TWI679301B - 緊密層形成方法、緊密層形成系統及記憶媒體 - Google Patents
緊密層形成方法、緊密層形成系統及記憶媒體 Download PDFInfo
- Publication number
- TWI679301B TWI679301B TW105108086A TW105108086A TWI679301B TW I679301 B TWI679301 B TW I679301B TW 105108086 A TW105108086 A TW 105108086A TW 105108086 A TW105108086 A TW 105108086A TW I679301 B TWI679301 B TW I679301B
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- Prior art keywords
- substrate
- coupling agent
- compact layer
- forming
- layer forming
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000000758 substrate Substances 0.000 claims abstract description 167
- 239000007822 coupling agent Substances 0.000 claims abstract description 51
- 230000008569 process Effects 0.000 claims abstract description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 48
- 230000007246 mechanism Effects 0.000 claims description 40
- 238000004140 cleaning Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 9
- 238000007772 electroless plating Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000004590 computer program Methods 0.000 claims description 2
- 230000008878 coupling Effects 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 abstract description 6
- 238000007747 plating Methods 0.000 description 98
- 239000003054 catalyst Substances 0.000 description 69
- 239000010949 copper Substances 0.000 description 44
- 239000007788 liquid Substances 0.000 description 32
- 239000000243 solution Substances 0.000 description 31
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 23
- 239000010408 film Substances 0.000 description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 22
- 229910052710 silicon Inorganic materials 0.000 description 22
- 239000010703 silicon Substances 0.000 description 22
- 239000002105 nanoparticle Substances 0.000 description 16
- 239000006087 Silane Coupling Agent Substances 0.000 description 14
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 10
