L, sulfuric acid 20ml/L)
→ washing
→ acid elution (sulfuric acid 30ml/L)
→ washing
25 ℃ of → activation (day ore deposit メ Le プ レ one テ イ Application グ system KG-522), 3 minutes
→ washing
→ acid dipping (sulfuric acid 30ml/L)
→ washing
85 ℃ of → chemical nickel platings (day ore deposit メ Le プ レ one テ イ Application グ system KG-530), 3 minutes
→ washing
→ chemical gilding
The plated film that obtains is carried out following evaluation.Amplify 3000 times of observations with SEM and have or not pitting corrosion.Fig. 1～3 show the SEM photo of the gold-plated tunicle of embodiment 1 and comparative example 1～2 respectively.Form with stain in the photo is observed pitting corrosion.Do not see that on the gold-plated tunicle of embodiment 1 this stain is pitting corrosion, but in the gold-plated tunicle of comparative example 1 and 2, seen pitting corrosion.In addition, the gold-plated tunicle of embodiment 2 is not seen pitting corrosion similarly to Example 1 yet.
In addition, after carrying out 20 minutes plating, use セ イ コ one electronic industry (strain) system fluorescent X-ray film thickness meter SFT-3200, measure coating film thickness, obtain speed of separating out.
Evaluation result is as shown in table 1.
Table 1
The composition of chemical gold plating liquid and characteristic thereof
| Embodiment 1 | Embodiment 2 | Comparative example 1 | Comparative example 2 | |
| Pitting corrosion | ○ | ○ | × | △ |
| Speed of separating out (μ m/20min) | 0.12 | 0.10 | 0.081 | 0.055 |
| Potassium auric cyanide (g/L) | 2 | 2 | 2 | 2 |
| EDTA(g/L) | 10 | 10 | 0 | 10 |
| Triethylenetetramine (TETA) (g/L) | 10 | 10 | 0 | 10 |
| SODIUM PHOSPHATE, MONOBASIC 2 hydrates (g/L) | 34 | 34 | 34 | 34 |
| Sodium hydroxymethane sulfonate (g/L) | 2 | - | 2 | 0 |
| Ethylenehydrinsulfonic acid sodium (g/L) | - | 2 | - | - |
| pH | 7.0 | 7.0 | 7.0 | 7.0 |
| The plating bath temperature (℃) | 88 | 88 | 88 | 88 |
Adjust pH with potassium hydroxide
Below, to the plated film that obtains in embodiment 1 and the comparative example 1, weld the test of cohesive strength.
The welding cohesive strength, use Pb/Sn=37/63,0.4mm φ (SPARKLE BALLS thousand lives metal system) as solder sphere, use RMA type (NH-100VK-1 ア サ ヒ chemical research is made) as solder flux, the following heating-type that carries out collides tension test (heat bump pull test).Test is carried out 12 times, and table 2 illustrates maximum value, minimum value and the mean value of wherein having removed outlier.
Metering equipment: adhesion test machine 4000 series (デ イ ヅ society system)
Heating condition: 270 ℃ of design temperatures
5 seconds heat-up times
Cooling finishes 50 ℃
300 μ m/ seconds of trial speed
Reflow ovens: far infrared rays formula counter-current welding equipment (RF-330 Japan パ Le ス technical study is made)
Reflux conditions: 230 ℃ of peak temperatures
Table 2
| Embodiment 1 | Comparative example 1 | |
| Maximum value | 1462 | 1377 |
| Minimum value | 1181 | 976 |
| Mean value | 1321 | 1185 |
Unit: gf
As shown in Table 2, the welding cohesive strength of the tunicle that obtains among the embodiment 1 is higher than the welding cohesive strength of the tunicle that comparative example 1 obtains.Can think that this is that nickel is few to the diffusion of Gold plated Layer because the tunicle of embodiment 1 does not have pitting corrosion, nickel surface is difficult to form the high layer of phosphorus containing ratio, or owing to there is not pitting corrosion, nickel surface is difficult to oxidation, has improved the welding cohesive strength.
The industry utilizability
If use chemical gold plating liquid of the present invention, then can obtain the gold-plated tunicle that the surface does not have pitting corrosion. And then, if chemical gold plating liquid of the present invention is used for joint and the circuit surface of the electronics industry parts such as circuit, IC encapsulation, ito substrate, IC-card of printed circuit board, then can improve the caking property with the chemical nickel plating tunicle of substrate, when welding, can guarantee enough weld strengths.
Claims (5)
1. a chemical gold plating liquid is characterized in that, contains water-soluble gold compound, contains the hydroxy alkyl sulfonic acid shown in the following general formula or its salt as reductive agent and contain amine compound,
(in the following formula, R represents hydrogen, carboxyl, maybe in substituent phenyl, naphthyl, saturated or undersaturated alkyl, ethanoyl, acetonyl, pyridyl and the furyl any can be arranged, and X represents hydrogen, Na, K and NH
4In any, n is 0～4 integer).
2. chemical gold plating liquid as claimed in claim 1 is characterized in that, also contains the phosphoric acid based compound.
3. chemical gold plating liquid as claimed in claim 1 or 2 is characterized in that, the reductive agent shown in the above-mentioned general formula is sodium hydroxymethane sulfonate (HOCH
2SO
3Na).
4. as each described chemical gold plating liquid of claim 1～3, it is characterized in that above-mentioned amine compound is Triethylenetetramine (TETA) (H
2N (CH
2)
2NH (CH
2)
2NH (CH
2)
2NH
2).
