TWI820793B - 用於填充穿孔的整平劑及電解組合物 - Google Patents
用於填充穿孔的整平劑及電解組合物 Download PDFInfo
- Publication number
- TWI820793B TWI820793B TW111126078A TW111126078A TWI820793B TW I820793 B TWI820793 B TW I820793B TW 111126078 A TW111126078 A TW 111126078A TW 111126078 A TW111126078 A TW 111126078A TW I820793 B TWI820793 B TW I820793B
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- Prior art keywords
- group
- substrate
- plating
- alkyl
- aryl
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 41
- 238000011049 filling Methods 0.000 title claims description 22
- 239000000758 substrate Substances 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 125000003118 aryl group Chemical group 0.000 claims description 29
- 238000009713 electroplating Methods 0.000 claims description 29
- 238000007747 plating Methods 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 24
- 125000001072 heteroaryl group Chemical group 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 19
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 claims description 15
- 238000007772 electroless plating Methods 0.000 claims description 14
- 125000000217 alkyl group Chemical group 0.000 claims description 10
- 229910021645 metal ion Inorganic materials 0.000 claims description 8
- 125000005843 halogen group Chemical group 0.000 claims description 5
- GBXQPDCOMJJCMJ-UHFFFAOYSA-M trimethyl-[6-(trimethylazaniumyl)hexyl]azanium;bromide Chemical compound [Br-].C[N+](C)(C)CCCCCC[N+](C)(C)C GBXQPDCOMJJCMJ-UHFFFAOYSA-M 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 125000001424 substituent group Chemical group 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 229940100198 alkylating agent Drugs 0.000 description 7
- 239000002168 alkylating agent Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- -1 and in this case Chemical compound 0.000 description 6
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 159000000000 sodium salts Chemical class 0.000 description 5
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 229910001431 copper ion Inorganic materials 0.000 description 4
