TWI683032B - 無電極銅電鍍組成物 - Google Patents
無電極銅電鍍組成物 Download PDFInfo
- Publication number
- TWI683032B TWI683032B TW107100153A TW107100153A TWI683032B TW I683032 B TWI683032 B TW I683032B TW 107100153 A TW107100153 A TW 107100153A TW 107100153 A TW107100153 A TW 107100153A TW I683032 B TWI683032 B TW I683032B
- Authority
- TW
- Taiwan
- Prior art keywords
- copper
- electrodeless
- composition
- acid
- plating
- Prior art date
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- 239000010949 copper Substances 0.000 title claims abstract description 89
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 88
- 239000000203 mixture Substances 0.000 title claims abstract description 82
- 238000007747 plating Methods 0.000 title claims abstract description 43
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 17
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 239000008139 complexing agent Substances 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims description 31
- 238000009713 electroplating Methods 0.000 claims description 23
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000003002 pH adjusting agent Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- TXCXZVFDWQYTIC-UHFFFAOYSA-N 5-pyridin-4-yl-3h-1,3,4-oxadiazole-2-thione Chemical compound O1C(S)=NN=C1C1=CC=NC=C1 TXCXZVFDWQYTIC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 150000003892 tartrate salts Chemical class 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 abstract description 15
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- -1 n-octyl Chemical group 0.000 description 47
- 239000000243 solution Substances 0.000 description 23
- 150000001875 compounds Chemical class 0.000 description 19
- 238000000151 deposition Methods 0.000 description 16
- 230000008021 deposition Effects 0.000 description 16
- 235000002639 sodium chloride Nutrition 0.000 description 14
- 150000002430 hydrocarbons Chemical group 0.000 description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 13
- 239000003054 catalyst Substances 0.000 description 11
- 125000000217 alkyl group Chemical group 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000011347 resin Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 9
- 239000004094 surface-active agent Substances 0.000 description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 8
- 125000004432 carbon atom Chemical group C* 0.000 description 8
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 125000004430 oxygen atom Chemical group O* 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 239000012776 electronic material Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 5
- 238000005530 etching Methods 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- 125000001072 heteroaryl group Chemical group 0.000 description 5
- 125000005842 heteroatom Chemical group 0.000 description 5