5. an ormolu is characterized in that, is to use the described chemical gold plating liquid of each of claim 1～4 to make.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP164807/2003 | 2003-06-10 | ||
| JP2003164807 | 2003-06-10 | ||
| JP2003416315 | 2003-12-15 | ||
| JP416315/2003 | 2003-12-15 | ||
| PCT/JP2004/004656 WO2004111287A2 (en) | 2003-06-10 | 2004-03-31 | Electroless gold plating solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1802452A true CN1802452A (en) | 2006-07-12 |
| CN100510174C CN100510174C (en) | 2009-07-08 |
Family
ID=33554380
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004800160274A Expired - Lifetime CN100510174C (en) | 2003-06-10 | 2004-03-31 | Electroless gold plating solution |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JP4638818B2 (en) |
| KR (1) | KR100749992B1 (en) |
| CN (1) | CN100510174C (en) |
| HK (1) | HK1090096A1 (en) |
| TW (1) | TWI284157B (en) |
| WO (1) | WO2004111287A2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101275224B (en) * | 2007-01-11 | 2011-05-18 | 上村工业株式会社 | Method for maintaining plating capacity in electroless gold plating bath |
| CN101319318B (en) * | 2006-12-06 | 2012-02-22 | 上村工业株式会社 | Electroless gold plating bath, electroless gold plating method and electronic parts |
| US8124174B2 (en) | 2007-04-16 | 2012-02-28 | C. Uyemura & Co., Ltd. | Electroless gold plating method and electronic parts |
| CN101319319B (en) * | 2006-12-06 | 2012-04-25 | 上村工业株式会社 | Electroless gold plating bath, electroless gold plating method and electronic parts |
| CN105543816A (en) * | 2016-02-01 | 2016-05-04 | 哈尔滨工业大学（威海） | Chemical gold plating solution |
| TWI707060B (en) * | 2015-04-30 | 2020-10-11 | 日商日本高純度化學股份有限公司 | Electroless gold plating solution, aldehyde-amine adduct replenishing solution and gold film formed by using them |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005098088A1 (en) * | 2004-04-05 | 2005-10-20 | Nippon Mining & Metals Co., Ltd. | Electroless gold plating liquid |
| JP4831710B1 (en) | 2010-07-20 | 2011-12-07 | 日本エレクトロプレイテイング・エンジニヤース株式会社 | Electroless gold plating solution and electroless gold plating method |
| JP6329589B2 (en) * | 2016-06-13 | 2018-05-23 | 上村工業株式会社 | Film formation method |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2667323B2 (en) * | 1991-04-01 | 1997-10-27 | 川崎製鉄株式会社 | Antioxidant, auxiliary for plating bath and plating bath using the same |
| JP3920462B2 (en) * | 1998-07-13 | 2007-05-30 | 株式会社大和化成研究所 | Aqueous solutions for obtaining noble metals by chemical reduction deposition |
| US6383269B1 (en) * | 1999-01-27 | 2002-05-07 | Shipley Company, L.L.C. | Electroless gold plating solution and process |
| JP4932094B2 (en) * | 2001-07-02 | 2012-05-16 | 日本リーロナール有限会社 | Electroless gold plating solution and electroless gold plating method |
| JP3697181B2 (en) * | 2001-07-27 | 2005-09-21 | 日本高純度化学株式会社 | Electroless gold plating solution |
-
2004
- 2004-03-31 CN CNB2004800160274A patent/CN100510174C/en not_active Expired - Lifetime
- 2004-03-31 JP JP2005506873A patent/JP4638818B2/en not_active Expired - Lifetime
- 2004-03-31 WO PCT/JP2004/004656 patent/WO2004111287A2/en active Application Filing
- 2004-03-31 KR KR1020057023540A patent/KR100749992B1/en active IP Right Grant
- 2004-04-08 TW TW093109714A patent/TWI284157B/en active
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319318B (en) * | 2006-12-06 | 2012-02-22 | 上村工业株式会社 | Electroless gold plating bath, electroless gold plating method and electronic parts |
| CN101319319B (en) * | 2006-12-06 | 2012-04-25 | 上村工业株式会社 | Electroless gold plating bath, electroless gold plating method and electronic parts |
| CN101275224B (en) * | 2007-01-11 | 2011-05-18 | 上村工业株式会社 | Method for maintaining plating capacity in electroless gold plating bath |
| US8124174B2 (en) | 2007-04-16 | 2012-02-28 | C. Uyemura & Co., Ltd. | Electroless gold plating method and electronic parts |
| CN101469420B (en) * | 2007-04-16 | 2012-10-03 | 上村工业株式会社 | Electroless gold-plating method and electronic component |
| TWI707060B (en) * | 2015-04-30 | 2020-10-11 | 日商日本高純度化學股份有限公司 | Electroless gold plating solution, aldehyde-amine adduct replenishing solution and gold film formed by using them |
| CN105543816A (en) * | 2016-02-01 | 2016-05-04 | 哈尔滨工业大学（威海） | Chemical gold plating solution |
Also Published As
| Publication number | Publication date |
|---|---|
| TWI284157B (en) | 2007-07-21 |
| CN100510174C (en) | 2009-07-08 |
| WO2004111287A3 (en) | 2005-03-03 |
| HK1090096A1 (en) | 2006-12-15 |
| JP4638818B2 (en) | 2011-02-23 |
| KR100749992B1 (en) | 2007-08-16 |
| JPWO2004111287A1 (en) | 2006-07-20 |
| TW200500496A (en) | 2005-01-01 |
| WO2004111287A2 (en) | 2004-12-23 |
| KR20060031617A (en) | 2006-04-12 |
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