- KUAUJXBLDYVELT-UHFFFAOYSA-N 2-[[2,2-dimethyl-3-(oxiran-2-ylmethoxy)propoxy]methyl]oxirane Chemical compound C1OC1COCC(C)(C)COCC1CO1 KUAUJXBLDYVELT-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- VHNQIURBCCNWDN-UHFFFAOYSA-N pyridine-2,6-diamine Chemical compound NC1=CC=CC(N)=N1 VHNQIURBCCNWDN-UHFFFAOYSA-N 0.000 description 3
- GWEHVDNNLFDJLR-UHFFFAOYSA-N 1,3-diphenylurea Chemical compound C=1C=CC=CC=1NC(=O)NC1=CC=CC=C1 GWEHVDNNLFDJLR-UHFFFAOYSA-N 0.000 description 2
- RUFPHBVGCFYCNW-UHFFFAOYSA-N 1-naphthylamine Chemical compound C1=CC=C2C(N)=CC=CC2=C1 RUFPHBVGCFYCNW-UHFFFAOYSA-N 0.000 description 2
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LZXHHNKULPHARO-UHFFFAOYSA-M (3,4-dichlorophenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].C1=C(Cl)C(Cl)=CC=C1C[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 LZXHHNKULPHARO-UHFFFAOYSA-M 0.000 description 1
- 229940051269 1,3-dichloro-2-propanol Drugs 0.000 description 1
- DEWLEGDTCGBNGU-UHFFFAOYSA-N 1,3-dichloropropan-2-ol Chemical compound ClCC(O)CCl DEWLEGDTCGBNGU-UHFFFAOYSA-N 0.000 description 1
- BGPJLYIFDLICMR-UHFFFAOYSA-N 1,4,2,3-dioxadithiolan-5-one Chemical compound O=C1OSSO1 BGPJLYIFDLICMR-UHFFFAOYSA-N 0.000 description 1
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 1
- LMPMFQXUJXPWSL-UHFFFAOYSA-N 3-(3-sulfopropyldisulfanyl)propane-1-sulfonic acid Chemical compound OS(=O)(=O)CCCSSCCCS(O)(=O)=O LMPMFQXUJXPWSL-UHFFFAOYSA-N 0.000 description 1
- WRBSVISDQAINGQ-UHFFFAOYSA-N 3-(dimethylcarbamothioylsulfanyl)propane-1-sulfonic acid Chemical compound CN(C)C(=S)SCCCS(O)(=O)=O WRBSVISDQAINGQ-UHFFFAOYSA-N 0.000 description 1
- SNKZJIOFVMKAOJ-UHFFFAOYSA-N 3-Amino-1-propanesulfonic acid Natural products NCCCS(O)(=O)=O SNKZJIOFVMKAOJ-UHFFFAOYSA-N 0.000 description 1
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 1
- OBDVFOBWBHMJDG-UHFFFAOYSA-N 3-mercapto-1-propanesulfonic acid Chemical compound OS(=O)(=O)CCCS OBDVFOBWBHMJDG-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 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 1
- 239000005456 alcohol based solvent Substances 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 150000003927 aminopyridines Chemical class 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 1
- 229940073608 benzyl chloride Drugs 0.000 description 1