- 238000005245 sintering Methods 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- 238000009792 diffusion process Methods 0.000 description 8
- 230000006870 function Effects 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 229910052763 palladium Inorganic materials 0.000 description 6
- 239000002270 dispersing agent Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910021332 silicide Inorganic materials 0.000 description 3
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 229920002873 Polyethylenimine Polymers 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002296 dynamic light scattering Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- -1 palladium ions Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 1
- 239000005750 Copper hydroxide Substances 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910018503 SF6 Inorganic materials 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910001956 copper hydroxide Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 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
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- PEVJCYPAFCUXEZ-UHFFFAOYSA-J dicopper;phosphonato phosphate Chemical compound [Cu+2].[Cu+2].[O-]P([O-])(=O)OP([O-])([O-])=O PEVJCYPAFCUXEZ-UHFFFAOYSA-J 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 150000002941 palladium compounds Chemical class 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- NXJCBFBQEVOTOW-UHFFFAOYSA-L palladium(2+);dihydroxide Chemical compound O[Pd]O NXJCBFBQEVOTOW-UHFFFAOYSA-L 0.000 description 1
- 230000009955 peripheral mechanism Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- 238000005406 washing Methods 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
- 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
- C23C18/02—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 thermal decomposition
- C23C18/04—Pretreatment of the material to be coated
-
- H—ELECTRICITY
