KR20030027694A - 막형성 방법, 적층막, 절연막 및 반도체용 기판 - Google Patents
막형성 방법, 적층막, 절연막 및 반도체용 기판 Download PDFInfo
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- KR20030027694A KR20030027694A KR1020020057742A KR20020057742A KR20030027694A KR 20030027694 A KR20030027694 A KR 20030027694A KR 1020020057742 A KR1020020057742 A KR 1020020057742A KR 20020057742 A KR20020057742 A KR 20020057742A KR 20030027694 A KR20030027694 A KR 20030027694A
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- INUOIYMEJLOQFN-UHFFFAOYSA-N tributoxy(phenyl)silane Chemical compound CCCCO[Si](OCCCC)(OCCCC)C1=CC=CC=C1 INUOIYMEJLOQFN-UHFFFAOYSA-N 0.000 description 1
- WAAWAIHPWOJHJJ-UHFFFAOYSA-N tributoxy(propyl)silane Chemical compound CCCCO[Si](CCC)(OCCCC)OCCCC WAAWAIHPWOJHJJ-UHFFFAOYSA-N 0.000 description 1
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- JXXQPVMVSMWLGZ-UHFFFAOYSA-N tributoxy(tributoxysilylmethyl)silane Chemical compound CCCCO[Si](OCCCC)(OCCCC)C[Si](OCCCC)(OCCCC)OCCCC JXXQPVMVSMWLGZ-UHFFFAOYSA-N 0.000 description 1
- ZYXLOEAJFSQDQG-UHFFFAOYSA-N tributoxy-(2-tributoxysilylphenyl)silane Chemical compound CCCCO[Si](OCCCC)(OCCCC)C1=CC=CC=C1[Si](OCCCC)(OCCCC)OCCCC ZYXLOEAJFSQDQG-UHFFFAOYSA-N 0.000 description 1
- UYZUVKDKSJFNIN-UHFFFAOYSA-N tributoxy-(3-tributoxysilylphenyl)silane Chemical compound CCCCO[Si](OCCCC)(OCCCC)C1=CC=CC([Si](OCCCC)(OCCCC)OCCCC)=C1 UYZUVKDKSJFNIN-UHFFFAOYSA-N 0.000 description 1
- YBNXDKRALACDIA-UHFFFAOYSA-N tributoxy-(4-tributoxysilylphenyl)silane Chemical compound CCCCO[Si](OCCCC)(OCCCC)C1=CC=C([Si](OCCCC)(OCCCC)OCCCC)C=C1 YBNXDKRALACDIA-UHFFFAOYSA-N 0.000 description 1
- UCSBCWBHZLSFGC-UHFFFAOYSA-N tributoxysilane Chemical compound CCCCO[SiH](OCCCC)OCCCC UCSBCWBHZLSFGC-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- 229960004319 trichloroacetic acid Drugs 0.000 description 1
- ULIAPOFMBCCSPE-UHFFFAOYSA-N tridecan-7-one Chemical compound CCCCCCC(=O)CCCCCC ULIAPOFMBCCSPE-UHFFFAOYSA-N 0.000 description 1
- XVYIJOWQJOQFBG-UHFFFAOYSA-N triethoxy(fluoro)silane Chemical compound CCO[Si](F)(OCC)OCC XVYIJOWQJOQFBG-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 description 1
- HHPPHUYKUOAWJV-UHFFFAOYSA-N triethoxy-[4-(oxiran-2-yl)butyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCCC1CO1 HHPPHUYKUOAWJV-UHFFFAOYSA-N 0.000 description 1
- HPEPIADELDNCED-UHFFFAOYSA-N triethoxysilylmethanol Chemical compound CCO[Si](CO)(OCC)OCC HPEPIADELDNCED-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- KBFAHPBJNNSTGX-UHFFFAOYSA-N trimethoxy-(3-trimethoxysilylphenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC([Si](OC)(OC)OC)=C1 KBFAHPBJNNSTGX-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- LTOKKZDSYQQAHL-UHFFFAOYSA-N trimethoxy-[4-(oxiran-2-yl)butyl]silane Chemical compound CO[Si](OC)(OC)CCCCC1CO1 LTOKKZDSYQQAHL-UHFFFAOYSA-N 0.000 description 1
- SPHALHRGAQVBKI-UHFFFAOYSA-N trimethoxysilylmethanol Chemical compound CO[Si](CO)(OC)OC SPHALHRGAQVBKI-UHFFFAOYSA-N 0.000 description 1
- IJQHYEFNLXHUGV-UHFFFAOYSA-N trimethoxysilylmethyl acetate Chemical compound CO[Si](OC)(OC)COC(C)=O IJQHYEFNLXHUGV-UHFFFAOYSA-N 0.000 description 1
- IXJNGXCZSCHDFE-UHFFFAOYSA-N triphenoxy(phenyl)silane Chemical compound C=1C=CC=CC=1O[Si](C=1C=CC=CC=1)(OC=1C=CC=CC=1)OC1=CC=CC=C1 IXJNGXCZSCHDFE-UHFFFAOYSA-N 0.000 description 1
- AMUIJRKZTXWCEA-UHFFFAOYSA-N triphenoxy(propyl)silane Chemical compound C=1C=CC=CC=1O[Si](OC=1C=CC=CC=1)(CCC)OC1=CC=CC=C1 AMUIJRKZTXWCEA-UHFFFAOYSA-N 0.000 description 1
- MUCRQDBOUNQJFE-UHFFFAOYSA-N triphenoxy(triphenoxysilyl)silane Chemical compound C=1C=CC=CC=1O[Si]([Si](OC=1C=CC=CC=1)(OC=1C=CC=CC=1)OC=1C=CC=CC=1)(OC=1C=CC=CC=1)OC1=CC=CC=C1 MUCRQDBOUNQJFE-UHFFFAOYSA-N 0.000 description 1
- YRUALOZSEADDBR-UHFFFAOYSA-N triphenyl triphenoxysilyl silicate Chemical compound C=1C=CC=CC=1O[Si](O[Si](OC=1C=CC=CC=1)(OC=1C=CC=CC=1)OC=1C=CC=CC=1)(OC=1C=CC=CC=1)OC1=CC=CC=C1 YRUALOZSEADDBR-UHFFFAOYSA-N 0.000 description 1
- PTUUTGJMRQWABQ-UHFFFAOYSA-N triphenyl(phenylsilyloxy)silane Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(C=1C=CC=CC=1)O[SiH2]C1=CC=CC=C1 PTUUTGJMRQWABQ-UHFFFAOYSA-N 0.000 description 1
- VUWVDNLZJXLQPT-UHFFFAOYSA-N tripropoxy(propyl)silane Chemical compound CCCO[Si](CCC)(OCCC)OCCC VUWVDNLZJXLQPT-UHFFFAOYSA-N 0.000 description 1
- BZIXIRYKSIMLOB-UHFFFAOYSA-N tripropoxy(tripropoxysilylmethyl)silane Chemical compound CCCO[Si](OCCC)(OCCC)C[Si](OCCC)(OCCC)OCCC BZIXIRYKSIMLOB-UHFFFAOYSA-N 0.000 description 1
- FOUOZDXPXSKVEL-UHFFFAOYSA-N tripropoxy-(4-tripropoxysilylphenyl)silane Chemical compound CCCO[Si](OCCC)(OCCC)C1=CC=C([Si](OCCC)(OCCC)OCCC)C=C1 FOUOZDXPXSKVEL-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- GBGOZMPAPWGNGR-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-[2-[tris[(2-methylpropan-2-yl)oxy]silyl]ethyl]silane Chemical compound CC(C)(C)O[Si](OC(C)(C)C)(OC(C)(C)C)CC[Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C GBGOZMPAPWGNGR-UHFFFAOYSA-N 0.000 description 1
- NNKMRNUOGTXRCM-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-[3-[tris[(2-methylpropan-2-yl)oxy]silyl]phenyl]silane Chemical compound CC(C)(C)O[Si](OC(C)(C)C)(OC(C)(C)C)C1=CC=CC([Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C)=C1 NNKMRNUOGTXRCM-UHFFFAOYSA-N 0.000 description 1
- PITXUFPLSLHXRV-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-[4-[tris[(2-methylpropan-2-yl)oxy]silyl]phenyl]silane Chemical compound CC(C)(C)O[Si](OC(C)(C)C)(OC(C)(C)C)C1=CC=C([Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C)C=C1 PITXUFPLSLHXRV-UHFFFAOYSA-N 0.000 description 1
- QJJZQRNPNLTSNS-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-[tris[(2-methylpropan-2-yl)oxy]silylmethyl]silane Chemical compound CC(C)(C)O[Si](OC(C)(C)C)(OC(C)(C)C)C[Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C QJJZQRNPNLTSNS-UHFFFAOYSA-N 0.000 description 1