- 125000004433 nitrogen atom Chemical group N* 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 229930195734 saturated hydrocarbon Natural products 0.000 description 5
- 125000004434 sulfur atom Chemical group 0.000 description 5
- 230000008961 swelling Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 5
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 4
- ASSKVPFEZFQQNQ-UHFFFAOYSA-N 2-benzoxazolinone Chemical compound C1=CC=C2OC(O)=NC2=C1 ASSKVPFEZFQQNQ-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 229960003237 betaine Drugs 0.000 description 4
- 125000000753 cycloalkyl group Chemical group 0.000 description 4
- 239000003822 epoxy resin Substances 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910052763 palladium Inorganic materials 0.000 description 4
- 229920000647 polyepoxide Polymers 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 229920006380 polyphenylene oxide Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- FLFWJIBUZQARMD-UHFFFAOYSA-N 2-mercapto-1,3-benzoxazole Chemical compound C1=CC=C2OC(S)=NC2=C1 FLFWJIBUZQARMD-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical group O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 235000006708 antioxidants Nutrition 0.000 description 3
- 239000003093 cationic surfactant Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001879 copper Chemical class 0.000 description 3
- 238000007772 electroless plating Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 238000001465 metallisation Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical class [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- QFSYADJLNBHAKO-UHFFFAOYSA-N 2,5-dihydroxy-1,4-benzoquinone Chemical compound OC1=CC(=O)C(O)=CC1=O QFSYADJLNBHAKO-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
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 description 2
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 2
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 2
- 239000005750 Copper hydroxide Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- FFDGPVCHZBVARC-UHFFFAOYSA-N N,N-dimethylglycine Chemical compound CN(C)CC(O)=O FFDGPVCHZBVARC-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 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
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 2
- POJWUDADGALRAB-UHFFFAOYSA-N allantoin Chemical compound NC(=O)NC1NC(=O)NC1=O POJWUDADGALRAB-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 239000002280 amphoteric surfactant Substances 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- VERMEZLHWFHDLK-UHFFFAOYSA-N benzene-1,2,3,4-tetrol Chemical compound OC1=CC=C(O)C(O)=C1O VERMEZLHWFHDLK-UHFFFAOYSA-N 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- NTXGQCSETZTARF-UHFFFAOYSA-N buta-1,3-diene;prop-2-enenitrile Chemical compound C=CC=C.C=CC#N NTXGQCSETZTARF-UHFFFAOYSA-N 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 229910001956 copper hydroxide Inorganic materials 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 150000002118 epoxides Chemical class 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 2
