CN102534576A - 化学镀催化剂和方法 - Google Patents
化学镀催化剂和方法 Download PDFInfo
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- CN102534576A CN102534576A CN2011104625357A CN201110462535A CN102534576A CN 102534576 A CN102534576 A CN 102534576A CN 2011104625357 A CN2011104625357 A CN 2011104625357A CN 201110462535 A CN201110462535 A CN 201110462535A CN 102534576 A CN102534576 A CN 102534576A
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- Prior art keywords
- alkyl
- compsn
- metal
- water
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000003054 catalyst Substances 0.000 title abstract description 32
- 238000007747 plating Methods 0.000 title description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 65
- 239000002184 metal Substances 0.000 claims abstract description 65
- 239000000203 mixture Substances 0.000 claims abstract description 50
- 239000000758 substrate Substances 0.000 claims abstract description 43
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical class [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 239000003795 chemical substances by application Substances 0.000 claims description 29
- 229910052763 palladium Inorganic materials 0.000 claims description 29
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical class [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 26
- 150000001875 compounds Chemical class 0.000 claims description 26
- 239000010949 copper Chemical class 0.000 claims description 26
- 229910052802 copper Inorganic materials 0.000 claims description 25
- 125000004169 (C1-C6) alkyl group Chemical group 0.000 claims description 21
- 239000003381 stabilizer Substances 0.000 claims description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical class [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 18
- 230000002829 reductive effect Effects 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 15
- 230000008021 deposition Effects 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical class [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 10
- 238000007772 electroless plating Methods 0.000 claims description 10
- 229910052709 silver Inorganic materials 0.000 claims description 10
- 239000004332 silver Chemical class 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical class [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 239000010931 gold Chemical class 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Chemical class 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical class [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical class [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 229910052707 ruthenium Chemical class 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 238000001465 metallisation Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 27
