TWI682064B - 鍍浴組合物及鈀之無電鍍覆方法 - Google Patents
鍍浴組合物及鈀之無電鍍覆方法 Download PDFInfo
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- TWI682064B TWI682064B TW104111686A TW104111686A TWI682064B TW I682064 B TWI682064 B TW I682064B TW 104111686 A TW104111686 A TW 104111686A TW 104111686 A TW104111686 A TW 104111686A TW I682064 B TWI682064 B TW I682064B
- Authority
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- Taiwan
- Prior art keywords
- plating bath
- palladium
- acid
- group
- bath composition
- Prior art date
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 238000007747 plating Methods 0.000 title claims abstract description 139
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 79
- 239000000203 mixture Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000007772 electroless plating Methods 0.000 title claims abstract description 14
- -1 palladium ions Chemical class 0.000 claims abstract description 40
- 239000003381 stabilizer Substances 0.000 claims abstract description 35
- 239000000758 substrate Substances 0.000 claims abstract description 33
- 230000002378 acidificating effect Effects 0.000 claims abstract description 30
- 230000000694 effects Effects 0.000 claims abstract description 21
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 239000008139 complexing agent Substances 0.000 claims abstract description 13
- 150000001491 aromatic compounds Chemical class 0.000 claims abstract description 11
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 13
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 13
- 150000003839 salts Chemical group 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 10
- 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 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 claims description 9
- VYWYYJYRVSBHJQ-UHFFFAOYSA-N 3,5-dinitrobenzoic acid Chemical compound OC(=O)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1 VYWYYJYRVSBHJQ-UHFFFAOYSA-N 0.000 claims description 8
- LWFUFLREGJMOIZ-UHFFFAOYSA-N 3,5-dinitrosalicylic acid Chemical compound OC(=O)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1O LWFUFLREGJMOIZ-UHFFFAOYSA-N 0.000 claims description 8
- ZIIGSRYPZWDGBT-UHFFFAOYSA-N 610-30-0 Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O ZIIGSRYPZWDGBT-UHFFFAOYSA-N 0.000 claims description 8
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 claims description 8
- 159000000001 potassium salts Chemical class 0.000 claims description 8
- KAQBNBSMMVTKRN-UHFFFAOYSA-N 2,4,6-trinitrobenzoic acid Chemical compound OC(=O)C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O KAQBNBSMMVTKRN-UHFFFAOYSA-N 0.000 claims description 7
- JECYUBVRTQDVAT-UHFFFAOYSA-N 2-acetylphenol Chemical compound CC(=O)C1=CC=CC=C1O JECYUBVRTQDVAT-UHFFFAOYSA-N 0.000 claims description 7
- SLAMLWHELXOEJZ-UHFFFAOYSA-N 2-nitrobenzoic acid Chemical compound OC(=O)C1=CC=CC=C1[N+]([O-])=O SLAMLWHELXOEJZ-UHFFFAOYSA-N 0.000 claims description 7
- AFPHTEQTJZKQAQ-UHFFFAOYSA-N 3-nitrobenzoic acid Chemical compound OC(=O)C1=CC=CC([N+]([O-])=O)=C1 AFPHTEQTJZKQAQ-UHFFFAOYSA-N 0.000 claims description 7
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims description 7