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 description 2
- 229940093915 gynecological organic acid Drugs 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 229920006158 high molecular weight polymer Polymers 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- FBSFWRHWHYMIOG-UHFFFAOYSA-N methyl 3,4,5-trihydroxybenzoate Chemical compound COC(=O)C1=CC(O)=C(O)C(O)=C1 FBSFWRHWHYMIOG-UHFFFAOYSA-N 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920001643 poly(ether ketone) Polymers 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920001515 polyalkylene glycol Polymers 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000002952 polymeric resin Substances 0.000 description 2
- 229920001955 polyphenylene ether Polymers 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 229940079877 pyrogallol Drugs 0.000 description 2
- 229960001755 resorcinol Drugs 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 229940095064 tartrate Drugs 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-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
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- RFTORHYUCZJHDO-UHFFFAOYSA-N 1,3-dimethylimidazolidine-2,4-dione Chemical compound CN1CC(=O)N(C)C1=O RFTORHYUCZJHDO-UHFFFAOYSA-N 0.000 description 1
- VSOSXKMEQPYESP-UHFFFAOYSA-N 1,6-naphthyridine Chemical compound C1=CN=CC2=CC=CN=C21 VSOSXKMEQPYESP-UHFFFAOYSA-N 0.000 description 1
- FLBAYUMRQUHISI-UHFFFAOYSA-N 1,8-naphthyridine Chemical compound N1=CC=CC2=CC=CN=C21 FLBAYUMRQUHISI-UHFFFAOYSA-N 0.000 description 1
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 1
- MCTWTZJPVLRJOU-UHFFFAOYSA-O 1-methylimidazole Chemical compound CN1C=C[NH+]=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-O 0.000 description 1
- PAMIQIKDUOTOBW-UHFFFAOYSA-N 1-methylpiperidine Chemical compound CN1CCCCC1 PAMIQIKDUOTOBW-UHFFFAOYSA-N 0.000 description 1
- BAXOFTOLAUCFNW-UHFFFAOYSA-N 1H-indazole Chemical compound C1=CC=C2C=NNC2=C1 BAXOFTOLAUCFNW-UHFFFAOYSA-N 0.000 description 1
- VZYDKJOUEPFKMW-UHFFFAOYSA-N 2,3-dihydroxybenzenesulfonic acid Chemical compound OC1=CC=CC(S(O)(=O)=O)=C1O VZYDKJOUEPFKMW-UHFFFAOYSA-N 0.000 description 1
- JFJNVIPVOCESGZ-UHFFFAOYSA-N 2,3-dipyridin-2-ylpyridine Chemical compound N1=CC=CC=C1C1=CC=CN=C1C1=CC=CC=N1 JFJNVIPVOCESGZ-UHFFFAOYSA-N 0.000 description 1
- IKQCSJBQLWJEPU-UHFFFAOYSA-N 2,5-dihydroxybenzenesulfonic acid Chemical compound OC1=CC=C(O)C(S(O)(=O)=O)=C1 IKQCSJBQLWJEPU-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
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-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