- -1 metals ion Chemical class 0.000 description 23
- 238000000151 deposition Methods 0.000 description 14
- 229920005989 resin Polymers 0.000 description 13
- 239000011347 resin Substances 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 229910052718 tin Inorganic materials 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 239000003822 epoxy resin Substances 0.000 description 11
- 229920000647 polyepoxide Polymers 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 239000002253 acid Substances 0.000 description 9
- 239000012776 electronic material Substances 0.000 description 9
- 239000008399 tap water Substances 0.000 description 9
- 235000020679 tap water Nutrition 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000013543 active substance Substances 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 8
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 239000000084 colloidal system Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 230000009467 reduction Effects 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000002585 base Substances 0.000 description 6
- 229910000085 borane Inorganic materials 0.000 description 6
- 239000000872 buffer Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- UORVGPXVDQYIDP-UHFFFAOYSA-N trihydridoboron Substances B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 6
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 description 5
- 125000000217 alkyl group Chemical group 0.000 description 5
- 150000002148 esters Chemical class 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000004417 polycarbonate Substances 0.000 description 5
- 229920000515 polycarbonate Polymers 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000013112 stability test Methods 0.000 description 5
- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical compound [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 description 5
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical group CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 4
- 241000282326 Felis catus Species 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000002191 fatty alcohols Chemical class 0.000 description 4
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 4
- LOIYMIARKYCTBW-OWOJBTEDSA-N trans-urocanic acid Chemical compound OC(=O)\C=C\C1=CNC=N1 LOIYMIARKYCTBW-OWOJBTEDSA-N 0.000 description 4
