JP2015172239A - 無電解めっき液を用いた貫通電極の形成方法 - Google Patents
無電解めっき液を用いた貫通電極の形成方法 Download PDFInfo
- Publication number
- JP2015172239A JP2015172239A JP2015023207A JP2015023207A JP2015172239A JP 2015172239 A JP2015172239 A JP 2015172239A JP 2015023207 A JP2015023207 A JP 2015023207A JP 2015023207 A JP2015023207 A JP 2015023207A JP 2015172239 A JP2015172239 A JP 2015172239A
- Authority
- JP
- Japan
- Prior art keywords
- plating solution
- hole
- electroless
- copper
- forming
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000007772 electroless plating Methods 0.000 title abstract description 30
- 238000007747 plating Methods 0.000 claims abstract description 64
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052802 copper Inorganic materials 0.000 claims abstract description 61
- 239000010949 copper Substances 0.000 claims abstract description 61
- 238000009792 diffusion process Methods 0.000 claims abstract description 44
- 229920000642 polymer Polymers 0.000 claims abstract description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000010941 cobalt Substances 0.000 claims abstract description 23
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 23
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008139 complexing agent Substances 0.000 claims abstract description 20
- 125000003277 amino group Chemical group 0.000 claims abstract description 19
- 229910001092 metal group alloy Inorganic materials 0.000 claims abstract description 19
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 11
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 11
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010030 laminating Methods 0.000 claims abstract description 6
- 230000002265 prevention Effects 0.000 claims description 35
- 230000015572 biosynthetic process Effects 0.000 claims description 21
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 claims description 12
- 239000003002 pH adjusting agent Substances 0.000 claims description 12
- DYUWTXWIYMHBQS-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCNCC=C DYUWTXWIYMHBQS-UHFFFAOYSA-N 0.000 claims description 6
- 230000035515 penetration Effects 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 239000010703 silicon Substances 0.000 abstract description 10
- 229910052710 silicon Inorganic materials 0.000 abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 8
- 230000003449 preventive effect Effects 0.000 abstract 3
- 239000010410 layer Substances 0.000 description 75
- 239000000243 solution Substances 0.000 description 60
- 229910000531 Co alloy Inorganic materials 0.000 description 21
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 14