- OHJPGUSXUGHOGE-UHFFFAOYSA-N 2-methyl-6-(6-methylpyridin-2-yl)pyridine Chemical compound CC1=CC=CC(C=2N=C(C)C=CC=2)=N1 OHJPGUSXUGHOGE-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N 2-propanol Substances CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
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- 229920002223 polystyrene Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 239000001472 potassium tartrate Substances 0.000 description 1
- SCUZVMOVTVSBLE-UHFFFAOYSA-N prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1 SCUZVMOVTVSBLE-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- PBMFSQRYOILNGV-UHFFFAOYSA-N pyridazine Chemical compound C1=CC=NN=C1 PBMFSQRYOILNGV-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- WHMDPDGBKYUEMW-UHFFFAOYSA-N pyridine-2-thiol Chemical compound SC1=CC=CC=N1 WHMDPDGBKYUEMW-UHFFFAOYSA-N 0.000 description 1
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 239000001476 sodium potassium tartrate Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 235000011044 succinic acid Nutrition 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- XFLNVMPCPRLYBE-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate;tetrahydrate Chemical compound O.O.O.O.[Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O XFLNVMPCPRLYBE-UHFFFAOYSA-J 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- NJRXVEJTAYWCQJ-UHFFFAOYSA-N thiomalic acid Chemical compound OC(=O)CC(S)C(O)=O NJRXVEJTAYWCQJ-UHFFFAOYSA-N 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
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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
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- 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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- 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
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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- C—CHEMISTRY; METALLURGY
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/48—Stabilisers against degradation by oxygen, light or heat
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- 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
- C23C18/38—Coating with copper
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- C23C18/405—Formaldehyde
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
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- 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
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Abstract
本發明揭示無電極銅電鍍組成物，包含（a）銅離子，（b）用於銅離子之錯合劑，（c）還原劑，（d）pH值調節劑以及（e）穩定劑。穩定劑具有特定化學結構，且有助於使無電極銅電鍍組成物穩定以免分解。
Description
本發明關於無電極銅電鍍組成物。更特定言之，本發明關於包括穩定劑之無電極銅電鍍組成物，所述穩定劑能夠延長鍍銅組成物之使用壽命。
無電極銅電鍍組成物廣泛用於金屬化工業中，以用於在不同類型之基板上沈積銅。舉例而言，在製造印刷線路板時，使用無電極銅浴液將銅沈積至通孔及電路路徑中作為後續電解銅電鍍之基礎。無電極銅電鍍亦用於裝飾塑膠工業中，以用於將銅沈積在非導電性表面上作為視需要進一步電鍍銅、鎳、金、銀及其他金屬之基礎。