- LOIYMIARKYCTBW-UHFFFAOYSA-N trans-urocanic acid Natural products OC(=O)C=CC1=CNC=N1 LOIYMIARKYCTBW-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 150000001408 amides Chemical class 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 150000002460 imidazoles Chemical class 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002082 metal nanoparticle Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 230000003472 neutralizing effect Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229920002492 poly(sulfone) Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000012286 potassium permanganate Substances 0.000 description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- KGYLMXMMQNTWEM-UHFFFAOYSA-J tetrachloropalladium Chemical compound Cl[Pd](Cl)(Cl)Cl KGYLMXMMQNTWEM-UHFFFAOYSA-J 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- WLDPWZQYAVZTTP-UHFFFAOYSA-N 1-methyl-imidazole-2-carboxylic acid Chemical compound CN1C=CN=C1C(O)=O WLDPWZQYAVZTTP-UHFFFAOYSA-N 0.000 description 2
- NKWCGTOZTHZDHB-UHFFFAOYSA-N 1h-imidazol-1-ium-4-carboxylate Chemical compound OC(=O)C1=CNC=N1 NKWCGTOZTHZDHB-UHFFFAOYSA-N 0.000 description 2
- 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 2
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N 4-methylimidazole Chemical compound CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 2
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 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 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
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 229920013701 VORANOL™ Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 2
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 2
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 229960003237 betaine Drugs 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000010974 bronze Substances 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 2
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 2
- 229920001643 poly(ether ketone) Polymers 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920006380 polyphenylene oxide Polymers 0.000 description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 125000002769 thiazolinyl group Chemical group 0.000 description 2
- SYRHIZPPCHMRIT-UHFFFAOYSA-N tin(4+) Chemical compound [Sn+4] SYRHIZPPCHMRIT-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- XEJCDBUNISUVGZ-XRIGFGBMSA-N (2s)-2-amino-3-(1h-imidazol-5-yl)propanoic acid;dihydrochloride Chemical compound Cl.Cl.OC(=O)[C@@H](N)CC1=CN=CN1 XEJCDBUNISUVGZ-XRIGFGBMSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- 0 *c1c(*)nc(*)[n]1 Chemical compound *c1c(*)nc(*)[n]1 0.000 description 1
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- MXHKJQTYOAFPBY-UHFFFAOYSA-N 2-(2,3-dihydroxypropoxycarbonyl)benzoic acid Chemical compound OCC(O)COC(=O)C1=CC=CC=C1C(O)=O MXHKJQTYOAFPBY-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 1
- DKRXGTYXXJTMFZ-UHFFFAOYSA-N 2-ethyl-5-methyl-1h-imidazole-4-carboxylic acid Chemical class CCC1=NC(C)=C(C(O)=O)N1 DKRXGTYXXJTMFZ-UHFFFAOYSA-N 0.000 description 1