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical group OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 6
- 235000019253 formic acid Nutrition 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 150000002825 nitriles Chemical class 0.000 claims description 6
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 6
- GZVJGBAQVVJGKW-UHFFFAOYSA-N 2,4,6-triethylbenzoic acid Chemical compound CCC1=CC(CC)=C(C(O)=O)C(CC)=C1 GZVJGBAQVVJGKW-UHFFFAOYSA-N 0.000 claims description 5
- SQGIOBQKNXOJTC-UHFFFAOYSA-N 2,4-diethylbenzoic acid Chemical compound CCC1=CC=C(C(O)=O)C(CC)=C1 SQGIOBQKNXOJTC-UHFFFAOYSA-N 0.000 claims description 5
- MSWNGSGXXVLVPG-UHFFFAOYSA-N 3,5-diethylbenzoic acid Chemical compound CCC1=CC(CC)=CC(C(O)=O)=C1 MSWNGSGXXVLVPG-UHFFFAOYSA-N 0.000 claims description 5
- UEMBNLWZFIWQFL-UHFFFAOYSA-N 3,5-dinitrophenol Chemical compound OC1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1 UEMBNLWZFIWQFL-UHFFFAOYSA-N 0.000 claims description 5
- CHZPJUSFUDUEMZ-UHFFFAOYSA-N 3-acetylbenzoic acid Chemical compound CC(=O)C1=CC=CC(C(O)=O)=C1 CHZPJUSFUDUEMZ-UHFFFAOYSA-N 0.000 claims description 5
- RTZZCYNQPHTPPL-UHFFFAOYSA-N 3-nitrophenol Chemical compound OC1=CC=CC([N+]([O-])=O)=C1 RTZZCYNQPHTPPL-UHFFFAOYSA-N 0.000 claims description 5
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims description 5
- GZGSEMRMKBBQGA-UHFFFAOYSA-N 2,4-bis(ethenyl)phenol Chemical compound OC1=CC=C(C=C)C=C1C=C GZGSEMRMKBBQGA-UHFFFAOYSA-N 0.000 claims description 4
- UFBJCMHMOXMLKC-UHFFFAOYSA-N 2,4-dinitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O UFBJCMHMOXMLKC-UHFFFAOYSA-N 0.000 claims description 4
- DTNSDCJFTHMDAK-UHFFFAOYSA-N 2-cyanobenzoic acid Chemical compound OC(=O)C1=CC=CC=C1C#N DTNSDCJFTHMDAK-UHFFFAOYSA-N 0.000 claims description 4
- CHZCERSEMVWNHL-UHFFFAOYSA-N 2-hydroxybenzonitrile Chemical compound OC1=CC=CC=C1C#N CHZCERSEMVWNHL-UHFFFAOYSA-N 0.000 claims description 4
- SVBXZPJKKZULEW-UHFFFAOYSA-N 3,5-bis(ethenyl)phenol Chemical compound C(=C)C=1C=C(C=C(C1)C=C)O SVBXZPJKKZULEW-UHFFFAOYSA-N 0.000 claims description 4
- ADCUEPOHPCPMCE-UHFFFAOYSA-N 4-cyanobenzoic acid Chemical compound OC(=O)C1=CC=C(C#N)C=C1 ADCUEPOHPCPMCE-UHFFFAOYSA-N 0.000 claims description 4
- CVNOWLNNPYYEOH-UHFFFAOYSA-N 4-cyanophenol Chemical compound OC1=CC=C(C#N)C=C1 CVNOWLNNPYYEOH-UHFFFAOYSA-N 0.000 claims description 4
- FUGYGGDSWSUORM-UHFFFAOYSA-N 4-hydroxystyrene Chemical compound OC1=CC=C(C=C)C=C1 FUGYGGDSWSUORM-UHFFFAOYSA-N 0.000 claims description 4
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 4
- GYLKKXHEIIFTJH-UHFFFAOYSA-N 3-cyanobenzoic acid Chemical compound OC(=O)C1=CC=CC(C#N)=C1 GYLKKXHEIIFTJH-UHFFFAOYSA-N 0.000 claims description 3
- YNGIFMKMDRDNBQ-UHFFFAOYSA-N 3-ethenylphenol Chemical compound OC1=CC=CC(C=C)=C1 YNGIFMKMDRDNBQ-UHFFFAOYSA-N 0.000 claims description 3
- SGHBRHKBCLLVCI-UHFFFAOYSA-N 3-hydroxybenzonitrile Chemical compound OC1=CC=CC(C#N)=C1 SGHBRHKBCLLVCI-UHFFFAOYSA-N 0.000 claims description 3
- IRQWEODKXLDORP-UHFFFAOYSA-N 4-ethenylbenzoic acid Chemical compound OC(=O)C1=CC=C(C=C)C=C1 IRQWEODKXLDORP-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 150000004675 formic acid derivatives Chemical class 0.000 claims description 3