- KGOOITCIBGXHJO-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-phenylsilane Chemical compound CC(C)(C)O[Si](OC(C)(C)C)(OC(C)(C)C)C1=CC=CC=C1 KGOOITCIBGXHJO-UHFFFAOYSA-N 0.000 description 1
- DIZPPYBTFPZSGK-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-propylsilane Chemical compound CCC[Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C DIZPPYBTFPZSGK-UHFFFAOYSA-N 0.000 description 1
- QCKKBOHAYRLMQP-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]silane Chemical compound CC(C)(C)O[SiH](OC(C)(C)C)OC(C)(C)C QCKKBOHAYRLMQP-UHFFFAOYSA-N 0.000 description 1
- XMUJIPOFTAHSOK-UHFFFAOYSA-N undecan-2-ol Chemical compound CCCCCCCCCC(C)O XMUJIPOFTAHSOK-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/312—Organic layers, e.g. photoresist
- H01L21/3121—Layers comprising organo-silicon compounds
- H01L21/3122—Layers comprising organo-silicon compounds layers comprising polysiloxane compounds
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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
- C23C18/12—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 characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—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 characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1212—Zeolites, glasses
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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
- C23C18/12—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 characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—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 characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/122—Inorganic polymers, e.g. silanes, polysilazanes, polysiloxanes
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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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02126—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
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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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02126—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
- H01L21/0214—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC the material being a silicon oxynitride, e.g. SiON or SiON:H
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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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/022—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being a laminate, i.e. composed of sublayers, e.g. stacks of alternating high-k metal oxides
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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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
- H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
- H01L21/02211—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound being a silane, e.g. disilane, methylsilane or chlorosilane
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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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
- H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
- H01L21/02214—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and oxygen
- H01L21/02216—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and oxygen the compound being a molecule comprising at least one silicon-oxygen bond and the compound having hydrogen or an organic group attached to the silicon or oxygen, e.g. a siloxane
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- 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
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
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- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
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- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02337—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a gas or vapour
- H01L21/0234—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a gas or vapour treatment by exposure to a plasma
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- H—ELECTRICITY
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- 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
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02343—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a liquid
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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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02345—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to radiation, e.g. visible light
- H01L21/02348—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to radiation, e.g. visible light treatment by exposure to UV light
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/259—Silicic material
Abstract
(A) 기판에, (A-1) 자외선 조사 처리, 산소 플라즈마 처리, 질소 플라즈마 처리, 헬륨 플라즈마 처리, 아르곤 플라즈마 처리, 수소 플라즈마 처리, 암모니아 플라즈마 처리에서 선택되는 1종 이상의 처리 및 (A-2) 반응성기를 갖는 알콕시실란 화합물 및 그의 가수분해 축합물 또는 그 중 어느 하나의 처리, 또는 그 중 어느 하나의 처리를 행하는 공정, (B) 하기 화학식 1 내지 4로 표시되는 화합물로 이루어지는 군에서 선택된 1종 이상의 화합물, 및 이 화합물을 가수분해, 축합하여 얻어지는 가수분해 축합물 또는 그 중 어느 하나 및 유기 용매를 포함하는 막형성용 조성물을 도포하여 가열하는 공정을 포함하는 것을 특징으로 하는 막형성 방법에 관한 것이다.
식 중, R1은 1가의 유기기이고, R은 불소 원자 또는 1가의 유기기이고, R2는 1가의 유기기이고, a는 1 내지 2의 정수이고, R3은 1가의 유기기이고, R4내지 R7은 동일하거나 또는 상이하며 각각 1가의 유기기이고, b 및 c는 동일하거나 또는 상이하며 0 내지 2의 정수이고, R8은 산소 원자, 페닐렌기 또는 -(CH2)n-으로 표시되는 기 (여기서, n은 1 내지 6의 정수임)이며, d는 0 또는 1을 나타낸다.
또한, 본 발명은 상기 막형성 방법으로 얻어지는 적층막, 이 적층막을 포함하는 포함하는 절연막, 및 이 절연막을 사용한 반도체용 기판에 관한 것이다.
Description
본 발명은 적층막에 관한 것으로, 더욱 상세하게는 반도체 소자 등에 있어서 CVD법으로 형성되는 도포막과의 밀착성이 우수한 반도체용 적층막에 관한 것이다.
종래부터 반도체 소자 등에서의 층간 절연막으로서, CVD법 등의 진공 공정으로 형성된 실리카(SiO2)막이 많이 사용되고 있다. 또한, 최근 보다 균일한 층간 절연막을 형성하기 위해 SOG (Spin on Glass)막이라고 불리우는 테트라알콕시실란의 가수분해 생성물을 주성분으로 하는 도포형 절연막도 사용되고 있다. 또한, 반도체 소자 등의 고집적화에 따라 유기 SOG라고 불리우는 폴리오르가노실록산을 주성분으로 하는 비유전율이 낮은 층간 절연막이 개발되고 있다.