- CBECDWUDYQOTSW-UHFFFAOYSA-N 2-ethylbut-3-enal Chemical compound CCC(C=C)C=O CBECDWUDYQOTSW-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 101710134784 Agnoprotein Proteins 0.000 description 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- AUHKILPQYJJRTM-UHFFFAOYSA-N CC(N(C)C)C(=O)O.C(C)(=O)ON(C)C Chemical compound CC(N(C)C)C(=O)O.C(C)(=O)ON(C)C AUHKILPQYJJRTM-UHFFFAOYSA-N 0.000 description 1
- IOSRHVXYRKGYRQ-UHFFFAOYSA-N CC(N(C)C)C(=O)O.N1=CC=CC2=CC=CC=C12.CC=1NC=CN1 Chemical compound CC(N(C)C)C(=O)O.N1=CC=CC2=CC=CC=C12.CC=1NC=CN1 IOSRHVXYRKGYRQ-UHFFFAOYSA-N 0.000 description 1
- PMINQPJGHPSAPR-UHFFFAOYSA-N CCC(C[N+]1(CC)C([O-])=O)N=C1OC Chemical compound CCC(C[N+]1(CC)C([O-])=O)N=C1OC PMINQPJGHPSAPR-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
-
- 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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
-
- 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
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Abstract
本发明提供了稳定的零价金属组合物以及制备和使用该组合物的方法。该组合物适用于作为非导电基底的金属化催化剂,特别适用于电子器件制造。
Description
技术领域
本发明总体上涉及金属化学镀领域。更特别地,涉及电子器件制造用的非导电基底的金属化学镀催化剂。
背景技术
印刷电路板包括层状非导电绝缘基底,这些基底通过钻通孔或镀通孔实现电路板相对两侧或板相邻两层之间的连接。金属化学镀是一种在表面上制备金属镀膜的熟知工艺。绝缘表面的金属化学镀需要先沉积上一种催化剂。通常用于催化或催化层状非导电绝缘基底的方法是,在化学镀之前,使用酸性氯化物介质中的锡-钯水溶胶处理基底。胶体包括一个被锡(II)离子络合物的稳定层,例如SnCl3 -所包围的金属钯核,目的是作为表面稳定组分来阻止悬浮液中的胶体凝聚。
在催化过程中,钯基胶体吸附到绝缘基底表面上,例如环氧树脂或聚酰亚胺以催化金属化学镀,例如化学镀铜。虽然不希望受到理论限制,但人们通常认为在镀液中催化剂颗粒扮演了从还原剂向金属离子传输电子的载体角色。尽管化学镀的性能受到许多因素的影响,例如镀液配方和配体选择,但是催化步骤仍然是控制化学镀速率和机理的关键因素。
尽管锡/钯胶体催化剂作为金属尤其是铜的化学镀催化剂已经在商业上使用几十年了,其具有很多缺点,例如对空气敏感,价格高昂。伴随着电子器件尺寸缩小和性能提升,电路的封装密度越来越高,工业质量标准也随之提高。由于对可靠性的要求越来越高,特别是由于钯的价格过高且不稳定,寻找其它的催化剂组合物或者采用较便宜金属或者减少甚至淘汰使用先前金属的组合物尤为必要。另外,锡-钯胶体催化剂的稳定性也让人担忧。反离子可以阻止钯的凝聚,但是锡(II)离子很容易氧化成锡(IV),因此胶体不可能始终保持胶体结构。温度升高,搅拌加快,可以促进氧化。如果锡(II)含量降至接近于零,钯颗粒尺寸增加,团聚,沉降,化学镀停止。
人们花费了大量努力去寻找新的更好的化学镀催化剂。例如,由于钯价格高昂,一些人开始转向发展非贵金属催化剂,特别是胶体铜催化剂。另外,由于使用氯化锡还原钯成本较高并且氧化的锡需要单独的加速步骤,有一些人转去发展无锡的钯催化剂。然而,这些催化剂活性和可靠性不够,难以满足穿孔电镀要求。而且,这些催化剂稳定性不够,放置后一般活性逐渐降低,活性改变使这些催化剂在商业上使用不可靠和不实际。
人们研究了锡之外的钯离子稳定成分。例如,美国专利4,248,632公开了一些作为金属离子催化剂,例如钯离子(Pd2+),的稳定剂的吡啶和咪唑配体的稳定剂。金属离子只有吸附到非导电基底后才被还原。其它已知的稳定成分包括聚乙烯基吡咯烷酮(PVP)和其它聚合物。PVP充当了保护剂和稳定剂的角色。根据报道,金属-配体成分中的配体在将钯(II)催化剂固定到基底的过程中起到了积极作用。另外,其它使用钯离子的金属胶体,例如银/钯和铜/钯,也有报道。尽管人们已经开发了许多常规的锡/钯催化剂的替代催化剂,但这些催化剂仍然使用钯离子而且无一能够满足电子器件例如印刷电路板制造所必需的稳定性,活性和绝缘表面吸附性能。
发明内容
本发明提供了一种组合物,包括0.5至100ppm的零价金属,稳定剂化合物和水;其中的零价金属选自钯银,钴,镍,金,铜和钌;其中的稳定剂化合物具有化学式
其中R=H或(C1-C6)烷基;R1各自独立地选自H,(C1-C6)烷基和Z;Z=(C2-C6)烯基-Z1或(CR2R3)aZ1;R2和R3各自独立地选自H,羟基,(C1-C6)烷基,羟基(C1-C6)烷基,C(O)-(C1-C6)烷基,(C1-C6)烷基-C(O)-(C1-C6)烷基,CO2R4和NR5R6;R4=H,(C1-C6)烷基,羟基(C1-C6)烷基或(C1-C4)烷氧基(C1-C6)烷基;R5和R6各自独立地选自H,(C1-C6)烷基和(CR2R3)aZ2;Z1=C(S)SH,CO2H,或C(O)NR5R6;Z2=C(O)R4或CO2R4;和a=0-6;其中至少一个R1是Z。
本发明还提供了一种制备上述组合物的方法,包括将稳定剂化合物,水和水溶性金属盐混合,然后加入足量的还原剂,形成零价金属。