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 3
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims description 3
- 150000003141 primary amines Chemical class 0.000 claims description 3
- 150000003335 secondary amines Chemical class 0.000 claims description 3
- 150000003512 tertiary amines Chemical class 0.000 claims description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 claims description 2
- WDJHALXBUFZDSR-UHFFFAOYSA-N acetoacetic acid Chemical compound CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 claims 1
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 abstract description 21
- 238000000151 deposition Methods 0.000 abstract description 13
- 239000011159 matrix material Substances 0.000 description 11
- WPYMKLBDIGXBTP-UHFFFAOYSA-N Benzoic acid Natural products OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 9
- 230000004913 activation Effects 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- QDAWXRKTSATEOP-UHFFFAOYSA-N 2-acetylbenzoic acid Chemical compound CC(=O)C1=CC=CC=C1C(O)=O QDAWXRKTSATEOP-UHFFFAOYSA-N 0.000 description 6
- LPCJHUPMQKSPDC-UHFFFAOYSA-N 3,5-diethylphenol Chemical compound CCC1=CC(O)=CC(CC)=C1 LPCJHUPMQKSPDC-UHFFFAOYSA-N 0.000 description 6
- LUJMEECXHPYQOF-UHFFFAOYSA-N 3-hydroxyacetophenone Chemical compound CC(=O)C1=CC=CC(O)=C1 LUJMEECXHPYQOF-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- 239000005711 Benzoic acid Substances 0.000 description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 5
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 5
- 235000010233 benzoic acid Nutrition 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 5
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- 239000003929 acidic solution Substances 0.000 description 4
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 4
- QBHDSQZASIBAAI-UHFFFAOYSA-N 4-acetylbenzoic acid Chemical compound CC(=O)C1=CC=C(C(O)=O)C=C1 QBHDSQZASIBAAI-UHFFFAOYSA-N 0.000 description 3
- ONMOULMPIIOVTQ-UHFFFAOYSA-N 98-47-5 Chemical compound OS(=O)(=O)C1=CC=CC([N+]([O-])=O)=C1 ONMOULMPIIOVTQ-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000005121 nitriding Methods 0.000 description 3
- 150000002940 palladium Chemical class 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
- SPXOTSHWBDUUMT-UHFFFAOYSA-N 138-42-1 Chemical compound OS(=O)(=O)C1=CC=C([N+]([O-])=O)C=C1 SPXOTSHWBDUUMT-UHFFFAOYSA-N 0.000 description 2
- KOHSRHXKURUXCP-UHFFFAOYSA-N 2,4,6-triethylphenol Chemical compound CCC1=CC(CC)=C(O)C(CC)=C1 KOHSRHXKURUXCP-UHFFFAOYSA-N 0.000 description 2
- NHJVRSWLHSJWIN-UHFFFAOYSA-N 2,4,6-trinitrobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O NHJVRSWLHSJWIN-UHFFFAOYSA-N 0.000 description 2
- AMUGDZXUAMBOOT-UHFFFAOYSA-N 2,4-diethylbenzenesulfonic acid Chemical compound CCC1=CC=C(S(O)(=O)=O)C(CC)=C1 AMUGDZXUAMBOOT-UHFFFAOYSA-N 0.000 description 2
- LMLAXOBGXCTWBJ-UHFFFAOYSA-N 2,4-diethylphenol Chemical compound CCC1=CC=C(O)C(CC)=C1 LMLAXOBGXCTWBJ-UHFFFAOYSA-N 0.000 description 2