특히, 반도체 소자 등이 한층 더 고집적화 및 다층화됨에 따라 보다 비유전율이 낮은, 바람직하게는 비유전율이 2.5 이하이고, 동시에 기판과의 밀착성이 우수한 층간 절연막 재료가 요구되고 있다.
비유전율이 낮은 재료로서는, 암모니아의 존재하에서 알콕시실란을 축합하여얻어지는 미립자와 알콕시실란의 염기성 부분 가수분해물과의 혼합물로 이루어지는 조성물 (일본 특허 공개 (평)5-263045, (평)5-315319) 및 폴리알콕시실란의 염기성 가수분해물을 암모니아의 존재하에서 축합함으로써 얻어지는 도포액 (일본 특허 공개 (평)11-340219, (평)11-340220)이 제안되어 있지만, 이들 방법으로 얻어지는 재료는 단체 (單體)에서는 기판과의 밀착성이 떨어지거나, 비유전율이 2.5를 초과해 버린다는 문제가 있었다.
본 발명은 상기 문제점을 해결하기 위한 막형성 방법에 관한 것으로, 더욱 상세하게는 반도체 소자 등에서의 층간 절연막으로서, CVD법으로 형성되는 퇴적막과의 밀착성이 우수한 반도체용 절연막을 제공하는 것을 목적으로 한다.
본 발명은 (A) 기판에, (A-1) 자외선 조사 처리, 산소 플라즈마 처리, 질소 플라즈마 처리, 헬륨 플라즈마 처리, 아르곤 플라즈마 처리, 수소 플라즈마 처리, 암모니아 플라즈마 처리에서 선택되는 1종 이상의 처리 및 (A-2) 반응성기를 갖는 알콕시실란 화합물 (이하, "반응성 알콕시실란"이라고 함) 및 그의 가수분해 축합물 또는 그 중 어느 하나의 처리, 또는 그 중 어느 하나의 처리를 행하는 공정, (B) 하기 화학식 1로 표시되는 화합물 (이하, "화합물 (1)"이라고 함), 화학식 2로 표시되는 화합물 (이하, "화합물 (2)"라고 함), 하기 화학식 3으로 표시되는 화합물 (이하, "화합물 (3)"이라고 함) 및 하기 화학식 4로 표시되는 화합물 (이하, "화합물 (4)"라고 함)로 이루어지는 군에서 선택된 1종 이상의 화합물, 및 이 화합물을 가수분해, 축합하여 얻어지는 가수분해 축합물 또는 그 중 어느 하나 및 유기 용매를 포함하는 막형성용 조성물 (이하, "막형성용 조성물"이라고 함)을 도포하여 가열하는 공정을 포함하는 것을 특징으로 하는 막형성 방법을 제공하는 것이다.
<화학식 1>
HSi(OR1)3
<화학식 2>
RaSi(OR2)4-a
<화학식 3>
Si(OR3)4
<화학식 4>
R4 b(R5O)3-bSi-(R8)d-Si(OR6)3-cR7 c
식 중, R1은 1가의 유기기이고, R은 불소 원자 또는 1가의 유기기이고, R2는 1가의 유기기이고, a는 1 내지 2의 정수이고, R3은 1가의 유기기이고, R4내지 R7은 동일하거나 또는 상이하며 각각 1가의 유기기이고, b 및 c는 동일하거나 또는 상이하며 0 내지 2의 정수이고, R8은 산소 원자, 페닐렌기 또는 -(CH2)n-으로 표시되는 기 (여기서, n은 1 내지 6의 정수임)이며, d는 0 또는 1을 나타낸다.
이어서, 본 발명은 상기 막형성 방법으로 얻어지는 적층막에 관한 것이다.
이어서, 본 발명은 상기 적층막을 포함하는 절연막에 관한 것이다.
이어서, 본 발명은 상기 절연막을 사용한 반도체용 기판에 관한 것이다.
(A) 공정
본 발명에서 사용하는 기판은 통상의 반도체 형성에 사용되는 것을 들 수 있으며, 그 표면에 CVD막을 갖는 것이다. 이 CVD막은 Si를 함유하며 동시에 O, C, N, H의 군에서 선택되는 1종 이상의 원소를 더 함유하는 퇴적막이다. 이러한 퇴적막으로서는, 예를 들면 테트라메톡시실란, 테트라에톡시실란, 메틸 트리메톡시실란, 메틸 트리에톡시실란, 디메틸 디메톡시실란, 디메틸 디에톡시실란, 실란, 테트라메틸실란, 트리메틸실란, 디메틸실란, 메틸실란, 에틸실란, 페닐실란, 디페닐실란, 디실라노메탄, 비스(메틸실라노)메탄, 1,2-디실라노에탄, 1,2-비스(메틸실라노)에탄, 2,2-디실라노프로판, 1,3,5-트리실라노-2,4,6-트리메틸렌, 1,3-디메틸디실록산, 1,1,3,3-테트라메틸디실록산, 트리메틸실록산, 1,3-비스(실라노메틸렌)디실록산, 비스(1-메틸디실록사닐)메탄, 2,2-비스(1-메틸디실록사닐)프로판, 2,4,6,8-테트라메틸시클로테트라실록산, 옥타메틸시클로테트라실록산, 2,4,6-트리실란테트라히드로피란, 2,5-디실란테트라히드로푸란, 및 이들의 유도체 등이 사용되며, 산소, 일산화탄소, 이산화탄소, 질소, 아르곤, 물, 오존, 암모니아, N2O 등의 존재하에서 플라즈마 중합한 퇴적막을 사용할 수 있다.
본 발명의 막형성 방법에서는, 상기 CVD막을 설치한 기판을 (A-1) 자외선 조사 처리, 산소 플라즈마 처리, 질소 플라즈마 처리, 헬륨 플라즈마 처리, 아르곤 플라즈마 처리, 수소 플라즈마 처리, 암모니아 플라즈마 처리에서 선택되는 1종 이상의 처리 및 (A-2) 반응성기를 갖는 알콕시실란 화합물, 및 그의 가수분해 축합물 또는 그 중 어느 하나의 처리 또는 그 중 어느 하나의 처리를 행한 후, 막형성용 조성물을 도포 소성하는 것을 특징으로 한다.
(A-1)
자외선 조사 처리로서는 300 nm 이하의 파장, 보다 바람직하게는 200 nm 이하의 광을 기판에 조사하는 것이 바람직하며, 조사 분위기로서는 산소를 함유하는 기체 중에서 행하는 것이 바람직하다. 이 때의 광원 강도는 1 내지 100 mW/㎠, 기판으로의 자외선 조사 시간은 0.5 내지 100초인 것이 바람직하다.
산소 플라즈마 처리, 질소 플라즈마 처리, 헬륨 플라즈마 처리, 아르곤 플라즈마 처리, 수소 플라즈마 처리, 암모니아 플라즈마 처리는 산소, 질소, 헬륨, 아르곤, 수소, 암모니아의 분위기에서 플라즈마 처리를 행하여 기판을 처리할 수 있다. 이 때의 압력은 0.5 내지 500 mTorr, 플라즈마 조건으로서는 50 내지 150 ℃, RF 파워 50 내지 1000 W, 처리 시간 0.1 내지 5 min이다.