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 239000000654 additive Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 9
- 229910000990 Ni alloy Inorganic materials 0.000 description 9
- 229910001431 copper ion Inorganic materials 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 9
- 229910000085 borane Inorganic materials 0.000 description 8
- -1 molybdate ions Chemical class 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 230000000996 additive effect Effects 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 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
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000008034 disappearance Effects 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 235000015165 citric acid Nutrition 0.000 description 4
- 150000001879 copper Chemical class 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 229920003169 water-soluble polymer Polymers 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical class OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 2
- 239000005749 Copper compound Substances 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 150000008051 alkyl sulfates Chemical class 0.000 description 2
- 229940045714 alkyl sulfonate alkylating agent Drugs 0.000 description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 description 2
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001868 cobalt Chemical class 0.000 description 2
- 150000001869 cobalt compounds Chemical class 0.000 description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 2
- 229940044175 cobalt sulfate Drugs 0.000 description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000012790 confirmation Methods 0.000 description 2
- 150000001880 copper compounds Chemical group 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 125000005265 dialkylamine group Chemical group 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- 150000002816 nickel compounds Chemical class 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 125000005270 trialkylamine group Chemical group 0.000 description 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 2
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-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
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000000708 deep reactive-ion etching Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 239000005078 molybdenum compound Substances 0.000 description 1
- 150000002752 molybdenum compounds Chemical class 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229920000083 poly(allylamine) Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 1