- 125000001246 bromo group Chemical group Br* 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- WIYCQLLGDNXIBA-UHFFFAOYSA-L disodium;3-(3-sulfonatopropyldisulfanyl)propane-1-sulfonate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)CCCSSCCCS([O-])(=O)=O WIYCQLLGDNXIBA-UHFFFAOYSA-L 0.000 description 1
- 238000009429 electrical wiring Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-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
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004065 semiconductor Substances 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
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C217/00—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton
- C07C217/76—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings and etherified hydroxy groups bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings of the same carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/24—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D213/28—Radicals substituted by singly-bound oxygen or sulphur atoms
- C07D213/30—Oxygen atoms
-
- 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
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/425—Plated through-holes or plated via connections characterised by the sequence of steps for plating the through-holes or via connections in relation to the conductive pattern
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
- C25D5/56—Electroplating of non-metallic surfaces of plastics
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0703—Plating
- H05K2203/072—Electroless plating, e.g. finish plating or initial plating
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0703—Plating
- H05K2203/0723—Electroplating, e.g. finish plating
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Printing Elements For Providing Electric Connections Between Printed Circuits (AREA)
- Non-Metallic Protective Coatings For Printed Circuits (AREA)
- Electroplating Methods And Accessories (AREA)
- Pyridine Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
本發明關於一種整平劑及包含其的電解組合物。當基板中的穿孔被填
充有根據本發明的電解組合物時，該穿孔能夠在相對短的時間內被填充，同時最小化凹坑或空隙的形成。
Description
本發明關於一種能夠在印刷電路板的製造製程中形成的穿孔內部有效地填充電鍍銅之整平劑，以及包含其的電解組合物。
一般而言，印刷電路板是透過在由各種合成樹脂製成的基板的一個或兩個表面上形成金屬佈線，然後排列和固定半導體晶片、積體電路(ICs)或電子部件，並在它們之間實現電佈線來製造的。這些印刷電路板依據電子設備的需要高密度、高性能和薄膜化的趨勢，正在多層化、小型化或製成高度積體電路。