상기 CVD막을 설치한 기판을 자외선 조사, 산소 플라즈마 처리, 질소 플라즈마 처리, 헬륨 플라즈마 처리, 아르곤 플라즈마 처리, 수소 플라즈마 처리, 암모니아 플라즈마 처리에서 선택되는 1종 이상의 방법으로 처리함으로써, CVD 기판이 친수성을 띠게 되며 상부에 형성되는 절연막과의 밀착성이 향상된다.
(A-2)
본 발명의 (A-2) 공정에 있어서, 반응성 알콕시실란은 에폭시기, 이소시아네이트기, 비닐기, 수산기, 아세톡시기, 아미노기, 머캅토기 등의 반응성기를 가지며, 그의 가수분해 축합물도 사용할 수 있다.
이러한 반응성 알콕시실란으로서는, 예를 들면 3-글리시독시프로필 트리메톡시실란, 3-글리시독시프로필 트리에톡시실란, 3-글리시독시프로필메틸 디메톡시실란, 3-글리시독시프로필메틸 트리에톡시실란, 2-(3,4-에폭시시클로헥실)에틸 트리메톡시실란, 2-(3,4-에폭시시클로헥실)에틸 트리에톡시실란, 5,6-에폭시헥실 트리메톡시실란, 5,6-에폭시헥실 트리에톡시실란, 3-이소시아네이토프로필 트리메톡시실란, 3-이소시아네이토프로필 트리에톡시실란, 비닐 트리메톡시실란, 비닐 트리에톡시실란, N-[2-(비닐벤질아미노)]-3-아미노프로필 트리메톡시실란, N-[2-(비닐벤질아미노)]-3-아미노프로필 트리에톡시실란, N-(히드록시에틸)-N-메틸아미노프로필 트리메톡시실란, N-(히드록시에틸)-N-메틸아미노프로필 트리에톡시실란, 히드록시메틸 트리메톡시실란, 히드록시메틸 트리에톡시실란, 아세톡시메틸 트리메톡시실란, 아세톡시메틸 트리에톡시실란, 아세톡시프로필 트리메톡시실란, 아세톡시프로필 트리에톡시실란, N-(2-아미노에틸)-3-아미노프로필메틸 디메톡시실란, N-(2-아미노에틸)-3-아미노프로필메틸 디에톡시실란, N-(2-아미노에틸)-3-아미노프로필 트리메톡시실란, N-(2-아미노에틸)-3-아미노프로필 트리에톡시실란, 3-아미노프로필 트리메톡시실란, 3-아미노프로필 트리에톡시실란, N,N'-비스[3-(트리메톡시실릴)프로필]에틸렌디아민, N,N'-비스[3-(트리에톡시실릴)프로필]에틸렌디아민, 3-머캅토프로필 트리메톡시실란, 3-머캅토프로필 트리에톡시실란 등을 들 수 있다.
이들 반응성기를 갖는 알콕시실란 화합물은 2종 이상을 동시에 사용할 수도 있다.
이들 반응성기를 갖는 알콕시실란 화합물로서는, 아미노기를 갖는 알콕시실란 화합물이 특히 바람직하다.
반응성기를 갖는 알콕시실란 화합물 및 그의 가수분해 축합물 또는 그 중 어느 하나를 CVD막을 설치한 기판에 도포하는 방법으로서는, 스핀 코팅법, 침지법, 롤 코팅법, 스프레이법, 스캔 도포법 등의 도포 방법이 이용된다. 이들 도포 방법 중, 스핀 코팅법이 특히 바람직하다.
반응성기를 갖는 알콕시실란 화합물 및 그의 가수분해 축합물 또는 그 중 어느 하나를 도포할 때에는, 필요에 따라 상기 반응성기를 갖는 알콕시실란 화합물 및 그의 가수분해 축합물 또는 그 중 어느 하나를 유기 용매로 희석하여 사용할 수 있다.
유기 용매로서는 알콜계 용매, 케톤계 용매, 아미드계 용매, 에스테르계 용매 및 비양성자계 용매의 군에서 선택된 1종 이상을 들 수 있다.
여기서, 알콜계 용매로서는 메탄올, 에탄올, n-프로판올, i-프로판올, n-부탄올, i-부탄올, sec-부탄올, t-부탄올, n-펜탄올, i-펜탄올, 2-메틸부탄올, sec-펜탄올, t-펜탄올, 3-메톡시부탄올, n-헥산올, 2-메틸펜탄올, sec-헥산올, 2-에틸부탄올, sec-헵탄올, 헵탄올-3, n-옥탄올, 2-에틸헥산올, sec-옥탄올, n-노닐알콜, 2,6-디메틸헵탄올-4, n-데칸올, sec-운데실알콜, 트리메틸노닐알콜, sec-테트라데실알콜, sec-헵타데실알콜, 페놀, 시클로헥산올, 메틸시클로헥산올, 3,3,5-트리메틸시클로헥산올, 벤질알콜, 디아세톤알콜 등의 모노알콜계 용매;
에틸렌글리콜, 1,2-프로필렌글리콜, 1,3-부틸렌글리콜, 펜탄디올-2,4, 2-메틸펜탄디올-2,4, 헥산디올-2,5, 헵탄디올-2,4, 2-에틸헥산디올-1,3, 디에틸렌글리콜, 디프로필렌글리콜, 트리에틸렌글리콜, 트리프로필렌글리콜 등의 다가 알콜계 용매;
에틸렌글리콜 모노메틸에테르, 에틸렌글리콜 모노에틸에테르, 에틸렌글리콜 모노프로필에테르, 에틸렌글리콜 모노부틸에테르, 에틸렌글리콜 모노헥실에테르, 에틸렌글리콜 모노페닐에테르, 에틸렌글리콜 모노-2-에틸부틸에테르, 디에틸렌글리콜 모노메틸에테르, 디에틸렌글리콜 모노에틸에테르, 디에틸렌글리콜 모노프로필에테르, 디에틸렌글리콜 모노부틸에테르, 디에틸렌글리콜 모노헥실에테르, 프로필렌글리콜 모노메틸에테르, 프로필렌글리콜 모노에틸에테르, 프로필렌글리콜 모노프로필에테르, 프로필렌글리콜 모노부틸에테르, 디프로필렌글리콜 모노메틸에테르, 디프로필렌글리콜 모노에틸에테르, 디프로필렌글리콜 모노프로필에테르 등의 다가 알콜 부분 에테르계 용매 등을 들 수 있다.
이들 알콜계 용매는 1종 또는 2종 이상을 동시에 사용할 수도 있다.