本发明还提供了一种方法,包括:(a)提供具有多个通孔的基底;(b)将权利要求1的组合物施加到通孔表面上;和然后(c)通过化学金属镀将金属化学镀到通孔表面上。
具体实施方式
除非另有说明,说明书使用的下列缩写代表下述含义:约=大约;℃=摄氏度;g=克;mg=毫克;L=升;mL=毫升;ppm=百万分之一份;μm=micron=微米;nm=纳米;mm=毫米;DI=去离子;Tg=玻璃化转变温度;R.T.=室温;和rpm=每分钟转数。除非另有说明,所有数量为重量百分比(重量%),所有比值为摩尔比。所有的数值范围都包括端值且可以以任意的顺序组合,除非这些数值范围明显地限制为加合=100%。
术语“通孔”包括盲孔。另外,说明书中使用的术语“电镀”指的是金属化学镀,除非另有说明。“沉积”和“电镀”在本说明书可以互换。术语“烷基”包括直链的,支链的和环状烷基。同样地,术语“烯基”包括直链的,支链的和环状烯基。“卤素”包括氟,氯,溴和碘。术语“印刷电路板”和“印刷线路板”在说明书中可以互换。冠词“a”和“an”表示单数和复数。
本发明的组合物包括零价金属,稳定剂化合物和水。优选零价金属和稳定剂化合物以稳定纳米颗粒的形式出现在组合物中。更优选本发明组合物是包括含有零价金属和稳定剂化合物的稳定纳米颗粒的溶液。
本发明组合物中使用的水可以是任何形式,例如自来水和去离子水。合适的零价金属是那些在金属化学镀中可作为催化剂使用的金属,例如但不限于,钯,银,钴,镍,金,铜和钌。优选零价金属选自钯,银,钴,镍,铜和钌,以及更优选钯,银,铜,钴和镍;更优选是钯和银。零价金属的混合物也可以使用,例如钯和银的混合物或钯和铜的混合物。基于组合物的重量计,零价金属在组合物中的含量为0.5至100ppm。优选地,零价金属在组合物中的含量为1至100ppm;更优选为1至75ppm;更加优选是5至75ppm;进一步更优选地是5-50ppm;最优选地为5-35ppm。
合适的零价金属的稳定剂化合物选自下列化学式的化合物
其中R=H或(C1-C6)烷基;R1各自独立地选自H,(C1-C6)烷基和Z;Z=(C2-C6)烯基-Z1或(CR2R3)aZ1;R2和R3各自独立地选自H,羟基,(C1-C6)烷基,羟基(C1-C6)烷基,C(O)-(C1-C6)烷基,(C1-C6)烷基-C(O)-(C1-C6)烷基,CO2R4和NR5R6;R4=H,(C1-C6)烷基,羟基(C1-C6)烷基或(C1-C4)烷氧基(C1-C6)烷基;R5和R6各自独立地选自H,(C1-C6)烷基和(CR2R3)aZ2;Z1=C(S)SH,CO2H,或C(O)NR5R6;Z2=C(O)R4或CO2R4;和a=0-6;其中至少一个R1是Z。优选地,R=H或(C1-C3)烷基。优选地,每个R1各自独立地选自H,(C1-C3)烷基和Z,和更优选为H和Z。Z优选是(C2-C4)烯基-Z1或(CR2R3)aZ1。Z1优选是CO2H,或C(O)NR5R6。优选地,R2和R3各自独立地选自H,(C1-C3)烷基,CO2R4和NR5R6。R4优选是H或(C1-C3)烷基,更优选是H或CH3,进一步更优选是H。优选R5和R6各自独立地选自H,(C1-C3)烷基和(CR2R3)aZ2,更优选H,CH3和(CR2R3)aZ2,进一步更优选H。Z2优选是CO2R4;更优选是CO2H。优选a=0-4,更优选是a=1-4,进一步更优选是a=1-3。稳定剂化合物通常可通过商业途径获得,例如购自西格玛-阿尔德里奇公司(Sigma-Aldrich)(美国密苏里州圣路易斯市),或者可以通过现有已知方法制备。这些化合物可以直接使用或者进一步纯化。
特别合适的稳定剂化合物包括,但不限于:组氨酸(4-(2-氨基-2-羧乙基)咪唑);尿刊酸(4-咪唑丙烯酸);4,5-咪唑二羧酸;4-咪唑醋酸;4-咪唑羧酸;1-甲基-2-咪唑羧酸;4,5-咪唑二羧酸二胺;1H-咪唑-4-甲酰胺;和4-咪唑丙烯酰胺。优选的稳定剂包括:组氨酸;尿刊酸;4,5-咪唑二羧酸;4-咪唑醋酸;4-咪唑羧酸;和1-甲基-2-咪唑羧酸。
本发明组合物包含的零价金属和稳定剂化合物的摩尔比为1∶1至1∶20。优选地,零价金属和稳定剂化合物的摩尔比为1∶5至1∶20,更优选从1∶10至1∶20。。
任选地,本发明组合物可以包含一种或多种不同的在化学镀催化组合物中通常使用的添加剂,例如,表面活性剂,缓冲剂,pH调节剂,助溶剂例如有机溶剂。不同添加剂的混合物也可以使用,例如pH调节剂和缓冲剂。任意合适的表面活性都可以使用,包括阴离子的,非离子的,阳离子的和两性的表面活性剂。基于组合物的重量计,表面活性剂的含量为0至25ppm。使用时,优选表面活性剂的含量为0.5至25ppm和更优选从1至10ppm。可以使用的缓冲剂包括,但不限于,羧酸,例如柠檬酸,酒石酸,琥珀酸,苹果酸,丙二酸,马来酸,乳酸,醋酸和它们的盐;胺和它们的盐;氨基酸和它们的盐;和无机酸,例如硼酸,和它们的盐;无机碱例如碳酸氢钠。用于调节pH值的化合物可以包括,但不限于,碱金属氢氧化物,例如氢氧化钠和氢氧化钾,和酸例如无机酸。使用时,可选的缓冲剂和pH调节剂加入足够量以调节pH值到需要的范围。
一般来说,本发明组合物的pH值为6-14。优选地,本发明组合物是碱性的,就是说具有从>7至14的pH值,更优选具有从7.5至14的pH值,更加优选为7.5至10,进一步更优选为8至10。
本发明的组合物是纳米颗粒的稳定水溶液,可以用于催化电子元件制造中的金属化学镀。使用“稳定”意味着在20℃下储存3个月肉眼观察无沉淀析出。优选本发明组合物在20℃下储存6个月后,更优选是1年之后无沉淀现象。这些纳米颗粒具有不同的颗粒尺寸,如果颗粒尺寸太大,组合物可能不稳定,也就是说,会产生沉淀。合适的平均颗粒尺寸可以是从1nm至1μm,优选从1nm至500nm,更优选从1nm至100nm。颗粒尺寸可以通过已知技术测定,例如光散射或透射电子显微镜。
本发明的组合物可以通过将稳定剂化合物,水和水溶性金属盐和还原剂混合制备得到。优选地,稳定剂化合物,水和水溶性金属盐先混合,然后加入还原剂。还原剂用量可以是足以形成需要的零价金属的任意量。稳定剂化合物,水和水溶性金属盐可以任意顺序加入。一般来说,水溶性盐溶解在一定量水中。然后盐溶液加入到稳定剂水溶液中。随后搅拌混合物,通常在室温(约20℃)下,必要时可以调整pH值。通常搅拌棒的搅拌用于小体积,例如最高200mL。均化器则用于较大体积。通常的搅拌速度可以从3000至25000rpm。使用装置例如费舍尔科技有限公司(Fisher Scientific,Inc.)的POWERGENTM700均化器。随后,将还原剂加入到混合物中并继续搅拌。钯作为零价金属时,催化剂溶液在还原后颜色通常为灰色到黑色。还原后,我们认为形成了包含稳定剂和零价金属的稳定纳米颗粒。