印刷電路板的多層化透過增層法(build-up method)、疊孔法(stack via method)或類似方法來實現。為了實施這些方法，需要填充在印刷電路板的製造製程期間形成的穿孔。填充穿孔的方法可以包含使用絕緣油墨或導電膏(electrically conductive paste)的填充方法，或者使用電鍍法的填充方法。
如果透過電鍍法填充穿孔，當與填充絕緣油墨或導電膏的情況相比，能夠減少由於內部未填充而導致的空隙或凹坑的發生，但是存在電鍍製程需要花費很長的時間以及產率降低的問題。在此，為了提高電鍍方法的產
率，提出了透過施加高電流來減少電鍍製程中所花費的時間之方法，但是當施加高電流時，在電鍍製程期間會產生過量的氫氣，添加劑的分解速率加快且濃度不均勻，以及鍍層不均勻，由此存在印刷電路板的可靠性和穩定性劣化的問題。
因此，需要開發一種能夠確保印刷電路板的可靠性和穩定性同時提高電鍍方法的產率之技術。
[習知技術文件]
[專利文獻]
(專利文獻1)韓國專利申請公開案第2012-0077058號
本發明旨在提供一種整平劑，其能夠有效且均勻地填充形成於基板中之穿孔的內部。
另外，本發明旨在提供一種包含上述整平劑的銅電解組合物。
另外，本發明將提供一種以電解組合物填充基板中之穿孔的方法。
為了解決上述問題，本發明提供一種整平劑，其為下列式1或式2所表示的化合物：
其中，R1至R4各自獨立地選自由C1至C10烷基、C6至C20芳基和C2至C20雜芳基所組成之群，並且在此情況下，複數個R1為彼此相同或不同，複數個R2為彼此相同或不同，R5選自由C1至C10烷基、C6至C20芳基、C2至C20雜芳基和-NR10R11所組成之群，並且在此情況下，複數個R5為彼此相同或不同，R6和R7各自獨立地選自由C1至C10烷基、C6至C20芳基和C2至C20雜芳基所組成之群，n是從1至10的整數，R10和R11各自獨立地選自由氫、C1至C10烷基和C6至C20芳基所組成之群，以及R1至R7的烷基、芳基和雜芳基各自獨立地被一個或多個選自由鹵素基團、C1至C10烷基和C6至C20芳基所組成之群中的取代基所取代或未取代。
同時，本發明提供一種包含金屬離子源的電解組合物；及整平劑。
另外，本發明提供一種填充一基板的穿孔之方法，包含在該基板中形成一穿孔的步驟；透過在其上形成有該穿孔的基板上進行無電極鍍以形成一無電極鍍層的步驟；及透過在其上形成有該無電極鍍層的基板上進行電解電鍍來填充該穿孔的步驟，其中，該電解電鍍由電解組合物進行。
根據本發明的整平劑能夠在電鍍製程期間保持包括在電解組合物常數中的添加劑(例如光亮劑、載體、促進劑)的分解速率、濃度及類似常數。因此，如果以根據本發明的包括整平劑的電解組合物來執行填充穿孔，即使當施加高電流也能夠解決氫氣的過度產生和電鍍不均勻，藉此改善印刷電路板的產率、可靠性、穩定性和類似性質。
相關申請案的交叉引用：
本申請案基於35 U.S.C.§119(a)於2021年7月30日提交的韓國專利申請案第10-2021-0100645號的權益，其全部內容透過引用併入本文。
201:基板
202:無電極鍍層
203:銅電解鍍層
H:穿孔
I1~I4:電流
t1~t6:週期
圖1示意性地示出根據本發明實施例的填充基板中之穿孔的製程。
圖2圖示根據本發明的實施例的填充在基板中的穿孔之製程中的電解電鍍期間所施加的電流密度之波形的圖。
圖3示出根據本發明的實驗例1的實驗結果。
本發明的說明書和請求項中使用的術語和詞語不應被解釋為僅限於普通術語或字典術語，而應被解釋為與本發明的技術思想一致的意義和概念，基於以下原則進行解釋：發明人能夠適當地定義術語的概念，以盡可能最好的方式描述他/她的發明。
本發明關於一種能夠在形成於基板中的穿孔的內部有效地填充電鍍銅之整平劑，以及包含其的電解組合物，以下將對其詳細描述。
根據本發明的整平劑可以是由下列式1或式2表示的化合物。
其中，R1至R4各自獨立地選自由C1至C10烷基(具體地，C1至C5烷基)、C6至C20芳基(具體地，C6至C10芳基)和C2至C20雜芳基(具體地，C3至C10雜芳基)所組成之群，並且在此情況下，複數個R1為彼此相同或不同，複數個R2為彼此相同或不同，R5選自由C1至C10烷基(具體地，C1至C5烷基)、C6至C20芳基(具體地，C6至C10芳基)、C2至C20雜芳基(具體地，C3至C10雜芳基)和-NR10R11所組成之群，並且在此情況下，複數個R5為彼此相同或不同，並且R10和R11各自獨立地選自由氫、C1至C10烷基和C6至C20芳基所組成之群，R6和R7各自獨立地選自由C1至C10烷基(具體地，C1至C5烷基)、C6至C20芳基(具體地，C6至C10芳基)和C2至C20雜芳基(具體地，C3至C10雜芳基)所組成之群，以及
n是從1至10的整數(具體地，從1至5的整數)。
R1的烷基、芳基和雜芳基，R2的烷基、芳基和雜芳基，R3的烷基、芳基和雜芳基，R4的烷基、芳基和雜芳基、R5的烷基、芳基和雜芳基、R6的烷基、芳基和雜芳基，以及R7的烷基、芳基和雜芳基可以各自獨立地被一個或多個選自由鹵素基團、C1至C10烷基和C6至C20芳基所組成之群中的取代基所取代或未取代。