無論無電極銅電鍍組成物為否正在被有效使用，其通常皆傾向於在某一時間段之後自發地分解。認為電鍍組成物中產生之少量金屬銅原子核起始隨機沈積過程，其必然降低無電極銅電鍍組成物之整體穩定性且縮短適用之浴液之使用壽命。金屬銅原子核由單價氧化銅（Cu2
O）之歧化反應形成，所述反應由歸因於無電極銅電鍍組成物之不良穩定性之二價銅離子（Cu2+
）之不完全還原而產生。此類分解之無電極銅電鍍浴液可能產生具有深色外觀之品質較差之銅沈積薄膜。
為了解決所述問題，研發許多用於無電極銅電鍍浴液之穩定劑。參見US3,257,215；US3,361,580；US3,649,308；US3,310,430；US3,095,309；US3,222,195；US3,392,035；US3,453,123；US3,903,907；US3,436,233；US3,790,392以及US3,804,638。然而，此等專利中揭示之一些穩定劑引起其他問題，如無電極銅電鍍之低沈積速率或較差之銅沈積層。因此，仍然需要研發新的穩定劑，其可防止無電極銅電鍍浴液分解且延長浴液使用壽命，同時不降低沈積速率及銅沈積層之品質。
本發明之一個實施例為無電極銅電鍍組成物，包括（a）銅離子，（b）用於銅離子之錯合劑，（c）還原劑，（d）pH值調節劑以及（e）由以下式（1）表示之化合物
其中R1
及R2
獨立地選自具有1至20個碳原子之飽和或不飽和烴基，其中烴基之一或多個碳原子可由氮原子或氧原子置換，R1
及R2
可彼此組合以形成環或稠環，烴基可經烷基、環烷基、烷氧基、芳基、雜芳基或鹵素取代，且X為選自硫原子或氧原子之雜原子。
本發明之另一實施例為用於在基板上形成銅薄膜之方法，包括以下步驟：使基板與包括以下物質之組成物接觸：（a）銅離子，（b）用於銅離子之錯合劑，（c）還原劑，（d）pH值調節劑以及（e）由以下式（1）表示之化合物，
其中R1
及R2
獨立地選自具有1至20個碳原子之飽和或不飽和烴基，其中烴基之一或多個碳原子可由氮原子或氧原子置換，R1
及R2
可彼此組合且形成環或稠環，烴基可經烷基、環烷基、烷氧基、芳基、雜芳基或鹵素取代，且X為選自硫原子或氧原子之雜原子。
如本說明書通篇所使用，除非上下文另外明確指示，否則下文提供之縮寫具有以下含義：mg=毫克；ml=毫升；L=公升；cm=公分；m=公尺；mm=毫米；μm=微米（micron/micrometer）；min.=分鐘；ppm=毫克/公升=百萬分率；℃=攝氏度；g/L=公克/公升；wt%=重量百分比；DI=去離子化。
術語「電鍍」及「沈積」在整個本說明書中可互換地使用。術語「電鍍組成物」、「電鍍浴液」以及「電鍍溶液」在整個本說明書中可互換地使用。除非另外指出，否則所有量皆為重量百分比。
本發明之一個實施例包含無電極銅電鍍組成物，包括由以下式（1）表示之化合物
在式（1）中，R1
及R2
獨立地選自具有1至20個碳原子之飽和或不飽和烴基。飽和或不飽和烴基之實例包含（但不限於）烷基，如甲基、乙基、丙基、正丁基、第三丁基、異丁基、己基、正辛基、第三辛基、癸基、十四烷基、十六烷基以及十八烷基；環烷基，如環己基；芳基，如苯基、萘基以及伸聯苯基；烯基；炔基以及環烯基。烴基之一或多個碳原子可由氮原子或氧原子置換。此類基團之實例包含（但不限於）胺基、雜芳基以及稠合雜芳基。R1
及R2
可彼此組合以形成環或稠環。烴基可經烷基、環烷基、烷氧基、芳基、雜芳基或鹵素取代。X為選自硫原子或氧原子之雜原子。X較佳為硫原子。
當式（1）中之X為硫原子時，式（1）具有由以下式（3）表示之共振子。
在式（3）中，R1
及R2
與上文所描述相同。
當無電極銅電鍍浴液中包含由式（1）表示之化合物時，浴液穩定性提高且分解速度非常緩慢。
較佳地，R1
及R2
彼此組合以形成環或稠環。此類化合物由以下式（2）表示。
在式（2）中，R3
為具有2至20個碳原子之飽和或不飽和烴基，其中烴基之一或多個碳原子可由選自氮原子或氧原子之雜原子置換。更佳地，至少一個烴基由選自氮原子或氧原子之雜原子置換以形成雜芳基化合物。
由式（2）表示之化合物之實例包含（但不限於）
（2-巰基苯并噁唑），
（2-苯并噁唑啉酮），
（3-乙基-2-硫酮基-4-噁唑烷酮），
（5-甲氧基苯并噁唑-2-硫醇），
（5-氯-2-巰基苯并噁唑），及
5-(4-吡啶基)-1,3,4-噁二唑-2-硫醇。
較佳地，由式（2）表示之化合物選自巰基苯并噁唑、2-苯并噁唑啉酮以及5-(4-吡啶基)-1,3,4-噁二唑-2-硫醇。
可使用一或多種由式（1）表示之化合物之混合物。化合物之量通常為0.01 ppm至1000 ppm，較佳為0.1 ppm至10 ppm。
本發明之無電極銅電鍍組成物包括銅離子。銅離子源包含（但不限於）水溶性鹵化物、硝酸鹽、乙酸鹽、硫酸鹽以及銅之其他有機及無機鹽。可使用此類銅鹽中之一或多種之混合物提供銅離子。實例包含硫酸銅（如五水合硫酸銅）、氯化銅、硝酸銅、氫氧化銅及胺基磺酸銅。
組成物中可使用習知量之銅鹽。組成物中可包含一或多種銅離子源以提供至少0.5 g/L，較佳1 g/L至30 g/L，更佳1 g/L至20 g/之量之銅離子濃度。
本發明之無電極銅電鍍組成物包括一或多種用於銅離子之錯合劑。錯合劑起作用以防止無電極銅電鍍組成物中銅之氫氧化物沈積。錯合劑之實例包含（但不限於）有機酸，如羧酸及其鹽。此類羧酸包含（但不限於）：酒石酸、檸檬酸、乙酸、蘋果酸、丙二酸、抗壞血酸、草酸、乳酸、丁二酸及其鹽。此類鹽包含有機酸之鹼金屬鹽，如羅謝爾鹽（Rochelle salts），其包含酒石酸鉀鈉，及酒石酸二鉀。錯合劑亦可包含乙內醯脲及乙內醯脲衍生物中之一或多種，如1-甲基內醯脲、1,3-二甲基乙內醯脲以及5,5-二甲基乙內醯脲、氮基乙酸及其鹼金屬鹽、三乙醇胺、乙二胺四乙酸（EDTA）及其鹼金屬鹽（如乙二胺四乙酸四鈉）、經改質之乙二胺四乙酸（如三乙酸N-羥基乙二胺酯）、經羥基烷基取代之二鹼性三胺（如五羥基丙基二伸乙基三胺）以及如N,N-二羧基甲基L-谷氨酸四鈉鹽、S,S-乙二胺二丁二酸以及N,N,N',N'-四(2-羥基丙基)伸乙基二胺(伸乙基二氮基)四-2-丙醇等化合物。較佳地，錯合劑選自酒石酸鹽及EDTA，且最佳錯合劑為酒石酸鹽。
本發明之發明人發現由式（1）表示之化合物與酒石酸鹽之組合對隨後揭示之浴液穩定性展示極佳結果。
組成物中可包含至少0.5 g/L，較佳1 g/L至150 g/L，更佳10 g/L至100 g/L，最佳15 g/L至50 g/L之量之錯合劑。
本發明之無電極銅電鍍組成物包括一或多種還原劑。還原劑之實例包含（但不限於）次磷酸鹽，如鹼金屬次磷酸鹽，如次磷酸鈉，亞磺酸鹽化合物，如羥基甲烷亞磺酸鈉。還原劑亦可包含乙醛酸、甲醛、氫化硼鹽以及二甲基胺硼烷。較佳地，還原劑為甲醛。組成物中可包含至少1 g/L，較佳5 g/L至50 g/L，更佳5 g/L至30 g/L之量之還原劑。