- HLWRUJAIJJEZDL-UHFFFAOYSA-M sodium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetate Chemical compound [Na+].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC([O-])=O HLWRUJAIJJEZDL-UHFFFAOYSA-M 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000003658 tungsten compounds Chemical class 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/76841—Barrier, adhesion or liner layers
- H01L21/76843—Barrier, adhesion or liner layers formed in openings in a dielectric
- H01L21/76846—Layer combinations
-
- 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
- C23C18/1651—Two or more layers only obtained by electroless plating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
- C23C18/1879—Use of metal, e.g. activation, sensitisation with noble metals
-
- 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
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
-
- 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
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Abstract
【解決手段】基板に形成された孔の側壁に対し、(1)少なくともコバルトイオン又はニッケルイオン、錯化剤、還元剤及びpH調整剤を含有する無電解コバルトめっき液又は無電解ニッケルめっき液を用いて、前記孔の入り口から前記孔の中央部に銅に対する拡散防止層である金属合金膜を形成する工程、(2)少なくともコバルトイオンまたはニッケルイオン、錯化剤、還元剤、pH調整剤およびアミノ基を有するポリマーを含有する無電解コバルトめっき液または無電解ニッケルめっき液を用いて、前記孔の中央部から前記孔の底に拡散防止層である金属合金膜を形成する工程、及び(3)無電解銅めっき液を用いて、(1)工程及び(2)工程で形成された拡散防止層上に銅シード層を積層する工程を有する、上記貫通電極の形成方法。
【選択図】図2
Description
実装面積の省スペース化、処理速度の改善、消費電力の低減といった課題に対応すべく、シリコン、ガラス、セラミック等に貫通電極を形成し、半導体チップを積層する方法が提案されており、中でも基材にシリコンを使用したシリコン貫通ビア(TSV)を中心とした研究が盛んである。TSVは、シリコン基板に貫通孔を開けた後、貫通孔側壁にシリコン酸化膜やポリイミド等の絶縁層を形成し、貫通孔内に導電体である銅を充填することで形成される。
図1にTSV形成工程の一例を示す。まず、配線層が形成されたウェーハにDRIEなどでビアを形成し(図1a)、絶縁用酸化膜、バリアメタル層、更に導通用シードを成膜した後(図1b)、電気めっきによってビア内部に銅を充填する(図1c)。ウェーハ表層に析出した余剰の銅をCMPで取り除くとともに平坦化し(図1d)、その後ウェーハ裏面を削り込んで薄層化し、裏面まで貫通するTSVを形成する(図1e)。これをはんだなどの接合層を介して積み上げることで一つのパッケージとなる(図1f)。
また、PVDやCVDに代わる方法として、無電解めっき法による貫通孔側壁に対する拡散防止層、銅シード層の成膜手法が提案されているが(特許文献1)、無電解めっき法においても貫通孔上部において金属が堆積しやすいことに変わりはなく、ステップカバレッジの改善が必要である。
すなわち本発明は、以下の通りである。
<1> 貫通電極の形成方法であって、基板に形成された孔の側壁に対し、(1)少なくともコバルトイオンまたはニッケルイオン、錯化剤、還元剤およびpH調整剤を含有する無電解コバルトめっき液または無電解ニッケルめっき液を用いて、前記孔の入り口から前記孔の中央部に銅に対する拡散防止層である金属合金膜を形成する工程、
(2)少なくともコバルトイオンまたはニッケルイオン、錯化剤、還元剤、pH調整剤およびアミノ基を有するポリマーを含有する無電解コバルトめっき液または無電解ニッケルめっき液を用いて、前記孔の中央部から前記孔の底に拡散防止層である金属合金膜を形成する工程、及び
(3)無電解銅めっき液を用いて、(1)工程及び(2)工程で形成された拡散防止層上に銅シード層を積層する工程を有する、前記貫通電極の形成方法である。
<2> 前記アミノ基を有するポリマーの含有量が、めっき液全量に対して0.0001質量%〜0.02質量%である、上記<1>に記載の貫通電極の形成方法である。
<3> 前記アミノ基を有するポリマーが、アリルアミン重合体、ジアリルアミン重合体、または、アリルアミンもしくはジアリルアミンを含む共重合体である、上記<1>又は<2>に記載の貫通電極の形成方法である。
<4> (1)工程および(2)工程で使用するめっき液が、タングステンおよび/またはモリブデンを含有する、上記<1>から<3>のいずれかに記載の貫通電極の形成方法である。
<5> 前記孔の底における金属合金膜の膜厚(S)と、前記孔の入り口における金属合金膜の膜厚(C)との比(ステップカバレッジ(S/C)×100%)が30〜300%である、上記<1>から<4>のいずれかに記載の貫通電極の形成方法である。