- GWGBNENHEGYJSN-UHFFFAOYSA-N 2,4-dinitrobenzenesulfonic acid;hydrate Chemical compound O.OS(=O)(=O)C1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O GWGBNENHEGYJSN-UHFFFAOYSA-N 0.000 description 2
- RUXQUDWFOUUTIU-UHFFFAOYSA-N 3,5-diethylbenzenesulfonic acid Chemical compound CCC1=CC(CC)=CC(S(O)(=O)=O)=C1 RUXQUDWFOUUTIU-UHFFFAOYSA-N 0.000 description 2
- JWSNVFJCKKXKRE-UHFFFAOYSA-N 3,5-dinitrobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1 JWSNVFJCKKXKRE-UHFFFAOYSA-N 0.000 description 2
- MXVYJZNEWIGHQA-UHFFFAOYSA-N 3-ethylbenzenesulfonic acid Chemical compound CCC1=CC=CC(S(O)(=O)=O)=C1 MXVYJZNEWIGHQA-UHFFFAOYSA-N 0.000 description 2
- TXFPEBPIARQUIG-UHFFFAOYSA-N 4'-hydroxyacetophenone Chemical compound CC(=O)C1=CC=C(O)C=C1 TXFPEBPIARQUIG-UHFFFAOYSA-N 0.000 description 2
- BRIXOPDYGQCZFO-UHFFFAOYSA-N 4-ethylphenylsulfonic acid Chemical compound CCC1=CC=C(S(O)(=O)=O)C=C1 BRIXOPDYGQCZFO-UHFFFAOYSA-N 0.000 description 2
- HWTDMFJYBAURQR-UHFFFAOYSA-N 80-82-0 Chemical compound OS(=O)(=O)C1=CC=CC=C1[N+]([O-])=O HWTDMFJYBAURQR-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- 229910001252 Pd alloy Inorganic materials 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 150000001555 benzenes Chemical class 0.000 description 2
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- CRDYSYOERSZTHZ-UHFFFAOYSA-M selenocyanate Chemical compound [Se-]C#N CRDYSYOERSZTHZ-UHFFFAOYSA-M 0.000 description 2
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- GKWLKAFZCJLZIG-UHFFFAOYSA-N 1-(3-acetyl-4-hydroxyphenyl)ethanone Chemical compound CC(=O)C1=CC=C(O)C(C(C)=O)=C1 GKWLKAFZCJLZIG-UHFFFAOYSA-N 0.000 description 1
- GSTOHKXQBZZTPF-UHFFFAOYSA-N 1-(5-ethyl-2-hydroxyphenyl)ethanone Chemical compound CCC1=CC=C(O)C(C(C)=O)=C1 GSTOHKXQBZZTPF-UHFFFAOYSA-N 0.000 description 1
- IHGWXBWYZUMHLR-UHFFFAOYSA-N 2,4,6-triethylbenzenesulfonic acid Chemical compound CCC1=CC(CC)=C(S(O)(=O)=O)C(CC)=C1 IHGWXBWYZUMHLR-UHFFFAOYSA-N 0.000 description 1
- SJBOEHIKNDEHHO-UHFFFAOYSA-N 2-[2-aminoethyl(carboxymethyl)amino]acetic acid Chemical compound NCCN(CC(O)=O)CC(O)=O SJBOEHIKNDEHHO-UHFFFAOYSA-N 0.000 description 1
- DXVYOFQKMPEIBJ-UHFFFAOYSA-N 2-acetylbenzenesulfonic acid Chemical compound CC(=O)C1=CC=CC=C1S(O)(=O)=O DXVYOFQKMPEIBJ-UHFFFAOYSA-N 0.000 description 1
- UGHLEPMKNSFGCE-UHFFFAOYSA-N 2-ethylbenzenesulfonic acid Chemical compound CCC1=CC=CC=C1S(O)(=O)=O UGHLEPMKNSFGCE-UHFFFAOYSA-N 0.000 description 1
- RXFCIXRFAJRBSG-UHFFFAOYSA-N 3,2,3-tetramine Chemical compound NCCCNCCNCCCN RXFCIXRFAJRBSG-UHFFFAOYSA-N 0.000 description 1
- LXHVCQJGEYIDRJ-UHFFFAOYSA-N 3,5-bis(ethenyl)benzoic acid Chemical compound OC(=O)C1=CC(C=C)=CC(C=C)=C1 LXHVCQJGEYIDRJ-UHFFFAOYSA-N 0.000 description 1
- VWXZFDWVWMQRQR-UHFFFAOYSA-N 3-ethenylbenzoic acid Chemical compound OC(=O)C1=CC=CC(C=C)=C1 VWXZFDWVWMQRQR-UHFFFAOYSA-N 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 1
- DZVFPXYOSGUHDP-UHFFFAOYSA-N C(=C)C1=CC(=C(C(=O)O)C=C1)C=C Chemical compound C(=C)C1=CC(=C(C(=O)O)C=C1)C=C DZVFPXYOSGUHDP-UHFFFAOYSA-N 0.000 description 1
- OYHODLAPGNSRGG-UHFFFAOYSA-N C(=O)O.C(#N)C1=CC=CC=C1 Chemical compound C(=O)O.C(#N)C1=CC=CC=C1 OYHODLAPGNSRGG-UHFFFAOYSA-N 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910001096 P alloy Inorganic materials 0.000 description 1