本發明之無電極銅電鍍組成物可包括一或多種pH值調節劑。在無電極銅電鍍組成物中添加pH值調節劑以在較佳範圍內調節pH值。通常，可使用鹼性化合物。pH值調節劑之實例包含（但不限於）氫氧化鈉、氫氧化鉀、氫氧化鋰、氫氧化四甲基銨、三乙醇胺以及單乙醇胺。典型地使用氫氧化鈉、氫氧化鉀或其混合物。可按提供8及更大之pH值範圍之量包含此類鹼化合物，較佳pH值為10至14，更佳pH值為11至13.5。
無電極銅組成物中可包含其他添加劑。許多此類添加劑在此項技術中為熟知的。此類添加劑包含（但不限於）：界面活性劑、晶粒細化劑、加速劑、抗氧化劑以及抑制劑。
組成物中可包含習知界面活性劑。此類界面活性劑包含離子性（如陽離子性及陰離子性界面活性劑）、非離子性以及兩性界面活性劑。可使用界面活性劑之混合物。一般而言，無電極銅電鍍組成物中可包含習知量之界面活性劑。組成物中可包含0.001 g/L至50 g/L之量之界面活性劑。
陽離子性界面活性劑包含（但不限於）：四烷基銨鹵化物、烷基三甲基銨鹵化物、羥基乙基烷基咪唑啉、烷基苯甲烴銨鹵化物、乙酸烷基胺、油酸烷基胺以及烷基胺基乙基甘胺酸。
陰離子性界面活性劑包含（但不限於）：烷基苯磺酸鹽、烷基或烷氧基萘磺酸鹽、烷基二苯基醚磺酸鹽、烷基醚磺酸鹽、烷基硫酸酯、聚環氧乙烷烷基醚硫酸酯、聚氧乙烯烷基酚醚硫酸酯、高級醇磷酸單酯、聚氧化烯烷基醚磷酸（磷酸鹽）以及烷基磺基丁二酸鹽。
兩性界面活性劑包含（但不限於）：2-烷基-N-羧基甲基或乙基-N-羥乙基或甲基咪唑鎓甜菜鹼、2-烷基-N-羧基甲基或乙基-N-羧基甲基氧基乙基咪唑鎓甜菜鹼、二甲基烷基甜菜鹼、N-烷基-β-胺基丙酸或其鹽以及脂肪酸醯胺丙基二甲基胺基乙酸甜菜鹼。
較佳界面活性劑為非離子性。非離子性界面活性劑包含（但不限於）：烷基苯氧基聚乙氧基乙醇、具有20至150個重複單元之聚氧乙烯聚合物以及聚氧乙烯與聚氧丙烯之嵌段及無規共聚物。
添加晶粒細化劑以幫助提供具有相對較高可靠性的更精細之沈積表面。晶粒細化劑包含（但不限於）：高分子量聚合物化合物，如聚伸烷基二醇、聚丙烯醯胺、聚丙烯酸酯、聚丙二醇及聚乙二醇（PEG）以及尿囊素。高分子量聚合物化合物之分子量為500至20,000。舉例而言，可使用PEG 600、PEG 2000、PEG 4000、PEG 6000以及PEG 10000。組成物中可包含基本上0.1 ppm至300 ppm，較佳1 ppm至100 ppm之晶粒細化劑。
添加加速劑以加速電鍍過程。加速劑亦稱為促進劑。加速劑包含（但不限於）有機鹽，如銨鹽及硝酸鹽。組成物中可包含典型用於無電極銅組成物之習知量之加速劑。
抗氧化劑包含（但不限於）：單羥基、二羥基及三羥基苯酚，其中一個氫原子或多個氫原子可未經取代或經-COOH、-SO3
H、低碳烷基或低碳烷氧基、對苯二酚、兒茶酚、間苯二酚、對苯二酚、連苯三酚、偏苯三酚、間苯三酚、愈創木酚（guaiacol）、五倍子酸、3,4-二羥基苯甲酸、酚磺酸、甲酚磺酸、對苯二酚磺酸、兒茶酚磺酸及其鹽取代。組成物中可包含典型用於無電極銅組成物之習知量之抗氧化劑。
在無電極銅電鍍組成物中添加抑制劑以控制其電鍍率。有時抑制劑在無電極銅電鍍組成物中與穩定劑類似地起作用，且為此項技術中熟知的。組成物中可包含典型用於無電極銅組成物之習知量之抑制劑。
視情況地，本發明之無電極銅電鍍組成物包含其他典型用於無電極銅組成物之穩定劑。此類穩定劑之實例包含（但不限於）含硫化合物，如巰基丁二酸、二硫代二丁二酸、巰基吡啶、巰基苯并噻唑、硫脲以及硫脲衍生物；化合物，如吡啶、嘌呤、喹啉、吲哚、吲唑、咪唑、吡嗪以及其衍生物；醇，如炔烴醇、烯丙基醇、芳基醇以及環狀苯酚；經羥基取代之芳族化合物，如甲基-3,4,5-三羥基苯甲酸酯、2,5-二羥基-1,4-苯醌以及2,6-二羥基萘；胺；胺基酸；水可溶金屬化合物，如金屬氯化物及硫酸鹽；矽化合物，如矽烷、矽氧烷及低至中等分子量聚矽氧烷；鍺以及其氧化物及氫化物；以及聚伸烷基二醇、纖維素化合物、烷基苯基乙氧基化物及聚氧乙烯化合物；以及穩定劑，如噠嗪、甲基哌啶、1,2-二-(2-吡啶基)乙烯、1,2-二-(吡啶基)乙烯、2,2'-二吡啶基胺、2,2'-聯吡啶、2,2'-聯嘧啶、6,6'-二甲基-2,2'-聯吡啶、二-2-吡喃酮、N,N,N',N'-四伸乙基二胺、萘、1,8-萘啶、1,6-萘啶、四硫富瓦烯、三聯吡啶、酞酸、異酞酸以及2,2'-二苯甲酸。無電極銅組成物中可包含0.01 ppm至1000 ppm，較佳0.05 ppm至100 ppm，更佳1 ppm至30 ppm之量之此類添加劑。
無電極銅組成物可用於在導電及非導電基板上沈積銅。可按此項技術中已知之許多習知方法使用無電極組成物。典型地銅沈積為在20℃至80℃之溫度下進行。無電極組成物較佳在30℃至60℃之溫度下沈積銅。將待電鍍銅之基板浸沒於無電極組成物中或將無電極組成物噴霧至基板上。可使用習知電鍍時間將銅沈積至基板上。沈積可進行5秒至30分鐘；然而，電鍍時間可視基板上所需之銅厚度及電鍍浴液溫度而變化。銅電鍍率可在0.01微米/10分鐘至5微米/10分鐘，較佳0.1微米/10分鐘至2微米/10分鐘範圍內。
基板包含（但不限於）：包含無機及有機物質之材料，如玻璃、陶瓷、瓷、樹脂、紙、布以及其組合。金屬包覆及非包覆材料亦可為電鍍無電極銅組成物之基板。
基板亦包含印刷電路板。此類印刷電路板包含由熱固性樹脂、熱塑性樹脂以及其組合（包含纖維，如玻璃纖維，及前述浸透實施例）包覆及非包覆之金屬。
熱塑性樹脂包含（但不限於）：縮醛樹脂、丙烯酸樹脂（如丙烯酸甲酯）、纖維素樹脂（如乙酸乙酯）、丙酸纖維素、乙酸丁酸纖維素及硝酸纖維素、聚醚、耐綸、聚乙烯、聚苯乙烯、苯乙烯摻合物（如丙烯腈苯乙烯及共聚物及丙烯腈-丁二烯苯乙烯共聚物）、聚碳酸酯、聚氯三氟乙烯及乙烯基聚合物及共聚物，如乙酸乙烯酯、乙烯醇、乙烯基縮丁醛、氯乙烯、氯乙烯-乙酸酯共聚物、偏二氯乙烯以及乙烯基縮甲醛。
熱固性樹脂包含（但不限於）：鄰苯二甲酸烯丙酯、呋喃、三聚氰胺-甲醛、酚-醛及酚-糠醛共聚物（單獨的或與丁二烯丙烯腈共聚物或丙烯腈-丁二烯-苯乙烯共聚物複合）、聚丙烯酸酯、矽酮、脲甲醛、環氧樹脂、烯丙基樹脂、鄰酞酸甘油酯以及聚酯。
無電極銅組成物可用於電鍍低及高Tg
樹脂。低Tg
樹脂具有低於160℃之Tg
且高Tg
樹脂具有160℃及更高之Tg
。典型高Tg
樹脂具有160℃至280℃或如170℃至240℃之Tg
。高Tg
聚合物樹脂包含（但不限於）：聚四氟乙烯（PTFE）及聚四氟乙烯摻合物。此類摻合物包含例如具有聚亞苯基氧化物及氰酸酯之PTFE。其他類別之聚合物樹脂（其包含具有高Tg