具體地，考慮到整平劑與添加到電解組合物中的添加劑(例如，光亮劑、載體、促進劑等)之間的相互作用，R1和R2可以各自獨立地為被C6至C10芳基所取代的C1至C5烷基。更具體地，R1和R2都可以是由
所表示的官能基團(*表示黏合位置)。
另外，R3和R4可以各自獨立地為C1至C5烷基，具體地，甲基、乙基或丙基。
另外，R5可以選自由C2至C10雜芳基和-NR10R11所組成之群，並且在此情況下，R10和R11可以各自獨立地選自由氫和C6至C10芳基所組成之群。
具體地，R5可以是由
或
所表示的官能基團(*表示黏
合位置)。
另外，R6和R7各自獨立地為C1至C5烷基，具體地，甲基或乙基。
根據本發明的整平劑可以體現為由下列C-1或C-2表示的化合物，但不限於此：
本發明中的雜芳基可以是指包括諸如N、O、S、F及類似雜原子之一個或更多個雜原子的單價芳香環基。
本發明中的鹵素基團可以是指氟基、溴基、氯基、碘基及類似鹵素基團。
同時，根據本發明合成整平劑的方法沒有特別限制，但可以應用在溶劑的存在下使烷化劑化合物與基於胺的化合物反應以提高合成效率的方法。具體地，根據本發明的整平劑能夠透過將烷化劑化合物溶解在溶劑中，然後添加基於胺的化合物並使其反應來合成。在此，烷化劑化合物可以被定義為在與基於胺的化合物進行取代反應的同時在分子中賦予烷基或伸烷基的化合物。
烷化劑化合物沒有特別限制，但可以是選自由1,4-丁二醇、新戊二醇二環氧丙基醚、1,6-己二醇、聚醚胺(分子量400-500g/mol)和1,3-二氯-2-丙醇所組成之群中的至少一種。
基於胺的化合物沒有特別限制，但可以是選自由1,3-胺基苯、2,6-二胺基吡啶、苯胺、4-胺基苯酚、1-萘胺、苯甲基氯、2-胺基吡啶和1,3-二苯基脲所組成之群中的至少一種。
將烷化劑化合物溶解在溶劑中的溫度沒有特別限制，可以為50至180℃。另外，烷化劑化合物(a)與基於胺的化合物(b)的反應比(a：b)沒有特別限制，可以為2：1至6：1的重量比。
用來作為溶解烷化劑化合物的溶劑沒有特別限制，只要是一般已知溶劑即可，但考慮到溶解性和合成效率，溶劑可以是選自由水性溶劑(水、純水、去離子水等)、基於醇的溶劑(乙醇、甲醇等)和有機溶劑(乙腈、二甲基甲醯胺等)所組成之群中的至少一種。
本發明提供一種包含整平劑的電解組合物。具體地，根據本發明的電解組合物包括整平劑和金屬離子源。
根據本發明的電解組合物中包括的整平劑的描述與上述相同，並且由此將省略。此整平劑的濃度(含量)沒有特別限制，但當考慮到電路圖案的均勻性和電鍍效率時，其可以為3至50ml/l，並且具體為5至20ml/l。
根據本發明的電解組合物中包括的金屬離子源提供組合物中的金屬離子，並且可以是一般已知的材料。具體地，金屬離子源可以是銅離子源。金屬離子源的濃度(含量)沒有特別限制，但考慮到電路圖案的均勻性和密度，其可以為100至300g/L，並且具體為200至250g/L。
根據本發明的電解組合物可以進一步包括選自由強酸、鹵素離子源、光亮劑和載體(抑制劑)所組成之群中的至少一種以提高其物理性質。
根據本發明的電解組合物中包括的強酸除了pH控制以外，還作為電解質，可以是一般已知的材料。具體地，強酸可以是選自由硫酸、鹽酸、甲磺酸、乙磺酸、丙磺酸、三氟甲磺酸、磺酸、氫溴酸和氟硼酸所組成之群中的至少一種。強酸的濃度(含量)沒有特別限制，但當考慮到電解組合物的pH值時，其可以為50至150g/L，並且具體為90至110g/L。
根據本發明的電解組合物中包括的鹵素離子源用於將鹵素離子供應到組合物中，並且可以是一般已知的材料。具體地，鹵素離子源可以是氯離子源。鹵素離子源的濃度(含量)沒有特別限制，但當考慮到電路圖案的均勻性和密度時，其可以為30至60mg/L，並且具體為40至50mg/L。
根據本發明的電解組合物中包括的光亮劑是透過提高金屬離子的還原率來促進電鍍，並且可以是一般已知的材料。具體地，光亮劑可以是選自由雙-(3-磺丙基)二硫化物(鈉鹽)、3-巰基-1-丙磺酸(鈉鹽)、3-胺基-1-丙磺酸、O-乙基-S-(3-磺丙基)二硫代碳酸酯(鈉鹽)、3-(2-苯並噻唑-1-硫代)-1-丙磺酸(鈉鹽)和N,N-二甲基二硫代胺甲酸-(3-磺丙基)酯(鈉鹽)所組成之群中的至少一種。光亮劑的濃度(含量)沒有特別限制，但考慮到電鍍率及類似因素，其可以為0.5至5ml/L，具體為1至3.5ml/L。
根據本發明的電解組合物中包括的載體用於提高電路圖案的表面平坦度，並且可以是一般已知的材料。載體的濃度(含量)沒有特別限制，但當考慮到電路圖案的均勻性和電鍍效率，其可以為5至15ml/L，具體為8至12ml/L。
本發明提供一種以該電解組合物填充基板中之穿孔的方法。具體地，根據本發明的填充基板中之穿孔的方法包含透過在其上形成有穿孔的基
板上進行無電極鍍以形成無電極鍍層的步驟；及透過在其上形成有無電極鍍層的基板上進行電解電鍍來填充穿孔的步驟，將參照圖1進行如下詳細描述。
首先，在基板201中形成穿孔H。基板201可以是由傳統已知的絕緣樹脂所製成的基板201。穿孔H可以透過雷射加工或CNC加工形成。在此，穿孔H可以形成為不穿透基板201的凹槽或穿透基板201的孔的形式，如圖1所示。