只要水溶性良好,不同种类的金属盐都可以使用。合适的金属盐包括金属卤化物,金属硝酸盐,金属亚硝酸盐,金属氧化物,金属醋酸盐,金属葡萄糖酸盐,金属氟硼酸盐,金属烷基磺酸盐,金属硫酸盐,金属亚硫酸盐,金属硫代硫酸盐,金属硫氰酸盐和金属氰化物。典型的金属盐包括但不限于,氯化钯,四氯钯酸钠(palladium sodium chloride),四氯钯酸钾(palladiumpotassium chloride),四氯钯酸铵(palladium ammonium chloride),硫酸钯,硝酸钯,醋酸钯,氧化钯,硝酸银,氧化银,醋酸钴,氯化钴,硝酸钴,硫酸钴,硫酸镍,甲磺酸镍,醋酸镍,氟硼酸镍,氯化金,氰化金钾,亚硫酸金,硫代硫酸金,硫氰酸金,硫酸铜,葡萄糖酸铜,醋酸铜,硝酸铜,氯化钌,钌卟啉和氧化钌。金属盐用量可以随着水溶性变化而变化。例如,钯盐用量可以为5mg/L至10g/L,优选从100mg/L至5g/L。
各种各样的还原剂都可以用来形成本发明组合物。合适的还原剂包括但不限于,化合物例如硼氢化合物,例如氨硼烷,例如二甲基氨硼烷(DMAB),三甲基氨硼烷,异丙基氨硼烷和吗啉硼烷,硼氢化钠和硼氢化钾,次磷酸,及其铵盐,锂盐,钠盐,钾盐和钙盐,甲醛,次磷酸盐,例如次磷酸钠,无水肼(hydrazineanhydride),羧酸,例如甲酸和抗坏血酸,和还原糖类,例如葡萄糖,半乳糖,麦芽糖,乳糖,木糖和果糖,还原剂的用量决定于组合物中金属盐用量。通常来说,还原剂用量可以为5mg/L至500mg/L,优选用量为20mg/L至200mg/L。
由于上述催化剂组合物包含零价金属,例如Pd0。使用这些组合物的方法可以避免在金属化学镀之前的还原步骤。另外,这些组合物使金属较好地吸附到基底上。组合物是无锡的,由此避免了由锡(II)离子容易氧化至锡(IV)和破坏催化剂带来的种种问题。同时钯离子颗粒尺寸增加,团聚和沉降的问题也显著降低,甚至同时得到避免。由于锡不包含在组合物中,高昂的氯化锡不再需要,催化剂组合物的成本得到降低。进一步地,制备金属化基底时避免了使用锡时所需要的加速步骤,因此在制备金属化的非导电基底时减少了一个常规步骤。
本发明的组合物可以用作基底金属化学镀的催化剂,这些基底包括无机和有机材料,例如玻璃,陶瓷,瓷器,树脂,纸,织物和它们的组合。基底也包括金属包层和非包层材料,例如印刷电路板。这些印刷电路板包括使用热固性树脂,热塑性树脂和及其组合的金属包层和非包层基底,并且可以进一步包括纤维,例如玻璃纤维,和上面所述的实施材料。基底金属化各方法步骤的温度和时间均是常规的并且在现有技术中熟知的。
热塑性树脂包括但不限于,缩醛树脂,丙烯酸树脂例如丙烯酸甲酯,甲基丙烯酸甲酯,丙烯酸乙酯,甲基丙烯酸乙酯,丙烯酸丁酯和含有任意上述聚合物的共聚物;纤维素树脂例如纤维素丙酸酯,醋酸丁酸纤维素和硝酸纤维素;聚醚,尼龙,聚乙烯;聚苯乙烯;苯乙烯共混物例如丙烯腈苯乙烯、和共聚物以及丙烯腈-丁二烯-苯乙烯共聚物;聚碳酸酯;聚氯三氟乙烯;和乙烯基聚合物和共聚物例如醋酸乙烯酯,乙烯醇,乙烯基丁缩醛、氯乙烯,氯乙烯-醋酸共聚物,偏二氯乙烯和乙烯基甲醛。
热固性树脂包括但不限于,苯二甲酸烯丙酯,呋喃,三聚氰胺-甲醛,苯酚-甲醛和苯酚-糠醛共聚物,单独或者与丁二烯-丙烯腈共聚物或丙烯腈-丁二烯-苯乙烯共聚物复合,聚丙烯酸酯,聚硅氧烷,脲-甲醛,环氧树脂,烯丙基树脂,苯二甲酸甘油酯和聚醚。
本发明组合物可以催化低和高Tg的树脂。低Tg树脂的Tg低于160℃而高Tg树脂的Tg在160℃和更高温度。一般来说,高Tg树脂的Tg在160℃至280℃或者例如从170℃至240℃。高Tg聚合物树脂,包括但不限于,聚四氟乙烯(“PTFE”)和PTFE的混合物。典型的混合物包括PTFE与聚苯醚和氰酸酯的混合物。其它类型包括高Tg树脂的聚合物树脂是环氧树脂,例如双官能团和多官能团的环氧树脂,双马来酰胺/三嗪和环氧树脂(BT环氧树脂),环氧/聚苯醚树脂,丙烯腈丁二烯,聚碳酸酯(PC),聚苯醚(PPO),聚苯醚(PPE),聚苯硫醚(PPS),聚砜(PS),聚酰胺,聚酯例如聚对苯二甲酸乙二酯(PET),聚对苯二甲酸丁二酯(PBT),聚醚酮(PEEK),液晶聚合物,聚氨酯,聚醚酰亚胺,环氧树脂和它们的复合物。
在一个实施例中,本发明的组合物可以将零价金属沉积在通孔壁上,这些组合物可用于制造印刷电路板横向和纵向的过程。
印刷电路板中的通孔大体可以使用钻孔或冲压或其它现有技术中已知方法得到。通孔形成后,电路板任选地浸入水中,在通孔壁去钻污后,使用常见的有机溶液对电路板清洗和脱脂。去钻污是现有技术的熟知工艺,通常情况下通孔去钻污之前要进行溶剂膨胀处理。
溶剂膨胀是现有技术中的熟知工艺,通常可以用于通孔的去钻污。这样的溶剂膨胀剂,通常包括,但不限于,乙二醇醚和它们的相关醚醋酸酯。使用的乙二醇醚和它们的相关醚醋酸酯为常见用量。可使用的商业购买的溶剂膨胀剂例如有CIRCUPOSITTM调整剂(conditioner)3302,CIRCUPOSITTMholeprep 3303和CIRCUPOSITTMhole prep 4120,都可以从陶瓷电子材料公司(DowElectronic Materials)(美国马萨诸塞州莫尔伯勒市)买到。
可选地,通孔随后浸入水中。然后将一种氧化剂施加到通孔上。合适的氧化剂包括但不限于,硫酸,铬酸,碱性高锰酸钾或等离子体蚀刻。通常碱性高锰酸钾用作氧化剂。商业购买的氧化剂例如是购自陶瓷电子材料公司(DowElectronic Materials)的CIRCUPOSITTM促进剂(promoter)4130。
可选地,通孔再次浸入水中,然后通常向通孔中加入中和剂以中和所有氧化剂留下的酸性残留物和碱性残留物。通常来说,中和剂是含有一种或多种胺的碱性水溶液或者3重量%过氧化氢和3重量%硫酸的水溶液。可选地,通孔进入水中,将印刷电路板进行干燥。
中和步骤之后,基底(例如具有通孔的印刷电路板)通常通过施加碱性调节剂而得到调整。这样的碱性调整剂包括但不限于,含有一种或多种季铵的碱性表面活性剂水溶液和聚酰胺和一种或多种表面活性剂。所使用的表面活性剂通常是阳离子表面活性剂,其它表面活性剂,例如,阴离子的,非离子的,和两性的表面活性剂以及它们的组合。另外,pH调节剂和缓冲剂也可以包括在调整剂中。通常来说,阳离子表面活性剂与非离子表面活性剂组合使用。调整剂中表面活性剂的含量为0.05至5重量%,优选从0.25至1重量%。合适的碱性调整剂包括但不限于,CIRCUPOSITTM调整剂231,813和860,均购自陶瓷电子材料公司(Dow Electronic Materials)。可选地,通孔在调整后浸入水中。