本発明に使用される拡散防止層形成用の無電解めっき液は、金属塩、錯化剤、還元剤及びpH調整剤を含む水溶液であり、それぞれを任意の割合で混合して用いられる。金属塩は、コバルト化合物またはニッケル化合物が挙げられ、また、金属膜を合金化するためにタングステンおよび/またはモリブデンが含まれる場合もある。錯化剤は金属イオンが水酸化物として沈殿しないように金属イオンを錯体化して無電解めっき液中での安定性を向上させるためのものである。還元剤は、金属イオンを還元するためのものであり、pH調整剤はめっき液のpHを調整するものである。
無電解めっき液に含まれるコバルトイオン濃度としては0.005〜0.5mol/Lが好適であり、より好ましくは0.01〜0.4mol/Lであり、特に0.02〜0.3mol/Lが好ましいが、これら濃度に限定されることなく、適宜好適な濃度を決定できる。
無電解めっき液に含まれるニッケルイオン濃度としては0.005〜0.5mol/Lが好適であり、より好ましくは0.01〜0.4mol/Lであり、特に0.02〜0.3mol/Lが好ましいが、これら濃度に限定されることなく、適宜好適な濃度を決定できる。
無電解めっき液に含まれるタングステン酸イオン濃度としては0.005〜0.5mol/Lが好適であり、より好ましくは0.01〜0.4mol/Lであり、特に0.05〜0.3mol/Lが好ましいが、これら濃度に限定されることなく、適宜好適な濃度を決定できる。
無電解めっき液に含まれるモリブデン酸イオン濃度としては0.005〜0.5mol/Lが好適であり、より好ましくは0.01〜0.4mol/Lであり、特に0.05〜0.3mol/Lが好ましいが、これら濃度に限定されることなく、適宜好適な濃度を決定できる。
無電解めっき液に含まれる錯化剤の濃度は、コバルトイオン、ニッケルイオン濃度に対して1倍等量以上の濃度である必要があり、2倍以上が好適である。具体的には、0.01〜1mol/Lが好適であり、より好ましくは0.05〜0.8mol/Lであり、特に0.1〜0.6mol/Lが好ましい。錯化剤の濃度が0.01〜1mol/Lであるとき、安定的にめっき操作を行うことができる。
無電解めっき液に含まれる還元剤の濃度は、0.001〜0.6mol/Lが好適であり、より好ましくは0.005〜0.5mol/Lであり、特に0.01〜0.4mol/Lが好ましい。還元剤の濃度が0.001〜0.6mol/Lであるとき、めっき膜の形成を安定的に行うことができる。
無電解めっき液のpH値としては、7〜13が好適であり、より好ましくは7.5〜12であり、特に8〜11が好ましい。pH値が7〜13であるとき、めっき膜の形成を安定的に行うことができる。
これらの添加剤は、めっき被膜の平滑性を向上させるレベラーとしての役割を果たす。無電解めっき液に含まれる界面活性剤や水溶性高分子の濃度は1ppm〜5000ppmが好適である。
アミノ基を有するポリマーの平均分子量は、特に制限はないが300〜200000が好適であり、より好ましくは500〜100000である。
無電解めっき液中のアミノ基を有するポリマーの濃度は、0.0001〜0.02質量%が好適であり、より好ましくは0.0002〜0.01質量%であり、特に0.0003〜0.005質量%が好ましい。アミノ基を有するポリマーの濃度が0.0001質量%未満のとき、孔上部での膜成長抑制効果が得られず、均一な膜の成膜が不可能となる。また、アミノ基を有するポリマーの濃度が0.02質量%を超える場合は、ボトムアップ効果が低下するという不具合に加え、めっき液へのポリマーの溶解性が悪化するという問題も生じる。
無電解めっき液に含まれる銅イオン濃度としては0.001〜0.5mol/Lが好適であり、より好ましくは0.005〜0.4mol/Lであり、特に0.01〜0.3mol/Lが好ましいが、これら濃度に限定されることなく、適宜好適な濃度を決定できる。
無電解めっき液に含まれる錯化剤の濃度は、銅イオン濃度に対して1倍等量以上の濃度である必要があり、1.5倍以上が好適である。具体的には、0.0015〜1mol/Lが好適であり、より好ましくは0.0075〜0.8mol/Lであり、特に0.015〜0.6mol/Lが好ましい。錯化剤の濃度が0.0015〜1mol/Lであるとき、安定的にめっき操作を行うことができる。
無電解めっき液に含まれる還元剤の濃度は、0.001〜0.8mol/Lが好適であり、より好ましくは0.005〜0.7mol/Lであり、特に0.01〜0.6mol/Lが好ましい。還元剤の濃度が0.001〜0.8mol/Lであるとき、めっき膜の形成を安定的に行うことができる。
無電解めっき液のpH値としては、9〜14が好適であり、より好ましくは10〜13.5であり、特に10.5〜13が好ましい。pH値が9〜14であるとき、めっき膜の形成を安定的に行うことができる。
これらの添加剤は、めっき被膜の平滑性を向上させるレベラーとしての役割を果たす。無電解銅めっき液に含まれる界面活性剤や水溶性高分子の濃度は1ppm〜5000ppmが好適である。
無電解めっき処理温度としては、40℃〜90℃が好ましく、より好ましくは45℃〜80℃であり、特に50℃〜70℃が好ましい。
金属合金膜の膜厚を測定する方法としては、金属合金膜形成後の評価基材を孔に対し垂直方向に割断し、合金膜断面を走査型電子顕微鏡(SEM)を用いて観察し、測長することで膜厚を求めることができる。
評価基板
評価用の基材として、シリコンウェハにドライエッチング技術を用いて形成した直径10μm、深さ100μmの孔(L/D=10)の側壁に、絶縁層としてシリコン酸化膜を成膜した。続いて、シリコン酸化膜上にカップリング剤により吸着層を形成した後、パラジウム(Pd)コロイド溶液に浸漬させることで、反応開始触媒であるPdを付着させたウェハを形成した。
無電解コバルトめっき液
硫酸コバルト2質量%(0.13mol/L)、錯化剤としてクエン酸6質量%(0.32mol/L)、タングステン酸5質量%(0.2mol/L)、還元剤としてジメチルアミンボラン0.4質量%(0.07mol/L)を含有し、pH調整剤として水酸化テトラメチルアンモニウムでpH値を9.5にした水溶液を調製した。
無電解銅めっき液
硫酸銅0.5質量%(0.03mol/L)、エチレンジアミン四酢酸4質量%(0.14mol/L)、グリオキシル酸1質量%(0.14mol/L)、2,2’ビピリジル0.005質量%(50ppm)、ポリエチレングリコール0.05質量%(500ppm)を含有し、水酸化テトラメチルアンモニウムでpH値を12.5にした水溶液を調製した。