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
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- 239000004280 Sodium formate Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- OTBHHUPVCYLGQO-UHFFFAOYSA-N bis(3-aminopropyl)amine Chemical compound NCCCNCCCN OTBHHUPVCYLGQO-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-M chlorate Inorganic materials [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-N cyanic acid Chemical group OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 1
- IUNMPGNGSSIWFP-UHFFFAOYSA-N dimethylaminopropylamine Chemical compound CN(C)CCCN IUNMPGNGSSIWFP-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 150000002169 ethanolamines Chemical class 0.000 description 1
- QXXVZGZJCZODQS-UHFFFAOYSA-N formic acid 1-phenylethanone Chemical compound C(=O)O.C(C)(=O)C1=CC=CC=C1 QXXVZGZJCZODQS-UHFFFAOYSA-N 0.000 description 1
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- MGJXBDMLVWIYOQ-UHFFFAOYSA-N methylazanide Chemical compound [NH-]C MGJXBDMLVWIYOQ-UHFFFAOYSA-N 0.000 description 1
- UDGSVBYJWHOHNN-UHFFFAOYSA-N n',n'-diethylethane-1,2-diamine Chemical compound CCN(CC)CCN UDGSVBYJWHOHNN-UHFFFAOYSA-N 0.000 description 1
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 description 1
- DILRJUIACXKSQE-UHFFFAOYSA-N n',n'-dimethylethane-1,2-diamine Chemical compound CN(C)CCN DILRJUIACXKSQE-UHFFFAOYSA-N 0.000 description 1
- QHJABUZHRJTCAR-UHFFFAOYSA-N n'-methylpropane-1,3-diamine Chemical compound CNCCCN QHJABUZHRJTCAR-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- RGHXWDVNBYKJQH-UHFFFAOYSA-N nitroacetic acid Chemical compound OC(=O)C[N+]([O-])=O RGHXWDVNBYKJQH-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002941 palladium compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- HTIMQENIYIHRMC-UHFFFAOYSA-N propane-1,1,2-triamine Chemical compound CC(N)C(N)N HTIMQENIYIHRMC-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- AYGJDUHQRFKLBG-UHFFFAOYSA-M sodium;1,1-dioxo-1,2-benzothiazol-3-olate;dihydrate Chemical compound O.O.[Na+].C1=CC=C2C(=O)[N-]S(=O)(=O)C2=C1 AYGJDUHQRFKLBG-UHFFFAOYSA-M 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- BJHZMIPASCHBRO-UHFFFAOYSA-N sulfomethaneperoxoic acid Chemical compound OOC(=O)S(O)(=O)=O BJHZMIPASCHBRO-UHFFFAOYSA-N 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
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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
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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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
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- C23C18/1675—Process conditions
- C23C18/1676—Heating of the solution
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Abstract
本發明係關於一種鍍浴組合物及一種藉由無電鍍覆將鈀層沉積在基板上之方法。根據本發明之含水酸性鍍浴包括鈀離子源、還原劑、鈀離子之氮化錯合劑及選自由包括至少兩個殘基之芳香族化合物組成之群的水溶性穩定劑,其中至少一殘基係親水殘基及至少一殘基具有負中介效應。該鍍浴具有提高之抗不想要分解的穩定性,同時維持充分鍍覆速率。
Description
本發明係關於鍍浴組合物及鈀之無電鍍覆方法,其用於製造印刷電路板、IC基板及用於半導體晶圓之金屬化。
在製造印刷電路板、IC基板等等以及半導體晶圓之金屬化中之鈀之無電沉積係已經確立之技術。該等鈀層用作例如障壁層及/或可線接合及可焊接之面漆。