阳离子表面活性剂包括但不限于,四烷基铵卤化物,烷基三甲基卤化物,羟乙基烷基咪唑啉,烷基苯扎卤铵(alkylbenzalkonium halide),烷基胺醋酸酯,烷基胺油酸酯和烷基氨乙基甘氨酸。
非离子表面活性剂包括但不限于,脂肪醇类例如脂肪醇烷氧基化物。这样的脂肪醇含有氧化乙烯,氧化丙烯或它们的组合,以便形成分子内具有聚氧乙烯或聚氧丙烯链的化合物,即,(-O-CH2-CH2-)重复基团形成的链,或(-O-CH2-CH-CH3)重复基团形成的链,或它们的组合。通常来说,这样的脂肪醇烷氧基化物(alcohol alkoxylate)是具有7至15个碳原子的碳链,直链或支链的脂肪醇乙氧基化物,并且具有4至20摩尔的乙氧基化物,典型的是5至40摩尔的乙氧基化物,更典型地是5至15摩尔的乙氧基化物(ethoxylates)。一些这样的脂肪醇烷氧基化物可以商业购买得到。可购买到的脂肪醇烷氧基化物例如是NEODOL 91-6,NEODOL 91-8和NEODOL 91-9(每摩尔直链的脂肪醇乙氧基化物平均具有6至9摩尔氧化乙烯(ethylene oxide)的C9-C11醇)和NEODOL 1-73B(每摩尔直链的伯脂肪醇乙氧基化物平均具有7摩尔氧化乙烯的C11醇)。所有上述产品购自壳牌化学公司(Shell Chemicals)。
阴离子表面活性剂包括但不限于,烷基苯基磺酸盐,烷基或烷氧基萘磺酸盐,烷基二苯醚磺酸盐,烷基醚磺酸盐,烷基硫酸酯,聚氧乙烯烷基醚硫酸酯,聚氧乙烯烷基酚醚硫酸酯,高碳醇磷酸单酯,聚氧乙烯烷基醚磷酸(磷酸盐)和烷基琥珀酸酯磺酸盐。
两性表面活性剂包括但不限于,2-烷基-N-羧甲基或乙基-N-羟乙基或甲基咪唑啉甜菜碱,2-烷基-N-羧甲基或乙基-N-羧基甲氧基乙基咪唑啉甜菜碱,二甲基烷基甜菜碱,N-烷基-β-氨基丙酸或其盐和脂肪酸酰胺丙基二甲氨基乙酸甜菜碱。
本发明组合物的一个优势是它们可以用来在基底表面上,特别是印刷电路板中的通孔表面上沉积含有零价金属的组合物。在印刷电路板上沉积零价金属可以避免需要随后的还原步骤。这使得在制备金属化的非导电基底时减少了一个常规步骤。
调整步骤之后是通孔的微蚀刻处理。可以使用常规的微蚀刻组合物。暴露的铜(例如,内层)上的微蚀刻处理提供了微观上的粗糙铜表面,用来提高随后对化学沉积和电镀金属的吸附能力。微蚀刻组合物包括但不限于,60g/L至120g/L的过硫酸钠或氧化单过硫酸氢钠或氧化单过硫酸氢钾和硫酸(2%)的混合物,或硫酸/过氧化氢混合物。可商业购买的微蚀刻组合物例如是购自陶氏电子材料公司(Dow Electronic Materials)的CIRCUPOSITTMmicroetch 3330。可选地,通孔浸入水中。
可选地,之后微蚀刻处理过的通孔经过预浸处理。预浸液例如包括2%至5%的盐酸或25g/L至75g/L的氯化钠酸性水溶液。可选地,通孔浸入冷水中。
之后本发明的组合物作为金属化学沉积的催化剂施加到通孔上。组合物水溶液在从室温(约20℃)至50℃下施加到通孔上,通常是室温至40℃。在催化处理后通孔可选地浸入水中。
之后,通孔壁在金属化学镀液中化学镀上金属,例如是铜。可以使用常规的化学镀液包括浸液。这样的镀液是现有技术中熟知的。典型地,印刷线路板浸入含有所需金属的金属离子的金属化学镀液中,金属沉积到通孔壁上。沉积到通孔壁上的金属,包括但不限于,铜,镍,金,银和铜/镍合金。在沉积于通孔壁上的铜,铜/镍或镍之上也可以通过沉金液或沉银液得到一层金或银。优选地,铜,金或银沉积在通孔壁上,更优选铜沉积在通孔壁上。
金属沉积在通孔壁上之后,通孔可选地浸入水中。可选地,防锈组合物可以施加到沉积在通孔壁的金属上。可以使用常规的防锈组合物。防锈组合物的一个例子是购自陶氏电子材料公司(Dow Electronic Materials)的ANTITARNISHTM 7130。可选地,通孔浸入热水漂洗槽中,然后干燥电路板。
通孔通过化学沉积或金属镀液沉积金属后,基底可以经过进一步处理。进一步处理包括常规的光成像处理和在基底上的进一步金属沉积例如金属的电解沉积,例如,铜,铜合金,锡和锡合金。可以使用常规的金属电解液。这样的电解液是现有技术中熟知的。
本发明的组合物形成了零价金属纳米颗粒的稳定水溶液,可以用于催化非导电基底的金属化学沉积,特别是电子元件制造用的基底。另外,该组合物使基底对金属的吸附性能良好。该组合物是无锡的,由此避免了由锡(II)离子容易氧化至锡(IV)和破坏催化剂带来的种种问题。同时钯离子颗粒尺寸增加,团聚和沉降的问题也显著降低,甚至得到避免。由于锡不包含在组合物中,高昂的氯化锡不再需要,从而催化剂组合物的成本得到降低。另外,制备金属化基底时避免了使用锡时所需要的加速步骤。
实施例1
在室温(约20℃)下将155mg的组氨酸(4-(2-氨基-2-羧乙基)咪唑)加入到装有36mL去离子水的烧杯中,形成稳定剂溶液。滴加0.1N HCl直到所有组氨酸溶解。搅拌条件下,加入溶有29.4mg Na2PdCl4(Pd+2)的2mL去离子水。然后,混合物在室温下搅拌十分钟,pH值调节至5.4。随后,剧烈搅拌下溶液中加入溶有30mg NaBH4的2mL去离子水。溶液立即变成黑色,表明Pd+2还原成Pd0。
加速稳定性测试:上述催化剂溶液随后放入50℃水浴至少12小时,进一步测试其稳定性。结果催化剂组合物未显示出可见的沉淀或浑浊。
工作催化溶液通过用去离子水将催化浓度稀释至25ppm,用HCl/NaOH调节pH值到9.2,然后加入3g/L的作为缓冲剂的碳酸氢钠制备得到。催化溶液的pH值使用购自费舍尔科技有限公司(Fisher Scientific)的AccumetTMAB15型pH计测定。
实施例2
将310mg的组氨酸加入到装有38mL去离子水的烧杯中,混合物加热到60℃使组氨酸完全溶解。冷却至室温(约20℃)后,加入1mL 1×10-4mol/L的AgNO3溶液。然后溶液搅拌十分钟,使用0.1NNaOH调节pH值至12。搅拌的同时在溶液中加入0.05mL的甲醛溶液(37%),然后放入60℃水浴中。溶液缓慢地转变成亮橙色,并且随着反应进行颜色不断加深。大约三十分钟后,溶液颜色为深橙色。反应在60℃下继续一小时。得到的组氨酸/银纳米颗粒催化剂组合物然后经过实施例1的加速稳定性测试,未显示出沉淀或浑浊。