図2に拡散防止層及び銅シード層を積層する際の断面模式図を示す。孔を有する評価基材1を無電解コバルトめっき液(図2Aの2)に60℃で10分間浸漬(1段目処理)し、孔側壁の入り口から中央部にかけてコバルト合金膜(拡散防止層)3を形成した。
次いで、無電解コバルトめっき液2に添加剤4(下記表1に記載のアミノ基を有するポリマー)を添加し、1段目処理した上記基材を60℃で30分間浸漬(2段目処理、図2B)し、孔の側壁の中央部から底にかけてコバルト合金膜(拡散防止層)3を形成した。なお、本実施例で用いたアミノ基を有するポリマーは、すべてニットーボーメディカル株式会社製の市販品である。
銅シード層積層処理
2段目処理した上記基材を無電解銅めっき液5に45℃で15分間浸漬し、コバルト合金膜3上に銅シード層6を形成した(図2Cの6)。
コバルト合金膜の膜厚測定
コバルト合金膜形成後の評価基材を孔に対し垂直方向に割断し、コバルト合金膜断面を走査型電子顕微鏡(SEM)を用いて観察し、測長することで膜厚を求めた。また、孔の底における金属合金膜(拡散防止層)の膜厚と孔の入り口における金属合金膜(拡散防止層)の膜厚との比であるステップカバレッジ((S/C)×100%)は下記(1)式に従い求めた。
ステップカバレッジは30%〜300%を合格と判定した。
ステップカバレッジ(%)={孔の底における膜厚(nm)}/{孔の入り口における膜厚(nm)}×100 ・・・(1)
銅シード層成膜確認
拡散防止層(コバルト合金膜)上に銅シード層を積層した後のウェハを孔に対し垂直方向に割断し、走査型電子顕微鏡を用いて、銅の成膜状態およびコバルト合金膜の残存状態を観察した。
無電解コバルトめっき液の代わりに下記の無電解ニッケルめっき液を使用した以外は、実施例1と同様に行った。
無電解ニッケルめっき液
硫酸ニッケル2質量%(0.13mol/L)、錯化剤としてクエン酸4質量%(0.21mol/L)、還元剤としてジメチルアミンボラン0.3質量%(0.05mol/L)を含有し、pH調整剤として水酸化テトラメチルアンモニウムでpH値を8.5の水溶液を調製した。
ニッケル合金膜の膜厚測定
ニッケル合金膜形成後の評価基材を孔に対し垂直方向に割断し、ニッケル合金膜断面を、走査型電子顕微鏡(SEM)を用いて観察し、測長することで膜厚を求めた。
また、孔の底における金属合金膜(拡散防止層)の膜厚と孔の入り口における金属合金膜(拡散防止層)の膜厚との比であるステップカバレッジ((S/C)×100%)を上記(1)式に従い求めた。
ステップカバレッジは30%〜300%を合格と判定した。
銅シード層成膜確認
拡散防止層(ニッケル合金膜)上に銅シード層を積層した後のウェハを孔に対し垂直方向に割断し、走査型電子顕微鏡を用いて、銅の成膜状態およびニッケル合金膜の残存状態を観察した。
無電解コバルトめっき液を用いた2段目処理時に添加剤(アミノ基を有するポリマー)を添加しない以外は、実施例1と同様に行った。表3に無電解めっき処理結果を示す。
無電解コバルトめっき液を用いた2段目処理時の添加剤に、アミノ基を有するポリマー以外のアミン化合物を添加した以外は、実施例1と同様に行った。表4に無電解コバルトめっき液添加剤に各種アミン化合物を添加した際の、コバルト合金膜厚およびステップカバレッジ、銅シード層の成長の有無、銅シード層成膜時のコバルト合金膜の消失の有無を示す。
無電解コバルトめっき液を用いた2段目処理時の添加剤に硫黄系化合物を添加した以外は、実施例1と同様に行った。表5に無電解コバルトめっき液添加剤として硫黄系化合物を添加した際の、コバルト合金膜厚およびステップカバレッジ、銅シード層の成長の有無、銅シード層成膜時のコバルト合金膜の消失の有無を示す。
実施例1の拡散防止層形成において、無電解コバルトめっき処理の1段目処理のみ実施した。使用した評価用基材、コバルトめっき液は実施例1と同様のものを使用した。成膜後の膜厚測定結果を表6に示す。
実施例1の拡散防止層の形成において、無電解コバルトめっき処理の2段目処理のみ実施した。使用した評価用基材、コバルトめっき液は実施例1と同様のものを使用し、表7記載のアミノ基を有するポリマーを添加した。成膜後の膜厚測定結果を表7に示す。
B 拡散防止層形成工程(2段目)
C 銅シード層積層工程
1 評価基板
2 無電解コバルトめっき液または無電解ニッケルめっき液
3 拡散防止層
4 無電解めっき液添加剤
5 無電解銅めっき液
6 銅シード層
Claims (5)
- 貫通電極の形成方法であって、基板に形成された孔の側壁に対し、
(1)少なくともコバルトイオンまたはニッケルイオン、錯化剤、還元剤およびpH調整剤を含有する無電解コバルトめっき液または無電解ニッケルめっき液を用いて、前記孔の入り口から前記孔の中央部に銅に対する拡散防止層である金属合金膜を形成する工程、
(2)少なくともコバルトイオンまたはニッケルイオン、錯化剤、還元剤、pH調整剤およびアミノ基を有するポリマーを含有する無電解コバルトめっき液または無電解ニッケルめっき液を用いて、前記孔の中央部から前記孔の底に拡散防止層である金属合金膜を形成する工程、及び
(3)無電解銅めっき液を用いて、(1)工程及び(2)工程で形成された拡散防止層上に銅シード層を積層する工程を有する、前記貫通電極の形成方法。 - 前記アミノ基を有するポリマーの含有量が、めっき液全量に対して0.0001質量%〜0.02質量%である、請求項1に記載の貫通電極の形成方法。
- 前記アミノ基を有するポリマーが、アリルアミン重合体、ジアリルアミン重合体、または、アリルアミンもしくはジアリルアミンを含む共重合体である、請求項1又は2に記載の貫通電極の形成方法。
- (1)工程および(2)工程で使用するめっき液が、タングステンおよび/またはモリブデンを含有する、請求項1から3のいずれかに記載の貫通電極の形成方法。
- 前記孔の底における金属合金膜の膜厚(S)と、前記孔の入り口における金属合金膜の膜厚(C)との比(ステップカバレッジ(S/C)×100%)が30〜300%である、請求項1から4のいずれかに記載の貫通電極の形成方法。
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