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- 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
- H01L21/76871—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers
- H01L21/76874—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers for electroless plating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1619—Apparatus for electroless plating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
-
- 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
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- 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
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
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- 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
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67017—Apparatus for fluid treatment
- H01L21/67028—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like
- H01L21/6704—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing
- H01L21/67051—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing using mainly spraying means, e.g. nozzles
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- 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
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- 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
- H01L21/76871—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers
- H01L21/76873—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers for electroplating
-
- 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
- H01L21/76898—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics formed through a semiconductor substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/002—Processes for applying liquids or other fluent materials the substrate being rotated
- B05D1/005—Spin coating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
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Abstract
本發明係一種緊密層形成方法,緊密層形成系統及記憶媒體,其課題為於基板表面,形成薄膜之緊密層。
解決手段為對於基板而言,形成緊密層之緊密層形成方法係具備:使基板(2)旋轉同時,於基板(2)上,供給偶合劑之工程。基板(2)係以300rpm以下之低速進行旋轉,在此狀態,經由IPA而加以稀釋之偶合劑則加以供給至基板(2)上。
Description
本發明係有關對於基板而言形成緊密層之緊密層形成方法,緊密層形成系統及記憶媒體。
近年,LSI等之半導體裝置係欲對應於安裝面積之省空間化或處理速度之改善的課題,而更一層要求高密度化者。作為實現高密度化之技術的一例,知道有經由層積複數之配線基板之時,而製作三次元LSI等之多層基板之多層配線技術。
在多層配線技術中,準備矽基板,於此矽基板或形成於矽基板上之絕緣膜及矽膜等(基板)之凹部上,設置緊密層,而於此緊密層上,藉由觸媒層,作為導電性材料而使用銅(Cu),基板亦埋入Cu於凹部,但此情況,有於凹部內形成Cu擴散防止膜,再於此Cu擴散防止膜上,經由無電解Cu鍍敷而形成晶種膜之必要。因此,有著配線層之配線容積下降,以及於所埋入之Cu中,產生有孔隙之情況。另一方面,加以開發有於基板之凹部內,取代Cu而經由無電解鍍敷法而埋入鎳(Ni)系
金屬,作為配線層(無電解Ni鍍敷層)而使用的技術。
但於矽基板或形成於矽基板上之絕緣膜及矽膜等之上方,藉由緊密層及觸媒層而加以形成之無電解Ni鍍敷層,係成為與矽基板的矽結合而加以作為矽化物者。
如此之情況,矽基板或形成於矽基板上之絕緣膜及矽膜等之上方的緊密層則過度為厚加以形成時,產生有未進行Ni鍍敷層之矽化物化之問題。
〔專利文獻1〕日本特開2010-184113
本發明係考慮如此的點而作為之構成,其目的為提供:於矽基板或形成於矽基板上之絕緣膜及矽膜等之上方,可將為了形成無電解Ni鍍敷層等之鍍敷層的緊密層,呈成為適當的厚度之薄膜地形成者之緊密層形成方法,緊密層形成系統及記憶媒體。
本發明係在對於基板而言,形成無電解鍍敷層形成用的緊密層之緊密層形成方法中,具備準備基板的
工程,和使前述基板上旋轉同時,於前述基板上,供給偶合劑之工程,而在供給前述偶合劑時,將前述基板上保持為濕潤狀態同時,供給以與水有親和性之有機溶劑所稀釋之偶合劑者為特徵之緊密層形成方法。
本發明係在對於基板而言,形成緊密層之緊密層形成系統中,具備旋轉自由地保持基板之基板旋轉保持機構,和於前述基板上供給偶合劑,而於前述基板表面全域,形成緊密層之偶合劑供給部,而前述偶合劑供給部係供給以與水有親和性之有機溶劑所稀釋之偶合劑者為特徵之緊密層形成系統。
本發明係在收納對於緊密層形成系統,為了執行無電解鍍敷層形成用之緊密層形成方法之電腦程式之記憶媒體中,前述緊密層形成方法係具備準備基板的工程,和使前述基板上旋轉同時,於前述基板上,供給偶合劑之工程,而在供給前述偶合劑時,將前述基板上保持為濕潤狀態同時,供給以與水有親和性之有機溶劑所稀釋之偶合劑者為特徵之記憶媒體。
如根據本發明,可於基板上,均一地形成適當厚度之薄膜所成之緊密層者。
2‧‧‧基板
2a‧‧‧凹部
10‧‧‧鍍敷處理系統
11‧‧‧基板搬送機械手臂
12‧‧‧緊密層形成部
13‧‧‧觸媒層形成部
14‧‧‧鍍敷層形成部
15‧‧‧鍍敷層燒結部
15A‧‧‧加熱板
15a‧‧‧密閉套筒
15b‧‧‧排氣口
15c‧‧‧N2氣體供給口
16‧‧‧無電解Cu鍍敷層形成部
17‧‧‧電解Cu鍍敷層形成部
18‧‧‧卡匣站
19‧‧‧控制部
19A‧‧‧記憶媒體
21‧‧‧緊密層
22‧‧‧觸媒層
23‧‧‧鍍敷層
24‧‧‧無電解Cu鍍敷層
25‧‧‧電解Cu鍍敷層
32‧‧‧吐出噴嘴
92‧‧‧噴嘴
104‧‧‧噴嘴頭
圖1係顯示組裝有在本發明之實施形態的緊密層形成系統之鍍敷處理系統全體的方塊圖。
圖2係顯示組裝有在本發明之實施形態的緊密層形成系統之鍍敷處理方法全體的流程圖。
圖3(a)~(f)係顯示加以鍍敷處理方法之基板的圖。
圖4係顯示在本發明之實施形態的緊密層形成方法之工程圖。
圖5係顯示緊密層形成系統之側剖面圖。
圖6係顯示緊密層形成系統之平面圖。
圖7係顯示鍍敷層燒結部之側剖面圖。
經由圖1乃至圖7而對於本發明之一實施形態加以說明。
首先,對於經由圖1而組裝經由本發明之緊密層形成系統之鍍敷處理系統而加以敘述。
如圖1所示,鍍敷處理系統10係對於具有半導體晶圓等之凹部2a的基板(矽基板或形成於矽基板上之絕緣膜及矽膜等)2而言,施以鍍敷處理者(參照圖3(a)~(f))。
如此之鍍敷處理系統10係具備:加以載置有