包括鈀離子源、氮化錯合劑及選自甲酸及其衍生物之還原劑的無電鍍鈀浴組合物係揭示於US 5,882,736中。與含有次磷酸作為還原劑產生鈀-磷合金層之鍍浴組合物相比,此等無電鍍鈀浴組合物適合沉積純鈀。
包括鈀離子之鍍浴組合物之穩定性係此等鍍浴組合物之重要特徵,此係由於鈀之高價及所沉積之鈀層要求具有可預測性質(諸如內應力,及對於該鈀層沉積在其上之下方基板的高黏著性)。
此鍍浴之穩定性意指該鍍浴係抗分解(即,在鍍浴本身中金屬鈀之不想要沉澱)穩定。由此,穩定鍍浴與不穩定鍍浴相比具有較長壽命。同時,自此鍍浴之鈀沉積速率應足夠高,例如高於10nm/min,以滿足商業鍍鈀方法之要求。
本發明之目標係提供鍍浴組合物及鈀之無電鍍覆方法,其中提高該鍍浴抗不想要分解之穩定性,同時維持在基板上沉積之鈀層的性質。
此目標利用用於鈀無電沉積之含水酸性鍍浴組合物來解決,該含水酸性鍍浴組合物包括:(i)鈀離子源,(ii)鈀離子之氮化錯合劑,(iii)選自由甲酸、其衍生物及鹽組成之群的還原劑,(iv)選自由包括至少兩個殘基之芳香族化合物組成之群的水溶性穩定劑,其中至少一殘基係親水殘基及至少一殘基具有負中介效應,及其中該至少一親水殘基矽選自由羥基、羧基、磺酸及其鹽組成之群;且其中該至少一親水殘基係選自由羥基、羧基、磺酸根及其鹽組成之群;且其中該至少一具有負中介效應之殘基係選自由硝基、腈、乙醯基、羧基及磺酸根組成之群。
此目標進一步藉由無電鍍鈀方法來解決,該方法包括按此順序之以下步驟:a)提供具有金屬表面之基板,b)提供含水酸性鍍浴組合物,其包括(i)鈀離子源,(ii)至少一鈀離子之氮化錯合劑,(iii)選自由甲酸、其衍生物及鹽組成之群的還原劑,(iv)選自由包括至少兩個殘基之芳香族化合物組成之群的水溶性穩定劑,其中至少一殘基係親水殘基及至少一殘基具有
負中介效應,且其中該至少一親水殘基係選自由羥基、羧基、磺酸根及其鹽組成之群;且其中至少一具有負中介效應之殘基係選自由硝基、腈、乙醯基、羧基及磺酸根組成之群;及c)使該基板與該含水酸性鍍浴組合物接觸及由此將鈀層沉積在該基板之金屬表面。
根據本發明之鍍浴具有归因於該水溶性穩定劑之改良之抗不想要分解穩定性,同時維持充分高之鈀在基板上之沉積速率。此外,在根據本發明之無電鍍鈀方法中該含水酸性鍍浴之穩定效能允許沉積具有期望性質(諸如內應力及長時間對下方基板之黏著性)之鈀層。
根據本發明之含水無電鍍鈀浴含有鈀離子源,其係水溶性鈀化合物,諸如氯化鈀、硝酸鈀、乙酸鈀、硫酸鈀及過氯酸鈀。視情況,包括鈀離子及鈀離子之氮化錯合劑之錯合化合物可添加至該鍍浴,而不在鍍浴中藉由將鈀鹽及該鈀離子之氮化錯合劑作為獨立成分添加至該鍍浴來形成此錯合化合物。適宜作為鈀離子源之錯合化合物係例如二氯二乙二胺鈀、二硝基二乙二胺鈀及二乙酸二乙二胺鈀。
在鍍浴中鈀離子之濃度範圍係0.5至500mmol/l,較佳地1至100mmol/l。
該無電鍍鈀浴進一步包括鈀離子之氮化錯合劑。該氮化錯合劑係選自包括一級胺、二級胺及三級胺之群。適宜胺係例如乙二胺、1,3-二胺基-丙烷、1,2-雙(3-胺基-丙基-胺基)-乙烷、2-二乙基-胺基-乙基-胺、二伸乙基-三胺、二伸乙基-三胺-五-乙酸、硝基-乙酸、N-(2-
羥基-乙基)-乙二胺、乙二胺-N,N-二乙酸、2-(二甲基-胺基)-乙胺、1,2-二胺基-丙胺、1,3-二胺基-丙胺、3-(甲基-胺基)-丙胺、3-(二甲基-胺基)-丙胺、3-(二乙基-胺基)-丙胺、雙-(3-胺基-丙基)-胺、1,2-雙-(3-胺基-丙基)-烷胺、二伸乙基-三胺、三伸乙基-四胺、四伸乙基-五胺、五-伸乙基-六胺及其混合物。
在根據本發明之無電鍍浴中之鈀離子之氮化錯合劑與鈀離子的莫耳比範圍係2:1至50:1。
根據本發明之無電鍍浴進一步包括使該鍍浴為自催化,即無電鍍浴之還原劑。在該還原劑存在時,將鈀離子還原為金屬鈀。此鍍覆機制使根據本發明之鍍浴區分為1)不含有鈀離子還原劑之浸漬型鍍鈀浴2)需要外部電流以沉積鈀層之用於電鍍鈀的鍍浴。
根據本發明之無電鍍浴係特別適用於在甲酸、其衍生物及鹽作為還原劑存在時沉積鈀層。適宜甲酸之衍生物係例如甲酸酯,諸如甲酸甲酯、甲酸乙酯及甲酸丙酯。其他適宜之甲酸衍生物係例如經取代及未經取代之胺諸如甲醯胺。適宜甲酸鹽之抗衡離子係例如選自氫、鋰、鈉、鉀及銨。
將該還原劑以10至1000mmol/l之濃度添加至無電鍍浴。
次磷酸離子及/或胺硼烷化合物及/或硼氫化鈉不適宜作為還原劑,由於鈀合金層自此等鍍浴組合物沉積。較佳地,根據本發明之無電鍍鈀浴亦不含有還原劑甲醛,由於此化合物之毒性。
根據本發明之含水酸性鍍浴進一步包括選自由包括至少兩個殘基之芳香族化合物組成之群的水溶性穩定劑,其中至少一殘基係親水殘基及至少一殘基具有負中介效應。
關於穩定劑之術語「水溶性」本文定義為在添加至根據本發明之含水酸性鍍浴組合物的該水溶性穩定劑之需要濃度之水溶性。
術語「芳香族化合物」本文定義為苯之衍生物及聚芳香族烴,
諸如萘。
該等苯之衍生物、萘及等等包括至少兩個殘基,其中至少一者係親水殘基及至少另一殘基係具有負中介效應之殘基。該至少一親水殘基提高根據本發明之水溶性穩定劑的溶解性。
親水殘基係選自由羥基、羧基、磺酸根及其鹽組成之群。較佳地,該親水殘基係選自由羥基、羧基及其鹽組成之群。
具有負中介效應之殘基係選自由硝基、腈、乙醯基、羧基及磺酸根組成之群。較佳地,具有負中介效應之殘基係選自由硝基、腈、乙醯基及羧基組成之群。
在本發明之另一實施例中,具有負中介效應之殘基較佳係選自由腈、乙醯基及羧基組成之群。選自由包括至少一親水殘基及作為至少一具有負中介效應殘基之硝基之芳香族化合物組成之群的水溶性穩定劑可引起不想要之用於鈀之無電沉積之含水酸性鍍浴組合物的黃色變色。
該水溶性穩定劑可包括多於一個先前提及之親水殘基及/或多於一個先前提及之具有負中介效應之殘基。
先前提及之親水殘基及先前提及之具有負中介效應之殘基可以任何組合存在於該穩定劑中,當將該等分子添加至可為根據本發明之鍍浴的含水酸性溶液時,該組合導致在該含水酸性溶液中之分子穩定。由此,具有先前提及之親水殘基之全部列舉成員可與先前提及之具有負中介效應之殘基之全部列舉成員組合。
水溶性穩定劑亦係彼等包括例如至少兩個磺酸根殘基或至少兩個羧基殘基的芳香族化合物,由於此等殘基均係根據本發明之親水殘基及具有負中介效應之殘基。
親水殘基諸如羥基、羧基、磺酸根可藉由將該水溶性穩定劑與鹼性水溶液(例如,NaOH、KOH或NH4OH之水溶液)接觸轉化為相應
鹽諸如鹼金屬鹽。該相應鹽與對應質子化化合物相比具有在酸性含水溶液中之較高穩定性。
更佳地,該水溶性穩定劑係選自由下列組成之群:2-硝基苯酚、3-硝基苯酚、4-硝基苯酚、3,5-二硝基苯酚、2,4-二硝基苯酚、2,4,6-三硝基苯酚、2-硝基苯甲酸、3-硝基苯甲酸、4-硝基苯甲酸、3,5-二硝基苯甲酸、2,4-二硝基苯甲酸、2,4,6-三硝基苯甲酸、2-羥基-3,5-二硝基苯甲酸、2-硝基苯磺酸、3-硝基苯磺酸、4-硝基苯磺酸、3,5-二硝基苯磺酸、2,4-二硝基苯磺酸、2,4,6-三硝基苯磺酸、2-乙醯基苯甲酸、3-乙醯基苯甲酸、4-乙醯基苯甲酸、3,5-二乙醯基苯甲酸、2,4-二乙醯基苯甲酸、2,4,6-三乙醯基苯甲酸、2-乙醯基苯酚、3-乙醯基苯酚、4-乙醯基苯酚、3,5-二乙醯基苯酚、2,4-二乙醯基苯酚、2,4,6-三乙醯基苯酚、2-乙醯基苯磺酸、3-乙醯基苯磺酸、4-乙醯基苯磺酸、3,5-二乙醯基苯磺酸、2,4-二乙醯基苯磺酸、2,4,6-三乙醯基苯磺酸、2-氰基苯甲酸、3-氰基苯甲酸、4-氰基苯甲酸、2-羥基苯甲腈、3-羥基苯甲腈、4-羥基苯甲腈、及其相應銨、鈉及鉀鹽。