케톤계 용매로서는 아세톤, 메틸에틸케톤, 메틸-n-프로필케톤, 메틸-n-부틸케톤, 디에틸케톤, 메틸-i-부틸케톤, 메틸-n-펜틸케톤, 에틸-n-부틸케톤, 메틸-n-헥실케톤, 디-i-부틸케톤, 트리메틸노나논, 시클로헥사논, 2-헥사논, 메틸시클로헥사논, 2,4-펜탄디온, 아세토닐아세톤, 아세토페논, 펜촌 등 외에, 아세틸아세톤, 2,4-헥산디온, 2,4-헵탄디온, 3,5-헵탄디온, 2,4-옥탄디온, 3,5-옥탄디온, 2,4-노난디온, 3,5-노난디온, 5-메틸-2,4-헥산디온, 2,2,6,6-테트라메틸-3,5-헵탄디온, 1,1,1,5,5,5-헥사플루오로-2,4-헵탄디온 등의 β-디케톤류 등을 들 수 있다.
이들 케톤계 용매는 1종 또는 2종 이상을 동시에 사용할 수도 있다.
아미드계 용매로서는 포름아미드, N-메틸포름아미드, N,N-디메틸포름아미드, N-에틸포름아미드, N,N-디에틸포름아미드, 아세트아미드, N-메틸아세트아미드, N,N-디메틸아세트아미드, N-에틸아세트아미드, N,N-디에틸아세트아미드, N-메틸프로피온아미드, N-메틸피롤리돈, N-포르밀모르폴린, N-포르밀피페리딘, N-포르밀피롤리딘, N-아세틸모르폴린, N-아세틸피페리딘, N-아세틸피롤리딘 등을 들 수 있다.
이들 아미드계 용매는 1종 또는 2종 이상을 동시에 사용할 수도 있다.
에스테르계 용매로서는 디에틸카르보네이트, 탄산 에틸렌, 탄산 프로필렌, 탄산 디에틸, 아세트산 메틸, 아세트산 에틸, γ-부티로락톤, γ-발레로락톤, 아세트산 n-프로필, 아세트산 i-프로필, 아세트산 n-부틸, 아세트산 i-부틸, 아세트산 sec-부틸, 아세트산 n-펜틸, 아세트산 sec-펜틸, 아세트산 3-메톡시부틸, 아세트산 메틸펜틸, 아세트산 2-에틸부틸, 아세트산 2-에틸헥실, 아세트산 벤질, 아세트산 시클로헥실, 아세트산 메틸시클로헥실, 아세트산 n-노닐, 아세토아세트산 메틸, 아세토아세트산 에틸, 아세트산 에틸렌글리콜 모노메틸에테르, 아세트산 에틸렌글리콜 모노에틸에테르, 아세트산 디에틸렌글리콜 모노메틸에테르, 아세트산 디에틸렌글리콜 모노에틸에테르, 아세트산 디에틸렌글리콜 모노-n-부틸에테르, 아세트산 프로필렌글리콜 모노메틸에테르, 아세트산 프로필렌글리콜 모노에틸에테르, 아세트산 프로필렌글리콜 모노프로필에테르, 아세트산 프로필렌글리콜 모노부틸에테르, 아세트산 디프로필렌글리콜 모노메틸에테르, 아세트산 디프로필렌글리콜 모노에틸에테르, 디아세트산 글리콜, 아세트산 메톡시트리글리콜, 프로피온산 에틸, 프로피온산 n-부틸, 프로피온산 i-아밀, 옥살산 디에틸, 옥살산 디-n-부틸, 락트산 메틸, 락트산 에틸, 락트산 n-부틸, 락트산 n-아밀, 말론산 디에틸, 프탈산 디메틸, 프탈산 디에틸 등을 들 수 있다.
이들 에스테르계 용매는 1종 또는 2종 이상을 동시에 사용할 수도 있다.
비양성자계 용매로서는 아세토니트릴, 디메틸술폭시드, N,N,N',N'-테트라에틸술파미드, 헥사메틸인산 트리아미드, N-메틸모르폴론, N-메틸피롤, N-에틸피롤, N-메틸-Δ3-피롤린, N-메틸피페리딘, N-에틸피페리딘, N,N-디메틸피페라진, N-메틸이미다졸, N-메틸-4-피페리돈, N-메틸-2-피페리돈, N-메틸-2-피롤리돈, 1,3-디메틸 -2-이미다졸리디논, 1,3-디메틸테트라히드로-2(1H)-피리미디논 등을 들 수 있다.
이들 유기 용매 중에서 특히 하기 화학식 5로 표시되는 유기 용매가 특히 바람직하다.
식 중, R15및 R16은 각각 독립적으로 수소 원자, 탄소수 1 내지 4의 알킬기 또는 CH3CO-로부터 선택되는 1가의 유기기이고, g는 1 내지 2의 정수이다.
이상의 유기 용매는 1종 또는 2종 이상을 혼합하여 사용할 수 있다.
상기 CVD막을 설치한 기판 상에 도포한 상기 반응성기를 갖는 알콕시실란 화합물, 및 그의 가수분해 축합물 또는 그 중 어느 하나를 가열에 의해 건조할 때에는 핫 플레이트, 오븐, 퍼니스 등을 사용할 수 있으며, 가열 분위기로서는 대기하, 질소 분위기하, 아르곤 분위기하, 진공하, 산소 농도를 조절한 감압하 등에서 행할 수 있다. 건조는 통상 60 ℃ 내지 400 ℃, 바람직하게는 60 ℃ 내지 200 ℃이며, 통상 30초 내지 2시간, 바람직하게는 30초 내지 1시간 동안 행해진다.
상기 (A-2) 공정 처리에 의해 CVD막을 설치한 기판 상에 반응성기를 갖는 알콕시실란 화합물, 및 그의 가수분해 축합물 또는 그 중 어느 하나가 통상 200 nm 이하, 바람직하게는 100 nm 이하, 특히 바람직하게는 50 nm 이하로 퇴적된다.
(B) 공정
상기와 같이 처리한 CVD막을 설치한 기판에 막형성용 조성물을 도포할 때에는 스핀 코팅, 침지법, 롤 코팅법, 스프레이법 등의 도장 수단이 이용된다.
이 때의 막 두께는 건조막 두께로서 1회 도포로 두께 0.02 내지 2.5 ㎛ 정도, 2회 도포로 두께 0.04 내지 5.0 ㎛ 정도의 도포막을 형성할 수 있다. 그 후, 상온에서 건조하거나, 또는 80 내지 600 ℃ 정도의 온도에서 통상 5 내지 240분 정도 가열하여 건조함으로써 유리질 또는 거대 고분자의 절연막을 형성할 수 있다.
이 때의 가열 방법으로서는 핫 플레이트, 오븐, 퍼니스 등을 사용할 수 있으며, 가열 분위기로서는 대기하, 질소 분위기, 아르곤 분위기, 진공하, 산소 농도를 조절한 감압하 등에서 행할 수 있다.
또한, 전자선 및 자외선을 조사함으로써 도포막을 형성시킬 수도 있다.