实施例3
Na2PdCl4(138mg)溶于100mL去离子水,加入80mg的CuSO4·5H2O。溶液变成蓝灰色。然后在溶液中加入73mg的组氨酸,溶液变成微黄色。所得溶液使用0.1NNaOH调节pH值至~5.5。然后71mg的NaBH4溶于5mL去离子水。一小份(0.5mL)NaBH4溶液随后在剧烈搅拌下加入到钯/铜溶液中。NaBH4加入后观察到颜色变为黑色。所得催化剂溶液以Pd计稀释至250ppm,室温下搅拌30分钟。催化剂溶液然后经过实施例1的加速稳定性测试,未显示出沉淀或浑浊。
实施例4
将24.5mg的尿刊酸(4-咪唑丙烯酸)加入到装有36mL去离子水的烧杯中。混合物加热到60℃使尿刊酸完全溶解。冷却至室温后,搅拌条件下,加入溶有13.2mg Na2PdCl4的2mL去离子水。白色浑浊的混合物在室温(约20℃)搅拌三十分钟。然后在剧烈搅拌下将溶有20mg NaBH4的2mL去离子水加入到上述混合物中。NaBH4加入后立即观察到颜色变为黑色。所得催化剂溶液在室温下搅拌30分钟。催化剂溶液然后经过实施例1的加速稳定性测试,未显示出沉淀或浑浊。
实施例5
下列稳定的纳米颗粒组合物按照实施例1-4的通用方法制备。在下表中,“DMAB”表示二甲基氨硼烷。
实施例6-对比例
重复实施例1的通用方法,不同的是下列化合物作为稳定剂:咪唑,4-甲基咪唑,2-甲基咪唑,组胺酸二盐酸盐和乙基4-甲基-5咪唑羧酸盐。使用这些化合物所得催化剂组合物均未通过实施例1的加速稳定性测试,形成沉淀或变得浑浊。
实施例7
不同的印刷线路板(Nelco-6环氧树脂/玻璃,NP-175环氧树脂/玻璃,370T,FR-406,TU-752环氧树脂/玻璃,SY-1141和SY-1000-2环氧树脂/玻璃)使用化学镀铜液,按照下列通用方法进行金属化。
在每块板上钻出多个通孔。通孔的平均直径是1mm。然后每块板上的通孔进行去钻污处理,制备化学镀铜液和采用下列垂直式的方法化学镀铜:
1.在80℃下每基块板使用240升溶剂膨胀处理7分钟。膨胀处理液是含有10%二甘醇单丁醚和35g/L氢氧化钠的水溶液。
2.然后室温下将基板在冷的自来水中浸泡4分钟。
3.然后每块基板上的通孔使用550升含有50-60g/L碱性高锰酸钾的碱性氧化剂水溶液在pH值为12,80℃下处理10分钟。
4.室温下将基板在冷的自来水中浸泡4分钟。
5.然后基板上的通孔使用180升含有3重量%过氧化氢和3重量%硫酸的中和剂水溶液在50℃下处理5分钟。
6.将基板在冷的自来水中浸泡4分钟。
7.使用CONDITIONERTM860碱性调整剂对基板进行处理,调整剂包括一种阳离子表面活性剂和维持pH值在大约11的缓冲体系。碱性整理剂购自陶氏电子材料公司(Dow Electronic Materials)。是否需要调整剂要视所采用的具体的稳定零价金属纳米颗粒催化剂而定。
8.然后经步骤7调整处理的基板在室温下置于冷的自来水中浸泡4分钟。
9.然后每块基板上的通孔使用100升含有20g/L过硫酸钠的碱性水溶液在室温下处理2分钟。
10.室温下将基板在冷的自来水中浸泡4分钟。
11.通孔经过5%浓度的盐酸在室温下预浸处理1分钟。
12.然后室温下将基板在冷的自来水中浸泡1分钟。
13.为了使其通孔化学镀铜,一些基板在40℃下使用2升本发明的组合物灌注5分钟。零价金属纳米颗粒的浓度为25ppm。催化剂的pH值通常是9.6。作为对照,其它基板在40℃下使用2升具有钯颗粒浓度为25ppm的常规锡/钯催化剂灌注5分钟。该常规催化剂的配方如下:1g氯化钯;300mL浓盐酸;1.5g单宁酸钠;40g氯化锡和加水至一升。
14.然后室温下将基板在冷的自来水中浸泡2.5分钟。
15.然后板上的通孔壁在36℃下化学镀铜15分钟。化学镀铜液配方如下:
组分 | 用量 |
五水硫酸铜 | 2g |
甲醛 | 2.5g |
氢氧化钠 | 5g |
乙二胺四乙酸(EDTA) | 25g |
氯离子 | 5g |
2,2-联吡啶 | 2ppm |
水 | 加至一升 |
16.化学镀铜后,室温下将基板在冷的自来水中浸泡4分钟。
每块基板均被侧面切割,暴露出通孔的镀铜壁。从每个基板切割的孔壁中挑选出多个1mm厚的侧面切片,采用欧洲背光分级表测定通孔壁覆膜厚度。每个基板的切片(1mm)放在Olympus GX71光学显微镜下观察,放大倍数为50X。沉积铜膜的质量在显微镜下通过光照测定。背光结果显示本发明的催化组合物与常规的锡/钯(Sn/Pd)离子催化剂的性能相当。
Claims (10)
1.一种组合物,包括0.5至100ppm的零价金属,稳定剂化合物和水;其中零价金属选自钯,银,钴,镍,金,铜和钌;其中的稳定剂化合物具有化学式
其中R=H或(C1-C6)烷基;R1各自独立地选自H,(C1-C6)烷基和Z;Z=C2-C6)烯基-Z1或(CR2R3)aZ1;R2和R3各自独立地选自H,羟基,(C1-C6)烷基,羟基(C1-C6)烷基,C(O)-(C1-C6)烷基,(C1-C6)烷基-C(O)-(C1-C6)烷基,CO2R4和NR5R6;R4=H ,(C1-C6)烷基,羟基(C1-C6)烷基或(C1-C4)烷氧基(C1-C6)烷基;R5和R6各自独立地选自H,(C1-C6)烷基和(CR2R3)aZ2;Z1=C(S)SH,CO2H,或C(O)NR5R6;Z2=C(O)R4或CO2R4;和a=0-6;其中至少一个R1是Z。
2.权利要求1的组合物,其中组合物的pH值为6-14。
3.权利要求2的组合物,其中pH值为7.5-14。
4.权利要求1的组合物,其中组合物在20℃储存3个月无沉淀析出。
5.权利要求1的组合物,其中零价金属和稳定剂化合物的摩尔比为1∶1至1∶20。
6.权利要求1的组合物,其中Z1=CO2H。
7.一种方法,包括:
(a)提供具有多个通孔的基底;
(b)将权利要求1的组合物施加到通孔表面上;然后
(c)将金属化学镀到通孔表面上。
8.权利要求7的方法,还包括将第二种金属化学镀在步骤(c)化学镀的金属之上的步骤。
9.权利要求7的方法,还包括在步骤(b)之前,使通孔表面与氧化剂接触的步骤。
10.一种权利要求1的组合物的制备方法,包括将稳定剂化合物,水和水溶性金属盐混合,然后加入足够形成零价金属的量的还原剂。
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