甚至更佳地,該水溶性穩定劑係選自由下列組成之群:2-硝基苯酚、3-硝基苯酚、4-硝基苯酚、3,5-二硝基苯酚、2,4-二硝基苯酚、2,4,6-三硝基苯酚、2-硝基苯甲酸、3-硝基苯甲酸、4-硝基苯甲酸、3,5-二硝基苯甲酸、2,4-二硝基苯甲酸、2,4,6-三硝基苯甲酸、2-羥基-3.5-二硝基苯甲酸、2-硝基苯磺酸、3-硝基苯磺酸、4-硝基苯磺酸、3,5-二硝基苯磺酸、2,4-二硝基苯磺酸、2,4,6-三硝基苯磺酸、2-乙醯基苯甲酸、3-乙醯基苯甲酸、4-乙醯基苯甲酸、3,5-二乙醯基苯甲酸、2,4-二乙醯基苯甲酸、2,4,6-三乙醯基苯甲酸、2-乙醯基苯酚、3-乙醯基苯酚、4-乙醯基苯酚、3,5-二乙醯基苯酚、2,4-二乙醯基苯酚、2,4,6-三乙醯基苯酚、2-乙醯基苯磺酸、3-乙醯基苯磺酸、4-乙醯基苯磺酸、3,5-二乙醯基苯磺酸、2,4-二乙醯基苯磺酸、2,4,6-三乙醯
基苯磺酸及其相應銨、鈉及鉀鹽。
仍更佳地,該水溶性穩定劑係選自由下列組成之群:2-硝基苯酚、3-硝基苯酚、4-硝基苯酚、3,5-二硝基苯酚、2,4-二硝基苯酚、2,4,6-三硝基苯酚、2-硝基苯甲酸、3-硝基苯甲酸、4-硝基苯甲酸、3,5-二硝基苯甲酸、2,4-二硝基苯甲酸、2,4,6-三硝基苯甲酸、2-羥基-3,5-二硝基苯甲酸、2-乙醯基苯甲酸、3-乙醯基苯甲酸、4-乙醯基苯甲酸、3,5-二乙醯基苯甲酸、2,4-二乙醯基苯甲酸、2,4,6-三乙醯基苯甲酸、2-乙醯基苯酚、3-乙醯基苯酚、4-乙醯基苯酚、3,5-二乙醯基苯酚、2,4-二醯基苯酚、2,4,6-三乙醯基苯酚、2-氰基苯甲酸、3-氰基苯甲酸、4-氰基苯甲酸、2-羥基苯甲腈、3-羥基苯甲腈、4-羥基苯甲腈、及其相應銨、鈉及鉀鹽。
仍更佳地,該水溶性穩定劑係選自由下列組成之群:2-硝基苯酚、3-硝基苯酚、4-硝基苯酚、3,5-二硝基苯酚、2,4-二硝基苯酚、2,4,6-三硝基苯酚、2-硝基苯甲酸、3-硝基苯甲酸、4-硝基苯甲酸、3,5-二硝基苯甲酸、2,4-二硝基苯甲酸、2,4,6-三硝基苯甲酸、2-羥基-3,5-二硝基苯甲酸、2-乙醯基苯甲酸、3-乙醯基苯甲酸、4-乙醯基苯甲酸、3,5-二乙醯基苯甲酸、2,4-二乙醯基苯甲酸、2,4,6-三乙醯基苯甲酸、2-乙醯基苯酚、3-乙醯基苯酚、4-乙醯基苯酚、3,5-二乙醯基苯酚、2,4-二乙醯基苯酚、2,4,6-三乙醯基苯酚、及其相應銨、鈉及鉀鹽。
最佳地,該水溶性穩定劑係選自由下列組成之群:2-硝基苯甲酸、3-硝基苯甲酸、4-硝基苯甲酸、3,5-二硝基苯甲酸、2,4-二硝基苯甲酸、2,4,6-三硝基苯甲酸、2-羥基-3,5-二硝基苯甲酸及其相應銨、鈉及鉀鹽。
在本發明之另一實施例中,該水溶性穩定劑較佳地係選自由下列組成之群:2-乙醯基苯甲酸、3-乙醯基苯甲酸、4-乙醯基苯甲酸、
3,5-二乙醯基苯甲酸、2,4-二乙醯基苯甲酸、2,4,6-三乙醯基苯甲酸、2-乙醯基苯酚、3-乙醯基苯酚、4-乙醯基苯酚、3,5-二乙醯基苯酚、2,4-二乙醯基苯酚、2,4,6-三乙醯基苯酚、2-氰基苯甲酸、3-氰基苯甲酸、4-氰基苯甲酸、2-羥基苯甲腈、3-羥基苯甲腈、4-羥基苯甲腈、及其相應銨、鈉及鉀鹽;更佳地,2-乙醯基苯甲酸、3-乙醯基苯甲酸、4-乙醯基苯甲酸、3,5-二乙醯基苯甲酸、2,4-二乙醯基苯甲酸、2,4,6-三乙醯基苯甲酸、2-乙醯基苯酚、3-乙醯基苯酚、4-乙醯基苯酚、3,5-二乙醯基苯酚、2,4-二乙醯基苯酚、2,4,6-三乙醯基苯酚、及其相應銨、鈉及鉀鹽。
在根據本發明之鍍浴中該水溶性穩定劑之濃度範圍係1至200mg/l,更佳地5至150mg/l及最佳地10至100mg/l。
多於一種選自芳香族化合物之水溶性穩定劑可用於根據本發明之鍍浴,該芳香族化合物包括至少兩個殘基,其中至少一殘基係親水殘基及至少一殘基具有負中介效應。
視情況,該選自包括至少兩個殘基之芳香族化合物(其中至少一殘基係親水殘基及至少一殘基具有負中介效應)之水溶性穩定劑與至少一額外穩定劑一起存在於根據本發明之鍍浴中,該額外穩定劑選自包括元素硒、碲、銅、鎳、鐵及鉻之化合物及/或巰基-苯并噻唑、硒代-氰酸鹽、硫脲及氰酸亞鐵之群。在根據本發明之鍍浴中此可選額外穩定劑之濃度範圍係0.1至200mg/l。
然而,根據本發明之含水酸性鍍浴較佳地實質上不含上文提及之額外穩定劑,該穩定劑選自包括元素硒、碲、銅、鎳、鐵及鉻之化合物及/或巰基-苯并噻唑、硒代-氰酸鹽、硫脲及氰酸亞鐵之群,由於此等額外穩定劑係或與鈀共沉積(例如銅離子)及由此形成非較佳之鈀合金,或係毒性物質(例如硫脲)。
根據本發明之含水鍍浴係酸性鍍浴。該無電鍍浴之pH值較佳範
圍係4至7,由於該鍍浴在pH值低於4時係不穩定。更佳地,該鍍浴之pH值範圍係5至6。在pH值高於7時,該鍍浴易於在下方基板上藉由浸漬型鍍覆而沉積鈀,導致在鈀層與下方基板間之弱黏著性。此外,具有高於7之pH值之鍍浴組合物可浸蝕有機抗蝕材料諸如亦可作為部分該基板之阻焊劑材料。
鈀之沉積較佳地藉由在根據本發明之無電鍍浴中接觸具有金屬表面之基板來進行。待經鈀塗覆之金屬表面係選自由下列組成之群:銅、銅合金、鎳、鎳合金、鈷及鈷合金。待塗覆之金屬表面係例如印刷電路板、IC基板或半導體晶圓之部分。
使該基板與無電鍍浴接觸之適宜方法係例如將該基板浸入含水鍍浴組合物或將含水鍍浴組合物噴射在該基板上。
該鍍鈀方法在35至95℃之溫度下進行1至60min以獲得厚度範圍在0.01至5.0μm,更佳地0.02至1.0μm及甚至更佳地0.05至0.5μm之鍍鈀層。
在本發明之一實施例中,鈀之薄活化層首先藉由浸漬型鍍覆方法(交換反應)沉積至具有金屬表面之基板上,接著自根據本發明之無電鍍浴沉積鈀。
在無電鈀沉積前之金屬表面活化方法係在此項技術中已知及可應用於進行本發明。一種適宜含水活化浴可包括鈀鹽(諸如乙酸鈀、硫酸鈀及硝酸鈀)、鈀離子之錯合劑(諸如一級胺、二級胺、三級胺及乙醇胺)及酸(諸如硝酸、磺酸及甲磺酸)。視情況,此活化浴進一步含有氧化劑,諸如硝酸根離子、過氯酸根離子、氯酸根離子、過硼酸根離子、過碘酸根離子、過氧-二硫酸根離子及過氧離子。
在含水活化浴中鈀鹽之濃度範圍係0.005至20g/l,較佳地0.05至2.0g/l。鈀離子之錯合劑之濃度範圍係0.01至80g/l,較佳地0.1至8g/l。
該含水活化浴之pH值較佳範圍係0至5,較佳地1至4。
通常,於25至30℃下,將該基板浸沒在含水活化浴中1至4分鐘。在將該基板浸沒在含水活化浴中之前,清潔該基板之金屬表面。為此目的。蝕刻清潔一般在氧化、酸性溶液中進行,例如磺酸或過氧化氫溶液。較佳地,此後接著另一在酸性溶液,諸如例如,磺酸溶液中之清洗。
在根據本發明之鍍浴中之穩定劑增加此等鍍浴之壽命,由於抑制該鍍浴不想要分解。根據本發明之無電鍍鈀方法使鍍覆具有期望物理性質(諸如與在該技術中已知之無電鍍鈀方法相比,內應力及長時間對下方基板之充分黏著性)之鈀層成為可能。
實例
本發明進一步藉由以下非限制性實例闡明。
一般程序
鍍浴基質:鍍浴基質係在全部實例中使用,該基質具有在5至6範圍之pH值及包括水、鈀離子、甲酸鈉及作為鈀離子之氮化錯合劑之乙二胺。在實例1中測試不具有任何穩定劑之鍍浴基質之抗不想要浴分解的穩定性。在實例2至9中將不同量之穩定劑添加至該鍍浴基質及據此測試抗不想要分解之穩定性。