또한, 상기 도포막의 경화 속도를 제어하기 위해 필요에 따라 단계적으로 가열하거나, 질소, 공기, 산소, 감압 등의 분위기를 선택할 수 있다.
본 발명에 있어서, 막형성용 조성물은 상기 화합물 (1) 내지 (4)의 군에서 선택된 1종 이상의 화합물, 및 이 화합물을 가수분해, 축합한 가수분해 축합물 또는 그 중 어느 하나이다.
여기서, 본 발명에서의 가수분해물이란, 상기 화합물 (1) 내지 (4)에 포함되는 R10-기, R2O-기, R3O-기, R5O-기 및 R6O-기 모두가 가수분해되어 있을 필요는 없으며, 예를 들면 1개만 가수분해되어 있는 것, 2개 이상이 가수분해되어 있는 것, 또는 이들의 혼합물일 수도 있다.
또한, 본 발명에서의 가수분해 축합물은 화합물 (1) 내지 (4)의 가수분해물의 실란올기가 축합되어 Si-0-Si 결합을 형성한 것인데, 본 발명에서는 실란올기가 모두 축합되어 있을 필요는 없으며, 약간 일부의 실란올기가 축합된 것, 축합 정도가 상이한 것들의 혼합물 등도 포함한 개념이다.
화합물 (1);
상기 화학식 1에 있어서, R1의 1가의 유기기로서는 알킬기, 아릴기, 알릴기, 글리시딜기 등을 들 수 있다.
여기에서 알킬기로서는 메틸기, 에틸기, 프로필기, 부틸기 등을 들 수 있으며, 바람직하게는 탄소수가 1 내지 5이고, 이들 알킬기는 쇄상 또는 분지되어 있을 수도 있으며, 수소 원자가 불소 원자 등으로 더 치환될 수도 있다.
화학식 1에 있어서, 아릴기로서는 페닐기, 나프틸기, 메틸페닐기, 에틸페닐기, 클로로페닐기, 브로모페닐기, 플루오로페닐기 등을 들 수 있다.
화학식 1로 표시되는 화합물의 구체예로서는, 예를 들면 트리메톡시실란, 트리에톡시실란, 트리-n-프로폭시실란, 트리-iso-프로폭시실란, 트리-n-부톡시실란, 트리-sec-부톡시실란, 트리-tert-부톡시실란, 트리페녹시실란 등을 들 수 있다.
화합물 (1)로서 바람직한 화합물은 트리메톡시실란, 트리에톡시실란, 트리-n-프로폭시실란, 트리-iso-프로폭시실란 등이다.
이들은 1종 또는 2종 이상을 동시에 사용할 수도 있다.
화합물 (2);
상기 화학식 2에 있어서, R 및 R2의 1가의 유기기로서는 알킬기, 아릴기, 알릴기, 글리시딜기 등을 들 수 있다. 또한, 화학식 2에 있어서, R은 1가의 유기기, 특히 알킬기 또는 페닐기인 것이 바람직하다.
여기서, 알킬기로서는 메틸기, 에틸기, 프로필기, 부틸기 등을 들 수 있으며, 바람직하게는 탄소수가 1 내지 5이고, 이들 알킬기는 쇄상 또는 분지되어 있을 수도 있으며, 수소 원자가 불소 원자 등으로 더 치환될 수도 있다.
화학식 2에 있어서, 아릴기로서는 페닐기, 나프틸기, 메틸페닐기, 에틸페닐기, 클로로페닐기, 브로모페닐기, 플루오로페닐기 등을 들 수 있다.
화학식 2로 표시되는 화합물의 구체예로서는, 플루오로 트리메톡시실란, 플루오로 트리에톡시실란, 플루오로 트리-n-프로폭시실란, 플루오로 트리-iso-프로폭시실란, 플루오로 트리-n-부톡시실란, 플루오로 트리-sec-부톡시실란, 플루오로 트리-tert-부톡시실란, 플루오로 트리페녹시실란 등;
메틸 트리메톡시실란, 메틸 트리에톡시실란, 메틸 트리-n-프로폭시실란, 메틸 트리-iso-프로폭시실란, 메틸 트리-n-부톡시실란, 메틸 트리-sec-부톡시실란, 메틸 트리-tert-부톡시실란, 메틸 트리페녹시실란, 에틸 트리메톡시실란, 에틸 트리에톡시실란, 에틸 트리-n-프로폭시실란, 에틸 트리-iso-프로폭시실란, 에틸 트리-n-부톡시실란, 에틸 트리-sec-부톡시실란, 에틸 트리-tert-부톡시실란, 에틸 트리페녹시실란, 비닐 트리메톡시실란, 비닐 트리에톡시실란, 비닐 트리-n-프로폭시실란, 비닐 트리-iso-프로폭시실란, 비닐 트리-n-부톡시실란, 비닐 트리-sec-부톡시실란, 비닐 트리-tert-부톡시실란, 비닐 트리페녹시실란, n-프로필 트리메톡시실란, n-프로필 트리에톡시실란, n-프로필 트리-n-프로폭시실란, n-프로필 트리-iso-프로폭시실란, n-프로필 트리-n-부톡시실란, n-프로필 트리-sec-부톡시실란, n-프로필 트리-tert-부톡시실란, n-프로필 트리페녹시실란, i-프로필 트리메톡시실란, i-프로필 트리에톡시실란, i-프로필 트리-n-프로폭시실란, i-프로필 트리-iso-프로폭시실란, i-프로필 트리-n-부톡시실란, i-프로필 트리-sec-부톡시실란, i-프로필 트리-tert-부톡시실란, i-프로필 트리페녹시실란, n-부틸 트리메톡시실란, n-부틸 트리에톡시실란, n-부틸 트리-n-프로폭시실란, n-부틸 트리-iso-프로폭시실란, n-부틸 트리-n-부톡시실란, n-부틸 트리-sec-부톡시실란, n-부틸 트리-tert-부톡시실란, n-부틸 트리페녹시실란, sec-부틸 트리메톡시실란, sec-부틸 트리에톡시실란, sec-부틸-트리-n-프로폭시실란, sec-부틸-트리-iso-프로폭시실란, sec-부틸-트리-n-부톡시실란, sec-부틸-트리-sec-부톡시실란, sec-부틸-트리-tert-부톡시실란, sec-부틸-트리페녹시실란, t-부틸 트리메톡시실란, t-부틸 트리에톡시실란, t-부틸 트리-n-프로폭시실란, t-부틸 트리-iso-프로폭시실란, t-부틸 트리-n-부톡시실란, t-부틸 트리-sec-부톡시실란, t-부틸 트리-tert-부톡시실란, t-부틸 트리페녹시실란, 페닐 트리메톡시실란, 페닐 트리에톡시실란, 페닐 트리-n-프로폭시실란, 페닐 트리-iso-프로폭시실란, 페닐 트리-n-부톡시실란, 페닐 트리-sec-부톡시실란, 페닐 트리-tert-부톡시실란, 페닐 트리페녹시실란, 비닐 트리메톡시실란, 비닐 트리에톡시실란, γ-아미노프로필 트리메톡시실란, γ-아미노프로필 트리에톡시실란, γ-글리시독시프로필 트리메톡시실란, γ-글리시독시프로필 트리에톡시실란, γ-트리플루오로프로필 트리메톡시실란, γ-트리플루오로프로필 트리에톡시실란 등;