收納基板2之卡匣(未圖示)之卡匣站18,和自卡匣站18上之卡匣取出基板2而搬送之基板搬送機械手臂11,和基板搬送機械手臂11所運行之運行路徑11a。
另外,於運送路徑11a之一側,加以配置:於基板2上使矽烷偶合劑等之偶合劑吸附,形成本發明之緊密層21之緊密層形成部(緊密層形成系統)12,和使觸媒吸附於基板2之緊密層21上而形成後述之觸媒層22的觸媒層形成部13,和於基板2之觸媒層22上,形成作為後述之Cu擴散防止膜而發揮機能之鍍敷層23之鍍敷層形成部14。
另外,於運行路徑11a之另一側,加以配置有:燒結加以形成於基板2之鍍敷層23之層燒結部15,和於形成於基板2之鍍敷層23上,為了形成作為後述之晶種膜而發揮機能之無電解銅鍍敷層(無電解Cu鍍敷層)24之無電解Cu鍍敷層形成部16。
另外,於鄰接於鍍敷層燒結部15,加以形成於基板2之凹部2a內,加以配置有將無電解Cu鍍敷層24作為晶種膜而為了充填電解銅鍍敷層(電解Cu鍍敷層)25之電解Cu鍍敷層形成部17。
另外,上述之鍍敷處理系統之各構成構件,例如卡匣站18,基板搬送機械手臂11,緊密層形成部(緊密層形成系統)12,觸媒層形成部13,鍍敷層形成部14,鍍敷層燒結部15,無電解Cu鍍敷層形成部16及電解Cu鍍敷層形成部17係均依照記錄於設置在控制部
19之記憶媒體19A的各種程式,由控制部19加以驅動控制,經由此而加以進行對於基板2之各種處理。在此,記憶媒體19A係收納各種之設定資料或後述之鍍敷處理程式等之各種程式。作為記憶媒體19A係可加以使用可由電腦讀取之ROM或RAM等之記憶體,或硬碟,CD-ROM、DVD-ROM或可撓性磁碟等之磁碟狀記憶媒體等之公知的構成。
接著,對於為了形成緊密層21之緊密層形成部(緊密層形成系統)12而更加以敘述。
緊密層形成部12係可自圖5及圖6所示之液處理裝置而構成者。
然而,觸媒層形成部13,鍍敷層形成部14及無電解Cu鍍敷層形成部16,均可自與緊密層形成部12同樣的液處理裝置而構成者。緊密層形成部12係如圖5及圖6所示之構成。
緊密層形成部(緊密層形成系統)12係如圖5及圖6所示,具備:為了在套筒101之內部,旋轉保持基板2之基板旋轉保持機構(基板收容部)110,和供給偶合劑或洗淨液等於基板2表面之液供給機構30,90,和接受自基板2飛散之偶合劑或洗淨液等之杯狀物105,和排出由杯狀物105接受之偶合劑或洗淨液之排出口124,129,134,和排出集中於排出口的液之液排出機構120,125,130,和控制基板旋轉保持機構110,液供給機構30,90,杯狀物105,及液排出機構120,125,130
之控制機構160。
其中,基板旋轉保持機構110係如圖5及圖6所示,具有:在套筒101內延伸於上下之中空筒狀之旋轉軸111,和安裝於旋轉軸111之上端部的旋轉台112,和加以設置於旋轉台112之上面外周部,支持基板2之晶圓夾頭113,和旋轉驅動旋轉軸111之旋轉機構162。其中,旋轉機構162係經由控制機構160而加以控制,再經由旋轉機構162而加以旋轉驅動旋轉軸111,經由此,加以旋轉經由晶圓夾頭113而所支持之基板2。
接著,對於供給偶合劑或洗淨液等於基板2表面之液供給機構30,90,參照圖5及圖6而加以說明。液供給機構30,90係包含:對於基板2之表面而言,藉由噴嘴32而供給矽烷偶合劑之偶合劑供給機構30,和供給洗淨液於基板2之表面的洗淨液供給機構90。
更且,如圖5及圖6所示,噴嘴頭104係加以安裝於機械手臂103之前端部,此機械手臂103係成為可延伸於上下方向,且加以固定於經由旋轉機構165而加以旋轉驅動之支持軸102。另外,對於噴嘴頭104係加以安裝偶合劑供給機構30之噴嘴32,和洗淨液供給機構90之噴嘴92。
洗淨液供給機構90係如上述,包含安裝於噴
嘴頭104之噴嘴92。此情況,自噴嘴92,與水有親和性之有機溶劑,例如異丙醇(IPA)等之洗淨液,或DIW等之清洗處理液之任一則選擇性地加以吐出於基板2之表面。
接著,對於排出自基板2飛散之偶合劑或洗淨液等之液排出機構120,125,130,參照圖5加以說明。如圖5所示,對於套筒101內,係加以配置有經由升降機構164而驅動於上下方向,具有排出口124,129,134之杯狀物105。液排出機構120,125,130係成為排出集中於各排出口124,129,134的液之構成。
如圖5所示,排出偶合劑或洗淨液等之排出機構120,125係各具有經由流路切換器121,126而加以切換之回收流路122,127及廢棄流路123,128。其中,回收流路122,127係為了回收偶合劑或洗淨液等進行再利用之流路,另一方面,廢棄流路123,128係為了廢棄偶合劑或洗淨液等之流路。然而,如圖5所示,對於處理液排出機構130係僅加以設置廢棄流路133。