之樹脂）包含（但不限於）：環氧樹脂（如雙功能及多功能環氧樹脂）、雙馬來醯亞胺/三嗪及環氧樹脂（BT環氧化物）、環氧化物/聚苯醚樹脂、丙烯腈丁二烯苯乙烯、聚碳酸酯（PC）、聚苯醚（PPO）、聚亞苯基醚（PPE）、聚苯硫醚（PPS）、聚碸（PS）、聚醯胺、聚酯（如聚對苯二甲酸乙二酯（PET）及聚對苯二甲酸亞丁酯（PBT））、聚醚酮（PEEK）、液晶聚合物、聚胺基甲酸酯、聚醚醯亞胺、環氧化物以及其複合物。
無電極組成物可用於在印刷電路板基板之通孔或通路之壁上以及板之其他部分上沈積銅。無電極組成物可用於製造印刷電路板之水平及垂直製程中。
通常，板可用水沖洗，且清洗及去除油污，接著去除通孔壁上之膠渣。通常預備或軟化通孔之介電質或膠渣以應用溶劑膨脹開始。可使用任何習知溶劑膨脹劑。具體類型可視電介質材料之類型而變化。可進行少量實驗以測定哪種溶劑膨脹劑適用於特定電介質材料。溶劑膨脹劑包含（但不限於）：二醇醚及其相關乙酸醚。市售溶劑膨脹劑之實例為可自Dow Electronic Materials購得之CIRCUPOSIT™ Conditioner 3302A、CIRCUPOSIT™ Hole Prep 3303以及CIRCUPOSIT™ Hole Prep 4120溶液。
在溶劑膨脹劑之後，可施用促進劑。可使用習知促進劑。此類促進劑包含硫酸、鉻酸、鹼性高錳酸或等離子蝕刻。通常使用鹼性高錳酸作為促進劑。市售促進劑之實例為可自Dow Electronic Materials購得之CIRCUPOSIT™ Promoter 4130及CIRCUPOSIT™ MLB Promoter 3308溶液。基板及通孔可視情況用水沖洗。
接著可施用中和劑以中和由促進劑殘留之任何殘餘物。可使用習知中和劑。中和劑通常為含有一或多種胺之酸性水溶液或3重量%過氧化氫與3重量%硫酸之溶液。市售中和劑之實例為CIRCUPOSIT™ MLB Neutralizer 216-5。視情況地，用水沖洗基板及通孔且接著乾燥。
在中和之後，施用酸或鹼性調節劑。可使用習知調節劑。此類調節劑可包含一或多種陽離子性界面活性劑、非離子性界面活性劑、錯合劑以及pH值調節劑或緩衝劑。市售酸調節劑之實例為可自Dow Electronic Materials購得之CIRCUPOSIT™ Conditioners 3320A及3327溶液。適合之鹼性調節劑包含（但不限於）：含有一或多種三級胺及多元胺之水性鹼性界面活性劑溶液。市售鹼性界面活性劑之實例為CIRCUPOSIT™ Conditioner 231、3325、813以及860調配物。基板及通孔可視情況用水沖洗。
可在調節之後進行微蝕刻。可使用習知微蝕刻組成物。微蝕刻經設計以在暴露之金屬上提供微粗糙化金屬表面（例如內層及表面蝕刻），以增強後續電鍍無電極金屬及稍後電鍍物之黏合。微蝕刻劑包含（但不限於）：60 g/L至120 g/L過硫酸鈉或氧代單過硫酸鈉或氧代單過硫酸鉀及硫酸（2%）混合物，或一般硫酸/過氧化氫。市售微蝕刻組成物之實例為可自Dow Electronic Materials購得之CIRCUPOSIT™ Microetch 3330 Etch溶液及PREPOSIT™ 748 Etch溶液。視情況用水沖洗基板。
視情況地，可接著對微蝕刻基板及通孔進行預先浸漬。預先浸漬劑包含（但不限於）：有機鹽，如酒石酸鈉鉀或檸檬酸鈉、0.5%至3%硫酸或25 g/L至75 g/L氯化鈉之酸性溶液。
接著可對基板施用催化劑。可使用習知催化劑，如習知錫/鈀膠態催化劑。市售催化劑包含（但不限於）：可自Dow Electronic Materials購得之CATAPOSIT™ 44及CATAPOSIT™ 404催化劑調配物。施用可藉由此項技術中使用之習知方法進行，如將基板浸沒在催化劑溶液中或使用習知裝置通過噴霧或霧化進行。催化劑停留時間對於垂直設備而言可在1分鐘至10分鐘範圍內，典型地2分鐘至8分鐘，且對於水平設備而言為25秒至120秒。可在室溫至80℃，典型地30℃至60℃之溫度下施用催化劑。在施用催化劑之後，可視情況用水沖洗基板及通孔。
接著使用無電極銅組成物，在基板及通孔壁上無電極電鍍銅。電鍍時間及溫度可為習知的。通常銅沈積可在20℃至80℃，更通常30℃至60℃之溫度下進行。可將基板浸沒於無電極電鍍組成物中或可將無電極組成物噴霧至基板上。通常，無電極電鍍可進行5秒至30分鐘；然而，電鍍時間可視所需金屬厚度而變化。在鹼性環境中進行電鍍以防止基板上包覆之任何金屬之非所需腐蝕。
可視情況對金屬施用抗變色劑。可使用習知抗變色組成物。抗變色劑之實例為可自Dow Electronic Materials購得之ANTI TARNISH™ 7130溶液。基板可視情況用水沖洗且接著可將板乾燥。
在用銅電鍍基板之後，基板可經歷進一步處理。進一步處理可包含通過光成像進行之習知處理，及基板上之進一步金屬沈積，如例如銅、銅合金、錫及錫合金之電解金屬沈積。
無電極銅組成物提供替代性還原劑，其使得能夠排除許多習知還原劑且在儲存期間以及在銅沈積期間穩定。未能觀測氧化銅形成為組成物穩定性之一項指標。此外，可通過在空載若干小時之前及之後檢驗組成物之電鍍率來評估還原劑穩定性。對於穩定之組成物，在空載之前及之後觀測至基本上相同之電鍍率。無電極銅組成物提供均勻銅沈積物，其具有基本上均勻之粉紅色及光滑外觀，且通常符合商業上可接受之無電極銅浴液所需之工業標準。無電極銅組成物亦按商業上可接受之速率電鍍銅。排除習知的對環境有害之還原劑能夠產生環保之無電極銅電鍍組成物。 實例
以下實例進一步說明本發明之實施例，但並不意欲限制本發明之範圍。除非另有指示，否則所有份數及百分比為按重量計。 實例1-15 穩定性測試
進行穩定性測試以檢驗穩定劑使無電極銅電鍍浴在多種浴液溫度（50℃及40℃）下，在某一時間（22及44小時）穩定之效能。
使用2-巰基苯并噁唑（本發明實例）、5-(4-吡啶基)-1,3,4-噁二唑-2-硫醇（本發明實例）、硫脲（比較實例）以及2-巰基苯并噻唑（比較實例）作為穩定劑。亦使用2,2'-聯吡啶作為穩定劑以實現無電極銅電鍍溶液之鹼性穩定性。溶液調配物列舉於表1及2中。
根據表1及2中展示之調配物，在瓶子中製備一百（100）毫升溶液。在水浴中，在表2中展示之溫度下儲存每個瓶子。分析在儲存約22及44小時之後之銅含量，且結果亦列舉於表2中。通過下文所描述之滴定來分析剩餘在無電極銅電鍍溶液中之銅含量。 滴定方法 1) 使浴液樣品冷卻至室溫。將10 ml經冷卻之樣品（不含沈澱之銅）滴入250 ml錐形燒瓶中且添加15 ml 2.5%硫酸溶液。 2) 向混合物中添加約3 g過硫酸鈉。 3) 加熱至沸騰且保持兩分鐘。 4) 添加50 ml去離子水及25 ml 200 g/L之乙酸銨溶液。溫熱至約40℃。 5) 添加3滴PAR指示劑且用EDTA（0.05 M）自灰粉紅色滴定至灰綠色終點。 6) 所得銅含量可如下式計算： 銅（g/L）=[EDTA之毫升數×EDTA之莫耳濃度×63.54]/等分試樣（10 ml） 表1 