디메틸 디메톡시실란, 디메틸 디에톡시실란, 디메틸-디-n-프로폭시실란, 디메틸-디-iso-프로폭시실란, 디메틸-디-n-부톡시실란, 디메틸-디-sec-부톡시실란, 디메틸-디-tert-부톡시실란, 디메틸 디페녹시실란, 디에틸 디메톡시실란, 디에틸 디에톡시실란, 디에틸-디-n-프로폭시실란, 디에틸-디-iso-프로폭시실란, 디에틸- 디-n-부톡시실란, 디에틸-디-sec-부톡시실란, 디에틸-디-tert-부톡시실란, 디에틸 디페녹시실란, 디-n-프로필 디메톡시실란, 디-n-프로필 디에톡시실란, 디-n-프로필 -디-n-프로폭시실란, 디-n-프로필-디-iso-프로폭시실란, 디-n-프로필-디-n-부톡시실란, 디-n-프로필-디-sec-부톡시실란, 디-n-프로필-디-tert-부톡시실란, 디-n-프로필-디-페녹시실란, 디-iso-프로필 디메톡시실란, 디-iso-프로필 디에톡시실란, 디-iso-프로필-디-n-프로폭시실란, 디-iso-프로필-디-iso-프로폭시실란, 디-iso-프로필-디-n-부톡시실란, 디-iso-프로필-디-sec-부톡시실란, 디-iso-프로필-디- tert-부톡시실란, 디-iso-프로필-디-페녹시실란, 디-n-부틸 디메톡시실란, 디-n-부틸 디에톡시실란, 디-n-부틸-디-n-프로폭시실란, 디-n-부틸-디-iso-프로폭시실란, 디-n-부틸-디-n-부톡시실란, 디-n-부틸-디-sec-부톡시실란, 디-n-부틸-디-tert-부톡시실란, 디-n-부틸-디-페녹시실란, 디-sec-부틸 디메톡시실란, 디-sec-부틸 디에톡시실란, 디-sec-부틸-디-n-프로폭시실란, 디-sec-부틸-디-iso-프로폭시실란, 디- sec-부틸-디-n-부톡시실란, 디-sec-부틸-디-sec-부톡시실란, 디-sec-부틸-디-tert -부톡시실란, 디-sec-부틸-디-페녹시실란, 디-tett-부틸 디메톡시실란, 디-tert-부틸 디에톡시실란, 디-tert-부틸-디-n-프로폭시실란, 디-tert-부틸-디-iso-프로폭시실란, 디-tert-부틸-디-n-부톡시실란, 디-tert-부틸-디-sec-부톡시실란, 디-tert-부틸-디-tert-부톡시실란, 디-tert-부틸-디-페녹시실란, 디페닐 디메톡시실란, 디페닐-디-에톡시실란, 디페닐-디-n-프로폭시실란, 디페닐-디-iso-프로폭시실란, 디페닐-디-n-부톡시실란, 디페닐-디-sec-부톡시실란, 디페닐-디-tert-부톡시실란, 디페닐 디페녹시실란, 디비닐 트리메톡시실란 등을 들 수 있다.
화합물 (2)로서 바람직한 화합물은 메틸 트리메톡시실란, 메틸 트리에톡시실란, 메틸 트리-n-프로폭시실란, 메틸 트리-iso-프로폭시실란, 에틸 트리메톡시실란, 에틸 트리에톡시실란, 비닐 트리메톡시실란, 비닐 트리에톡시실란, 페닐 트리메톡시실란, 페닐 트리에톡시실란, 디메틸 디메톡시실란, 디메틸 디에톡시실란, 디에틸 디메톡시실란, 디에틸 디에톡시실란, 디페닐 디메톡시실란, 디페닐 디에톡시실란 등이다.
이들은 1종 또는 2종 이상을 동시에 사용할 수도 있다.
화합물 (3);
상기 화학식 3에 있어서, R3으로 표시되는 1가의 유기기로서는 상기 화학식 2와 동일한 유기기를 들 수 있다.
화학식 3으로 표시되는 화합물의 구체예로서는, 테트라메톡시실란, 테트라에톡시실란, 테트라-n-프로폭시실란, 테트라-iso-프로폭시실란, 테트라-n-부톡시실란, 테트라-sec-부톡시실란, 테트라-tert-부톡시실란, 테트라페녹시실란 등을 들 수 있다.
화합물 (4);
상기 화학식 4에 있어서, R4내지 R7로 표시되는 1가의 유기기로서는 상기 화학식 2와 동일한 유기기를 들 수 있다.
화학식 4 중 R8이 산소 원자인 화합물로서는 헥사메톡시디실록산, 헥사에톡시디실록산, 헥사페녹시디실록산, 1,1,1,3,3-펜타메톡시-3-메틸디실록산, 1,1,1,3,3-펜타에톡시-3-메틸디실록산, 1,1,1,3,3-펜타페녹시-3-메틸디실록산, 1,1,1,3,3-펜타메톡시-3-에틸디실록산, 1,1,1,3,3-펜타에톡시-3-에틸디실록산, 1,1,1,3,3-펜타페녹시-3-에틸디실록산, 1,1,1,3,3-펜타메톡시-3-페닐디실록산, 1,1,1,3,3-펜타에톡시-3-페닐디실록산, 1,1,1,3,3-펜타페녹시-3-페닐디실록산, 1,1,3,3-테트라메톡시-1,3-디메틸디실록산, 1,1,3,3-테트라에톡시-1,3-디메틸디실록산, 1,1,3,3-테트라페녹시-1,3-디메틸디실록산, 1,1,3,3-테트라메톡시-1,3-디에틸디실록산, 1,1,3,3-테트라에톡시-1,3-디에틸디실록산, 1,1,3,3-테트라페녹시-1,3-디에틸디실록산, 1,1,3,3-테트라메톡시-1,3-디페닐디실록산, 1,1,3,3-테트라에톡시-1,3-디페닐디실록산, 1,1,3,3-테트라페녹시-1,3-디페닐디실록산, 1,1,3-트리메톡시-1,3,3-트리메틸디실록산, 1,1,3-트리에톡시-1,3,3-트리메틸디실록산, 1,1,3 -트리페녹시-1,3,3-트리메틸디실록산, 1,1,3-트리메톡시-1,3,3-트리에틸디실록산, 1,1,3-트리에톡시-1,3,3-트리에틸디실록산, 1,1,3-트리페녹시-1,3,3-트리에틸디실록산, 1,1,3-트리메톡시-1,3,3-트리페닐디실록산, 1,1,3-트리에톡시-1,3,3-트리페닐디실록산, 1,1,3-트리페녹시-1,3,3-트리페닐디실록산, 1,3-디메톡시-1,1,3,3-테트라메틸디실록산, 1,3-디에톡시-1,1,3,3-테트라메틸디실록산, 1,3-디페녹시-1,1,3,3-테트라메틸디실록산, 1,3-디메톡시-1,1,3,3-테트라에틸디실록산, 1,3-디에톡시-1,1,3,3-테트라에틸디실록산, 1,3-디페녹시-1,1,3,3-테트라에틸디실록산, 1,3 -디메톡시-1,1,3,3-테트라페닐디실록산, 1,3-디에톡시-1,1,3,3-테트라페닐디실록산, 1,3-디페녹시-1,1,3,3-테트라페닐디실록산 등을 들 수 있다.