另外,如圖5及圖6所示,對於基板收容部110之出口側,係加以連接排出偶合劑之偶合劑排出機構120的回收流路122,而此回收流路122之中,對於基板收容部110之出口側附近,加以設置冷卻偶合劑之冷卻緩衝器120A。
接著,對於鍍敷層燒結部15加以敘述。
鍍敷層燒結部15係如圖7所示,具備:加以密閉之密閉套筒15a,和加以配置於密閉套筒15a內部之加熱板15A。
對於鍍敷層燒結部15之密閉套筒15a,係加以設置有為了搬送基板2之搬送口(未圖示),另外,對於密閉套筒15a內係自N2氣體供給口15c而加以供給N2氣體。
同時,密閉套筒15a內係經由排氣口15b而加以排氣,經由以N2氣體充滿在密閉套筒15a內,可將密閉套筒15a內保持為非活性環境者。
接著,對於如此之構成所成之本實施形態的作用,經由圖2乃至圖4而加以說明。
首先,在前工程中,對於半導體晶圓等所成之基板(矽基板或形成於矽基板上之絕緣膜及矽膜等)2而言,加以形成凹部2a,而將加以形成有凹部2a之基板2,加以搬送於鍍敷處理系統10內。
在此,作為形成凹部2a於基板2之方法,係可自以往公知的方法適宜採用者。具體而言,例如,作為乾蝕刻技術,可適用使用氟系或氯系氣體等之泛用技術,但對於特別是形成縱橫比(孔的深度/孔的口徑)之大的孔,係更可適合地採用可高速之深掘蝕刻之ICP-RIE
(Inductively Coupled Plasma Reactive Ion Etching:感應耦合電漿-反應性離子蝕刻)之技術的採用之方法,特別是可適合地採用反覆使用六氟化硫之蝕刻步驟與使用C4F8等之氟系氣體之保護步驟同時進行稱為蝕刻製程之方法。
並且,在鍍敷處理系統10之緊密層形成部12內中,於具有凹部2a之基板2上,加以形成緊密層21(參照圖2及圖3(a))。此情況,在緊密層形成部12內中,於具有凹部2a之基板2上,加以吸附矽烷偶合劑等之偶合劑,如此作為而於基板2上加以形成緊密層21。使矽烷偶合劑吸附而加以形成之緊密層21係使後述之觸媒層22與基板2之緊密性提升之構成。
接著,對於在緊密層形成部12內所進行之緊密層形成方法,經由圖4而更加以詳述。
首先,基板2則於緊密層形成部12之基板旋轉保持機構110上,以乾燥狀態加以載置。之後,如圖5所示,基板2則經由基板旋轉保持機構110而旋轉,其間自噴嘴頭104之噴嘴92,加以供給DIW至基板2上。由如此作為,對於基板2而言施以前洗淨(經由DIW之前洗淨)。
接著,在使基板2旋轉的狀態,自噴嘴頭104之噴嘴92加以供給之液體則被切換,自噴嘴92,取代DIW而加以供給與水有親和性之IPA於基板2上。由如此作為,殘留於基板2上的水則與IPA加以置換(經由IPA之置換)。
接著,在使基板2旋轉的狀態,自噴嘴頭104之噴嘴32,加以供給矽烷偶合劑於基板2上。另外,自噴嘴92,接著加以供給IPA,經由此而使基板2旋轉的同時,成為於此基板2上,加以供給經由IPA所稀釋之矽烷偶合劑者(偶合劑之旋轉塗佈)。
在此偶合劑之旋塗佈中,基板2係經由基板保持機構110,以300rpm以下的低速進行旋轉。另外,自噴嘴32所供給之矽烷偶合劑係經由自噴嘴92所供給之IPA,僅10~1000倍加以稀釋而供給至基板2上。
如上述,基板2係以300rpm以下的低速進行旋轉之同時,於基板2上,加以供給經由IPA而加以10~1000倍稀釋之矽烷偶合劑之故,在基板2上,矽烷偶合劑則於旋轉中加以噴飛而基板2上未產生有乾燥者。另外,矽烷偶合劑係如上述,經由IPA而加以稀釋之故,未有於基板2上,吸附矽烷偶合劑所成之緊密層21的厚度過度變厚者,而可形成適當厚度之薄膜所成之緊密層21。
另外,經由於基板2上形成薄膜所成之緊密層21之時,可確實地使緊密層21緊密於基板上者。另外,如後述,於緊密層21上,藉由觸媒層22而形成Ni或Ni系合金所成之鍍敷層23之情況,緊密層21係因成為薄膜之故,使鍍敷層23之Ni或Ni系合金,與矽基板2反應而可確實地進行Ni或Ni系合金之矽化物化者。
接著,在使基板2旋轉之狀態,加以停止自
噴嘴32之矽烷偶合劑之供給,且加以停止自噴嘴92之IPA的供給。之後,接著自噴嘴92加以供給DIW於基板2上,加以除去殘留於基板2上之多餘的矽烷偶合劑(經由DIW之清洗)。
如以上,自偶合劑供給機構30之噴嘴32加以供給偶合劑,而此偶合劑係經由自洗淨液供給機構90之噴嘴92所供給之IPA而加以稀釋之故,偶合劑供給機構30與洗淨液供給機構90係構成供給經由IPA所稀釋之偶合劑的偶合劑供給部。