測定抗不想要分解之穩定性之測試:將250ml含水酸性鍍鈀浴加熱至60℃之期望測試溫度,同時攪拌該鍍浴。接著,每60s將1ml鈀膠體溶液(60mg/l鈀)添加至該含水酸性鍍鈀浴,直至在該含水酸性鍍浴中形成灰色沉澱,表明給定鍍浴之不想要分解。該穩定性數對應於直至形成灰色沉澱(即,鍍浴之不想要分解)時添加之測試溶液量(鈀膠體溶液之ml數)。由此,直至形成灰色沉澱時添加至給定鍍浴之6ml鈀膠體溶液量對應於穩定性數6。
抗鍍鈀浴之不想要分解之穩定性以穩定性數表示。
實例1(對照)
在不添加穩定劑下,測試該鍍浴基質之抗不想要分解的穩定性。此鍍浴基質之穩定性數係10。
實例2(對照)
將30mg/l之1,3,5-三羥基苯(具有三個親水殘基但是無具有負中介效應之殘基之芳香族分子)添加至該鍍浴基質。此鍍浴之穩定性數係10。
實例3(對照)
將30mg/l硝基苯(具有一具有負中介效應之殘基但是無親水殘基之芳香族分子)添加至該鍍浴基質,但在鍍浴表面之頂部上仍為固體粒子。據此,呈需要量之硝基苯在鍍浴基質中不係水溶性。
實例4
將30mg/l之4-硝基苯酚添加至該鍍浴基質。此鍍浴之穩定性數係13。由此,該鍍浴之抗鍍浴之不想要分解之穩定性被視為足夠。
實例5
將40mg/l之4-硝基苯甲酸添加至該鍍浴基質。此鍍浴之穩定性數係14。由此,該鍍浴之抗鍍浴之不想要分解之穩定性被視為足夠。
實例6
將50mg/l之3,5-二硝基苯甲酸添加至該鍍浴基質。此鍍浴之穩定性數係17。由此,該鍍浴之抗鍍浴之不想要分解之穩定性被視為足夠。
實例7
將50mg/l之2,4-二硝基苯甲酸添加至該鍍浴基質。此鍍浴之穩定性數係15。由此,該鍍浴之抗鍍浴之不想要分解之穩定性被視為足夠。
實例8
將54mg/l之2-羥基-3,5-二硝基苯甲酸添加至該鍍浴基質。此鍍浴之穩定性數係15。由此,該鍍浴之抗鍍浴之不想要分解之穩定性被視為足夠。
實例9
將42.5mg/l之2-乙醯基苯甲酸添加至該鍍浴基質。此鍍浴之穩定性數係12。由此,該鍍浴之抗鍍浴之不想要分解之穩定性被視為足夠。
實例10(對照)
為模擬現實鍍覆狀況,在實例10至14使用已經使用之鍍浴。該已經使用之鍍浴已根據在一般程序中概述之鍍浴基質組合物來製備。在實例10至14中,根據在一般程序中概述之測試測定抗不想要分解之穩定性。
在實例10中測試不具有任何穩定劑之已經使用之鍍浴的抗不想要浴分解之穩定性。此鍍浴之穩定性數係6。
實例11
將40mg/l之4-硝基苯甲酸添加至根據實例10之已經使用之鍍浴。此鍍浴之穩定性數係11。由此,該鍍浴之抗鍍浴之不想要分解之穩定性被視為足夠。
實例12
將40mg/l之4-硝基苯酚添加至根據實例10之已經使用之鍍浴。此鍍浴之穩定性數係10。由此,該鍍浴之抗鍍浴之不想要分解之穩定性被視為足夠。
實例13(對照)
將40mg/l之二水合糖精鈉添加至根據實例10之已經使用之鍍浴。此鍍浴之穩定性數係9。
實例14
將40mg/l之3-硝基苯磺酸添加至根據實例10之已經使用之鍍浴。此鍍浴之穩定性數係8。
Claims (13)
- 一種用於鈀之無電沉積之含水酸性鍍浴組合物,其包括:(i)鈀離子源,(ii)鈀離子之氮化錯合劑,(iii)選自由甲酸、其衍生物及鹽組成之群的還原劑,(iv)選自由包括至少兩個殘基之芳香族化合物組成之群之水溶性穩定劑,其中至少一殘基係親水殘基及至少一殘基具有負中介效應,且其中該至少一親水殘基係選自由羥基、羧基及其鹽組成之群;且其中該至少一具有負中介效應之殘基係選自由硝基、腈、乙醯基及羧基組成之群。
- 如請求項1之含水酸性鍍浴組合物,其中該鈀離子源係選自由下列組成之群:氯化鈀、硝酸鈀、乙酸鈀、硫酸鈀、過氯酸鈀、二氯二乙二胺鈀、二硝基二乙二胺鈀及二乙酸二乙二胺鈀。
- 如請求項1之含水酸性鍍浴組合物,其中在該含水酸性鍍浴組合物中鈀離子之濃度範圍係0.5至500mmol/l。
- 如請求項1之含水酸性鍍浴組合物,其中該鈀離子之氮化錯合劑係選自由一級胺、二級胺及三級胺組成之群。
- 如請求項1之含水酸性鍍浴組合物,其中在無電鍍浴中該鈀離子之氮化錯合劑與鈀離子之莫耳比範圍係2:1至50:1。
- 如請求項1之含水酸性鍍浴組合物,其中該甲酸衍生物係選自由甲酸酯及甲酸之經取代與未經取代之醯胺組成之群。
- 如請求項1之含水酸性鍍浴組合物,其中該還原劑之濃度範圍係10至1000mmol/l。
- 如請求項1之含水酸性鍍浴組合物,其具有範圍由4至7之pH值。
- 如請求項1之含水酸性鍍浴組合物,其中該水溶性穩定劑係選自由下列組成之群:2-硝基苯酚、3-硝基苯酚、4-硝基苯酚、3,5-二硝基苯酚、2,4-二硝基苯酚、2,4,6-三硝基苯酚、2-硝基苯甲酸、3-硝基苯甲酸、4-硝基苯甲酸、3,5-二硝基苯甲酸、2,4-二硝基苯甲酸、2,4,6-三硝基苯甲酸、2-羥基-3,5-二硝基苯甲酸、2-乙醯基苯甲酸、3-乙醯基苯甲酸、4-乙醯基苯甲酸、3,5-二乙醯基苯甲酸、2,4-二乙醯基苯甲酸、2,4,6-三乙醯基苯甲酸、2-乙醯基苯酚、3-乙醯基苯酚、4-乙醯基苯酚、3,5-二乙醯基苯酚、2,4-二乙醯基苯酚、2,4,6-三乙醯基苯酚、2-氰基苯甲酸、3-氰基苯甲酸、4-氰基苯甲酸、2-羥基苯甲腈、3-羥基苯甲腈、4-羥基苯甲腈、及其相應銨、鈉及鉀鹽。
- 如請求項1之含水酸性鍍浴組合物,其中該水溶性穩定劑係選自由下列組成之群:2-硝基苯甲酸、3-硝基苯甲酸、4-硝基苯甲酸、3,5-二硝基苯甲酸、2,4-二硝基苯甲酸、2,4,6-三硝基苯甲酸、2-羥基-3,5-二硝基苯甲酸及其相應銨、鈉及鉀鹽。
- 如請求項1至10中任一項之含水酸性鍍浴組合物,其中該穩定劑之濃度範圍係0.1至200mg/l。
- 一種無電鍍鈀之方法,其包括以此順序之以下步驟:a)提供具有金屬表面之基板,b)提供如請求項1至11中任一項之含水酸性鍍浴組合物,c)使該基板與該含水酸性鍍浴組合物接觸及由此在該基板之該金屬表面上沉積鈀層。
- 如請求項12之無電鍍鈀之方法,其中在步驟c)中使該基板與該含水酸性鍍浴組合物在35至95℃之溫度下接觸1至60min。
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TWI707061B (zh) * | 2015-11-27 | 2020-10-11 | 德商德國艾托特克公司 | 鈀之電鍍浴組合物及無電電鍍方法 |
TWI692547B (zh) * | 2015-11-27 | 2020-05-01 | 德國艾托特克公司 | 鈀之電鍍浴組合物及無電電鍍方法 |
TW201816183A (zh) * | 2016-10-14 | 2018-05-01 | 日商上村工業股份有限公司 | 無電解鍍鎳浴 |
JP6934396B2 (ja) * | 2017-11-06 | 2021-09-15 | 上村工業株式会社 | 無電解ニッケル−リン−コバルトめっき浴及び無電解ニッケル−リン−コバルトめっき皮膜 |
JP7407644B2 (ja) * | 2020-04-03 | 2024-01-04 | 上村工業株式会社 | パラジウムめっき液及びめっき方法 |
KR102567948B1 (ko) * | 2021-09-23 | 2023-08-21 | (주)제이아이테크 | 페놀 계열의 수소-규소 결합의 안정성 개선을 위한 첨가제 |
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