接著，在其上形成有穿孔H的基板201上進行無電極鍍，以在穿孔H的內部和基板201的表面上形成無電極鍍層202。作為用於進行無電極鍍的鍍液組合物，可以使用一般已知的組合物。例如，可以使用包含銅離子、銅離子錯合劑、銅離子還原劑、pH調節劑和添加劑的鍍液組合物。另外，無電極鍍的條件沒有特別限制，但可以在20至60℃的溫度範圍內及pH 11至14以10μm/小時的速率進行。
然後，在其上形成有無電極鍍層202的基板201上進行電解電鍍以填充穿孔H。亦即，形成電解電鍍層203。作為用於進行電解電鍍的鍍液組合物，可以使用上述電解組合物。
在此，在以電解組合物進行電解電鍍期間施加的電流密度可以作為特定波形施加。亦即，參照圖2，可以施加具有「t1+t2+t3+t4+t5+t6」週期的階梯脈衝(+施加電流)-再脈衝(-施加電流)波形的電流密度。具體地，波形保持正電流I1持續一段時間t1，然後保持正電流I2持續一段時間t2，然後保持負電流I3持續一段時間t3，然後保持負電流I4持續一段時間t4，然後保持負電流I3持續一段時間t5，然後保持正電流I2持續一段時間t6，前述波形週期性地施加一段預定時間以進行電解電鍍。
在此，為了於填充電鍍期間最小化穿孔H之凹坑和空隙的形成，I1可以是2至5 ASD，I2可以是1至2 ASD，I3可以是-1至-2 ASD，並且I4可以是-3至-10 ASD。同時，t1,t2和t6可以分別為10至80ms(具體地，30至50ms)，並且t3,t4和t5可以分別為1至5ms(具體地，2至4ms)。
以此方式，在電解電鍍期間，由於電流密度作為被表示為「t1+t2+t3+t4+t5+t6」週期的階梯脈衝反向電鍍波形被施加，電解電鍍能夠在相對短的時間(具體為20至40分鐘)內完成，同時最小化凹坑和空隙的形成。
在下文中，將透過示例更詳細地描述本發明。然而，以下示例旨在解釋本發明，本發明所屬技術領域中具有通常知識者清楚的是，在本發明的範圍和精神內可以進行各種變化和修改，本發明的範圍不限於此。
[示例1]
將新戊二醇二環氧丙基醚加入到乙醇中，在約50℃的溫度下完全溶解。接著，加入2，6-二胺基吡啶，並且反應進行3至8小時以合成整平劑化合物。此時，新戊二醇二環氧丙基醚與2,6-二胺基吡啶的反應比為3：1的重量比。
[示例2]
將1,4-丁二醇加入甲醇中，在約50℃的溫度下完全溶解。接著，加入苯胺，並且反應進行3至8小時以合成整平劑化合物。此時，1,4-丁二醇與苯胺的反應比為3：1的重量比。
[製備例1]
製備電解組合物，其含有230g/L的五水硫酸銅、100g/L的硫酸、40至50mg/L的鹽酸、1至3.5ml/L的二硫二丙烷磺酸鈉、10ml/L的載體和10ml/l的示例1的整平劑。
[比較製備例1]
除了使用已知的整平劑(Dicolloy公司製造的KBPA)代替示例1的整平劑之外，以與製備例1中相同的方式製備電解組合物。
[實驗例1]
透過雷射加工在厚度為200μm的環氧樹脂基板上形成直徑為90μm且深度為100μm的穿孔。接著，將具有穿孔的環氧樹脂基板放入無電極鍍溶液中，該無電極鍍溶液中含有硫酸銅、EDTA、福馬林、氫氧化鈉和用於表面穩定的添加劑，在65℃下進行無電極鍍以形成銅種子層。然後，分別使用製備例1和比較製備例1中製備的電解組合物進行電解電鍍以填充穿孔。當以電解組合物電鍍時，電鍍條件設置如下。
- 電解組合物溫度：21至24℃
- 攪拌：0.5至1.5 LPM/con.
- 電極：不溶性電極
- 電流密度：在下表1的條件下施加階梯脈衝反向電鍍波形
完成穿孔填充電鍍後，用光學顯微鏡確認基板的橫截面，結果在圖3中示出。
參照圖3，確認以根據本發明的電解組合物進行電鍍的製備例1的情況下，穿孔填充良好，沒有空隙和凹坑發生，而在比較製備例1的情況下，產生了空隙和凹坑，由此穿孔的填充進行的不好。
[實驗例2]
當以實驗例1的電解組合物進行電鍍時，如下表2所示調整施加電流密度的條件，並且進行穿孔填充電鍍。填充電鍍完成後，評估基板的橫截面是否形成凹坑和空隙，結果在下列表3中示出。在此情況下，施加直流(DC)波形而不是階梯脈衝反向電鍍波形作為比較條件。
參照上表3，可以確認，當以根據本發明的電解組合物填充穿孔時，由於施加階梯脈衝反向電鍍波形，即使用於穿孔填充的電鍍時間相對短，電鍍仍進行良好，藉此最小化凹坑和空隙的發生。然而，可以確認，當施加DC波形時，需要60分鐘或更多的電鍍時間以防止凹坑和空隙的發生，並且當在30分鐘內進行電鍍時，會產生嚴重的凹坑。
201:基板
202:無電極鍍層
203:銅電解鍍層
H:穿孔
Claims (3)
- 一種電解組合物，其包含一金屬離子源；及一整平劑，其為下列式1或式2所表示的化合物：
- 一種填充一基板中之一穿孔的方法，包含以下步驟，在該基板上形成該穿孔；透過在其上形成有該穿孔的基板上進行無電極鍍以形成一無電極鍍層；及透過在其上形成有該無電極鍍層的基板上進行電解電鍍來填充該穿孔，其中，以如請求項1所述的電解組合物進行該電解電鍍。
- 如請求項2所述的填充一基板中之一穿孔的方法，其中，一階梯脈衝反向電鍍波形電流密度係被施加到該電解電鍍。
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