在緊密層形成部12中,加以形成有緊密層21之基板2係經由基板搬送機械手臂11而加以傳送至觸媒層形成部13。並且,在觸媒層形成部13中,於基板2之緊密層21上,加以供給例如包含成為觸媒之奈米鈀之觸媒溶液,加以吸附奈米鈀而形成觸媒層22(圖3(b))。此情況,作為觸媒層形成部13,係可使用如圖5及圖6所示之液處理裝置者。
接著,對於加以供給至基板2之觸媒溶液及含於觸媒溶液之觸媒加以說明。首先,對於觸媒加以說明。
作為加以吸附於基板2之緊密層21的觸媒,係適宜採用具有可促進鍍敷反應之觸媒作用之觸媒,但例如,加以使用奈米粒子所成之觸媒。在此,奈米粒子係指具有觸媒作用之膠狀的粒子,平均粒徑為20nm以下、例如成為0.5nm~20nm之範圍內的粒子者。作為構成奈米粒
子之元素,係例如,可舉出鈀,金,白金等。其中,可將奈米粒子的鈀作為n-Pd而表示者。
另外,作為構成奈米粒子之元素,使用釕亦可。
測定奈米粒子的平均粒徑的方法則無加以特別限定,可使用各種方法。例如,測定觸媒溶液內之奈米粒子的平均粒徑之情況,可使用動的光散射法等。動的光散射法係指於分散於觸媒溶液內之奈米粒子,照射雷射光,經由觀察其散射光,而算出奈米粒子的平均粒徑等之方法。
另外,測定吸附於基板2之凹部2a之奈米粒子的平均粒徑之情況,亦可自使用TEM或SEM等所得到之畫像,檢出特定個數之奈米粒子,例如20個奈米粒子,再算出此等奈米粒子粒徑之平均值者。
接著,對於自奈米粒子所成之觸媒所含有觸媒溶液加以說明。觸媒溶液係含有構成成為觸媒之奈米粒子的金屬之離子者。例如,奈米粒子是由鈀加以構成之情況,對於觸媒溶液係作為鈀離子源,而加以含有氯化鈀等之鈀化合物。
觸媒溶液之具體的組成係無特別加以限定,但理想係觸媒溶液之黏性係數則呈成為0.01Pa.s以下地加以設定觸媒溶液之組成。經由將觸媒溶液之黏性係數作為上述範圍內之時,即使基板2之凹部2a的直徑為小之情況,亦可充分地使觸媒溶液滲透至基板2之凹部2a的
下部者。經由此,可更確實地使觸媒吸附至基板2之凹部2a之下部為止者。
理想係觸媒溶液中之觸媒係經由分散劑而加以被覆。經由此,可縮小在觸媒之界面的界面能量者。隨之,認為更可促進在觸媒溶液內之觸媒的擴散,再經由此,更可以短時間而使觸媒到達至基板2之凹部2a之下部為止者。另外,認為可防止複數之觸媒產生凝集而其粒徑變大者,而經由此情況,亦更可促進在觸媒溶液內之觸媒的擴散者。
準備以分散劑所被覆之觸媒的方法則無特別加以限定者。例如,包含預先以分散劑所被覆之觸媒之觸媒溶液,則對於觸媒層形成部13而加以供給亦可。或是將以分散劑而被覆觸媒之工程,呈在觸媒層形成部13之內部實施,加以構成觸媒層形成部13亦可。
作為分散劑係具體而言,聚乙烯基吡咯烷酮(PVP)、聚丙烯酸(PAA)、聚乙烯亞胺(PEI)、四甲胺(TMA)、檸檬酸等為佳。
其他,加以添加為了調整特性之各種藥劑於觸媒溶液亦可。
然而,作為包含觸媒之觸媒溶液,係未加以限定於包含奈米鈀等之奈米粒子的觸媒溶液,而作為觸媒溶液而使用包含由氯化鈀水溶液所代表之鈀離子之水溶液,更且由作為pH調整所得到之氫氧化鈀水溶液,作為觸媒而使用氯化鈀水溶液中的鈀離子亦可。
如此,在觸媒形成部13中,形成觸媒層22於基板2上之後,基板2係經由基板搬送機械手臂11而加以傳送至鍍敷層形成部14。
接著,在鍍敷層形成部14中,於基板2之觸媒層22上,加以形成作為Cu擴散防止膜而發揮機能之鍍敷層23(參照圖3(c))。
此情況,鍍敷層形成部14係如圖5及圖6所示之液處理裝置所成,可於基板2之觸媒層22上,經由施以無電解鍍敷處理而形成鍍敷層23者。
在鍍敷層形成部14中形成鍍敷層23之情況,作為鍍敷液係例如,可使用含有Ni或Ni系合金之鍍敷液,而鍍敷液的溫度係保持為40~75℃。
如此,經由供給鍍敷液於基板2上之時,於基板2之觸媒層22上,經由無電解鍍敷處理,加以形成含有Ni或Ni系合金之鍍敷層23。
接著,加以形成鍍敷層23於觸媒層22上之基板2係經由基板搬送機械手臂11,自鍍敷層形成部14,加以傳送至鍍敷燒結部15之密閉套筒15a內。
並且,在此鍍敷燒結部15之密閉套筒15a內,基板2係為了抑制氧化而在充填有N2氣體之非活性環境中,在加熱板15A上加以加熱。由如此作為,加以燒結基板2之鍍敷層23。
在鍍敷燒結部15中,燒結鍍敷層23時之燒結溫度係成為150~200℃、而燒結時間係成為10~30分。
經由如此燒結基板2上之鍍敷層23,可將鍍敷層23內之水分釋放至外方,同時可提高鍍敷層23內之金屬間結合者。