表2 
實例16-30 碰撞測試
進行碰撞測試以檢驗在浴液中添加鈀催化劑時穩定劑之效能。此項測試主要旨在模擬鈀污染物在無電極銅電鍍溶液中之作用。鈀污染物視為引起無電極銅電鍍溶液分解之主要起因。因此，除了在溶液中添加2 ml含0.2% CATAPOSITTM
44催化劑之200 g/L氯化鈉溶液以外，條件與實例1至10之條件相同。無電極銅電鍍溶液之溫度及時間與實例1至10相同。每個實例之調配物及結果展示於表3中。 表3 
實例31-33 沈積率測試
進行沈積率測試以檢驗穩定劑對無電極銅電鍍溶液之沈積率及沈積顏色之作用。無電極電鍍之過程流程列舉於表4中。通過使用以下滴定方法測定銅沈積量來測量電鍍溶液之沈積率。結果展示於表5中。 沈積率分析 1) 將5 cm正方形（5 cm×5 cm）電鍍板置放於500 ml燒杯中。 2) 添加25 ml pH 10氨緩衝液及3滴過氧化氫（35%）。 3) 在板上溶解所有沈積物。 4) 添加25 ml去離子水。 5) 添加3滴PAN指示劑且用0.05 M EDTA滴定至綠色終點。 6) 根據下式計算電鍍厚度：電鍍厚度（μm）=(EDTA之毫升數×EDTA之莫耳濃度×63.54×10)/(8.92×總板面積（cm2
）)。 表4 
表5 
無
無
Claims (3)
- 一種無電極銅電鍍組成物，包括(a)銅離子，(b)用於銅離子之錯台劑，(c)還原劑，(d)pH值調節劑以及(e)0.1ppm至1ppm之5-(4-吡啶基)-1,3,4-噁二唑-2-硫醇。
- 如申請專利範圍第1項之無電極銅電鍍組成物，其中所述錯合劑為選自一或多種酒石酸鹽及乙二胺四乙酸。
- 一種對基板進行無電極銅電鍍的方法，包括以下步驟：(i)提供包括一或多個通孔及通路的基板；(ii)使所述包括一或多個通孔及通路的基板與包括以下物質之無電極銅電鍍組成物接觸：(a)銅離子，(b)用於銅離子之錯合劑，(c)還原劑，(d)pH值調節劑以及(e)0.1ppm至1ppm之5-(4-吡啶基)-1,3,4-噁二唑-2-硫醇；以及(iii)使用所述無電極銅組成物，在所述一或多個通孔及通路壁上無電極電鍍銅。
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| US10294569B2 (en) * | 2017-10-06 | 2019-05-21 | Rohm And Haas Electronic Materials Llc | Stable electroless copper plating compositions and methods for electroless plating copper on substrates |
| US10655227B2 (en) * | 2017-10-06 | 2020-05-19 | Rohm And Haas Electronic Materials Llc | Stable electroless copper plating compositions and methods for electroless plating copper on substrates |
| WO2019098011A1 (ja) * | 2017-11-16 | 2019-05-23 | 株式会社村田製作所 | 樹脂多層基板、電子部品およびその実装構造 |
| WO2019098012A1 (ja) * | 2017-11-16 | 2019-05-23 | 株式会社村田製作所 | 樹脂多層基板、電子部品およびその実装構造 |
| US20190382901A1 (en) * | 2018-06-15 | 2019-12-19 | Rohm And Haas Electronic Materials Llc | Electroless copper plating compositions and methods for electroless plating copper on substrates |
| KR102124324B1 (ko) * | 2018-11-14 | 2020-06-18 | 와이엠티 주식회사 | 도금 적층체 및 인쇄회로기판 |
| RU2705050C1 (ru) * | 2018-12-19 | 2019-11-01 | Сергей Геннадьевич Каплунов | Раствор для контактного меднения изделий из стали |
| US20220220617A1 (en) * | 2019-05-28 | 2022-07-14 | Atotech Deutschland Gmbh | Tin plating bath and a method for depositing tin or tin alloy onto a surface of a substrate |
| CN110344035A (zh) * | 2019-07-17 | 2019-10-18 | 安徽启明表面技术有限公司 | 化学镀镍稳定剂及化学镀镍液 |
| TWI780602B (zh) * | 2021-02-24 | 2022-10-11 | 超特國際股份有限公司 | 用於化學電鍍處理非導電區域的活化溶液及方法 |
| CN113463074B (zh) * | 2021-06-03 | 2022-06-14 | 广东硕成科技股份有限公司 | 一种沉铜组合物及沉铜方法 |
| CN113897600A (zh) * | 2021-09-29 | 2022-01-07 | 江西超洋科技有限公司 | 一种双络合体系低应力化学镀铜液及其制备方法和应用 |
| JP7348984B1 (ja) | 2022-04-18 | 2023-09-21 | 台湾上村股▲分▼有限公司 | 無電解銅めっき液及び前記無電解銅めっき液を利用するナノ双晶銅金属層の製造方法 |
| CN116949435B (zh) * | 2022-04-18 | 2025-09-16 | 台湾上村股份有限公司 | 无电镀铜镀液及无电镀制备纳米双晶铜金属层的方法 |
| CN117385348A (zh) * | 2023-09-11 | 2024-01-12 | 广东利尔化学有限公司 | 一种沉铜液以及稳定剂 |
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