由如此作為所形成之鍍敷層23係作為Cu擴散防止層而發揮機能。接著,加以形成作為Cu擴散防止層而發揮機能之鍍敷層23之基板2係之後經由基板搬送機械手臂11,而加以傳送至無電解Cu鍍敷層形成部16。
接著,在無電解Cu鍍敷層形成部16中,於基板2之鍍敷層積層體23上,加以形成有作為為了形成電解Cu鍍敷層25之晶種膜而發揮機能之無電解Cu鍍敷層24(參照圖3(d))。
此情況,無電解Cu鍍敷層形成部16係由如圖5及圖6所示之液處理裝置所成,經由施以無電解鍍敷處理於基板2之鍍敷層23上,可形成無電解Cu鍍敷層24。
在無電解Cu鍍敷層形成部16所形成之無電解Cu鍍敷層24係為作為為了形成電解Cu鍍敷層25之晶種膜而發揮機能之構成,對於在無電解Cu鍍敷層形成部16所使用之鍍敷液,係包含有成為銅離子源之銅氯,例如,有硫酸銅,硝酸銅,氯化銅,溴化銅,氧化銅,氫氧化銅,焦磷酸銅等。另外,對於鍍敷液係更含有銅離子之錯合劑及還原劑。另外對於鍍敷液係加以含有為了使鍍敷反應之安定性或速度提升之各種添加劑。
由如此作為,加以形成有無電解Cu鍍敷層
24之基板2係經由基板搬送機械手臂11,而加以傳送至電解Cu鍍敷層形成部17。然而,將加以形成有無電解Cu鍍敷層24之基板2傳送至燒結部15而燒結之後,加以傳送至電解Cu鍍敷層形成部17亦可。接著,在電解Cu鍍敷層形成部17中,對於基板2而言加以施以電解Cu鍍敷處理,於基板2之凹部2a內,將無電解Cu鍍敷層24作為晶種膜而加以充填電解Cu鍍敷層25(參照圖3(e))。
之後,基板2係自鍍敷處理系統10加以排出於外方,加以化學機械研磨基板2之背面側(與凹部2a相反側)((f))。
如以上,根據本實施形態,在緊密層形成部12中,以300rpm以下的低速而使基板2旋轉,再使基板2旋轉的同時,可於基板2上,經由IPA而供給稀釋為10~1000倍之矽烷偶合劑者。因此,可於基板2上,形成適當厚度之薄膜所成之緊密層21者。經由此而可容易地實現緊密層21上之Ni或Ni系合金所成之鍍敷層之矽化物化者。
接著,對於本發明之變形例加以說明。在上述實施形態中,顯示於緊密層21上,藉由觸媒層22而形成Ni或Ni系合金所成之鍍敷層23的例,但取代Ni或Ni系合金而形成包含Co-W-B之鍍敷層23亦可。
Claims (8)
- 一種緊密層形成方法,係對於基板而言,形成無電解鍍敷層形成用的緊密層之緊密層形成方法,其特徵為具備:係對於基板而言,形成緊密層之緊密層形成系統,該緊密層形成系統具備:旋轉自由地保持基板之基板旋轉保持機構,和於前述基板上供給偶合劑,而於前述基板表面全域,形成緊密層之偶合劑供給部;前述偶合劑供給部係供給以與水有親和性之有機溶劑所稀釋之偶合劑者;其中,該緊密層形成方法還具備:準備基板的工程,和使前述基板上旋轉同時,於前述基板上,供給偶合劑之工程;在供給前述偶合劑時,將前述基板上保持為濕潤狀態同時,供給以與水有親和性之有機溶劑所稀釋之偶合劑者。
- 如申請專利範圍第1項記載之緊密層形成方法,其中,在供給前述偶合劑時,以300rpm以下的旋轉數而使前述基板旋轉者。
- 如申請專利範圍第1項或第2項記載之緊密層形成方法,其中,前述偶合劑係經由異丙醇而加以稀釋者。
- 如申請專利範圍第3項記載之緊密層形成方法,其中,前述偶合劑係經由異丙醇而僅10~1000倍加以稀釋者。
- 如申請專利範圍第1項或第2項記載之緊密層形成方法,其中,在供給前述偶合劑之前,以與水有親和性之有機溶劑,預先將前述基板保持為濕潤狀態者。
- 如申請專利範圍第1項或第2項記載之緊密層形成方法,其中,在供給前述偶合劑之後,經由對於前述基板而言施以清洗處理之時,除去多餘之偶合劑者。
- 如申請專利範圍第6項記載之緊密層形成系統,其中,前述基板旋轉保持機構係以300rpm以下的旋轉數而使前述基板旋轉者。
- 一種記憶媒體,係在收納對於緊密層形成系統,為了執行無電解鍍敷層形成用之緊密層形成方法之電腦程式之記憶媒體,其特徵為具備:係對於基板而言,形成緊密層之緊密層形成系統,該緊密層形成系統具備:旋轉自由地保持基板之基板旋轉保持機構,和於前述基板上供給偶合劑,而於前述基板表面全域,形成緊密層之偶合劑供給部;前述偶合劑供給部係供給以與水有親和性之有機溶劑所稀釋之偶合劑者;其中,前述緊密層形成方法係具備:準備基板的工程,和使前述基板上旋轉同時,於前述基板上,供給偶合劑之工程;在供給前述偶合劑時,將前述基板上保持為濕潤狀態同時,供給以與水有親和性之有機溶劑所稀釋之偶合劑者。
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