이들 중 헥사메톡시디실록산, 헥사에톡시디실록산, 1,1,3,3-테트라메톡시-1,3-디메틸디실록산, 1,1,3,3-테트라에톡시-1,3-디메틸디실록산, 1,1,3,3-테트라메톡시-1,3-디페닐디실록산, 1,3-디메톡시-1,1,3,3-테트라메틸디실록산, 1,3-디에톡시-1,1,3,3-테트라메틸디실록산, 1,3-디메톡시-1,1,3,3-테트라페닐디실록산, 1,3-디에톡시-1,1,3,3-테트라페닐디실록산 등을 바람직한 예로서 들 수 있다.
또한, 화학식 4에 있어서, d가 0인 화합물로서는 헥사메톡시디실란, 헥사에톡시디실란, 헥사페녹시디실란, 1,1,1,2,2-펜타메톡시-2-메틸디실란, 1,1,1,2,2-펜타에톡시-2-메틸디실란, 1,1,1,2,2-펜타페녹시-2-메틸디실란, 1,1,1,2,2-펜타메톡시-2-에틸디실란, 1,1,1,2,2-펜타에톡시-2-에틸디실란, 1,1,1,2,2-펜타페녹시-2-에틸디실란, 1,1,1,2,2-펜타메톡시-2-페닐디실란, 1,1,1,2,2-펜타에톡시-2-페닐디실란, 1,1,1,2,2-펜타페녹시-2-페닐디실란, 1,1,2,2-테트라메톡시-1,2-디메틸디실란, 1,1,2,2-테트라에톡시-1,2-디에틸디실란, 1,1,2,2-테트라페녹시-1,2-디메틸디실란, 1,1,2,2-테트라메톡시-1,2-디에틸디실란, 1,1,2,2-테트라에톡시-1,2-디에틸디실란, 1,1,2,2-테트라페녹시-1,2-디에틸디실란, 1,1,2,2-테트라메톡시-1,2-디페닐디실란, 1,1,2,2-테트라에톡시-1,2-디페닐디실란, 1,1,2,2-테트라페녹시-1,2-디페닐디실란, 1,1,2-트리메톡시-1,2,2-트리메틸디실란, 1,1,2-트리에톡시-1,2,2-트리메틸디실란, 1,1,2-트리페녹시-1,2,2-트리메틸디실란, 1,1,2-트리메톡시-1,2,2-트리에틸디실란, 1,1,2-트리에톡시-1,2,2-트리에틸디실란, 1,1,2-트리페녹시-1,2,2-트리에틸디실란, 1,1,2-트리메톡시-1,2,2-트리페닐디실란, 1,1,2-트리에톡시-1,2,2-트리페닐디실란, 1,1,2-트리페녹시-1,2,2-트리페닐디실란, 1,2-디메톡시-1,1,2,2-테트라메틸디실란, 1,2-디에톡시-1,1,2,2-테트라메틸디실란, 1,2-디페녹시-1,1,2,2-테트라메틸디실란, 1,2-디메톡시-1,1,2,2-테트라에틸디실란, 1,2-디에톡시-1,1,2,2-테트라에틸디실란, 1,2-디페녹시-1,1,2,2-테트라에틸디실란, 1,2-디메톡시-1,1,2,2-테트라페닐디실란, 1,2-디에톡시-1,1,2,2--테트라페닐디실란, 1,2-디페녹시-1,1,2,2-테트라페닐디실란 등을 들 수 있다.
이들 중 헥사메톡시디실란, 헥사에톡시디실란, 1,1,2,2-테트라메톡시-1,2-디메틸디실란, 1,1,2,2-테트라에톡시-1,2-디메틸디실란, 1,1,2,2-테트라메톡시 -1,2-디페닐디실란, 1,2-디메톡시-1,1,2,2-테트라메틸디실란, 1,2-디에톡시-1,1,2,2-테트라메틸디실란, 1,2-디메톡시-1,1,2,2-테트라페닐디실란, 1,2-디에톡시 -1,1,2,2-테트라페닐디실란 등을 바람직한 예로서 들 수 있다.
또한, 화학식 4에 있어서, R8이 -(CH2)n-으로 표시되는 기의 화합물로서는 비스(트리메톡시실릴)메탄, 비스(트리에톡시실릴)메탄, 비스(트리-n-프로폭시실릴)메탄, 비스(트리-i-프로폭시실릴)메탄, 비스(트리-n-부톡시실릴)메탄, 비스(트리-sec-부톡시실릴)메탄, 비스(트리-t-부톡시실릴)메탄, 1,2-비스(트리메톡시실릴)에탄, 1,2-비스(트리에톡시실릴)에탄, 1,2-비스(트리-n-프로폭시실릴)에탄, 1,2-비스 (트리-i-프로폭시실릴)에탄, 1,2-비스(트리-n-부톡시실릴)에탄, 1,2-비스(트리-sec-부톡시실릴)에탄, 1,2-비스(트리-t-부톡시실릴)에탄, 1-(디메톡시메틸실릴)-1-(트리메톡시실릴)메탄, 1-(디에톡시메틸실릴)-1-(트리에톡시실릴)메탄, 1-(디-n-프로폭시메틸실릴)-1-(트리-n-프로폭시실릴)메탄, 1-(디-i-프로폭시메틸실릴)-1-(트리-i-프로폭시실릴)메탄, 1-(디-n-부톡시메틸실릴)-1-(트리-n-부톡시실릴)메탄, 1-(디-sec-부톡시메틸실릴)-1-(트리-sec-부톡시실릴)메탄, 1-(디-t-부톡시메틸실릴) -1-(트리-t-부톡시실릴)메탄, 1-(디메톡시메틸실릴)-2-(트리메톡시실릴)에탄, 1-(디에톡시메틸실릴)-2-(트리에톡시실릴)에탄, 1-(디-n-프로폭시메틸실릴)-2-(트리-n-프로폭시실릴)에탄, 1-(디-i-프로폭시메틸실릴)-2-(트리-i-프로폭시실릴)에탄, 1-(디-n-부톡시메틸실릴)-2-(트리-n-부톡시실릴)에탄, 1-(디-sec-부톡시메틸실릴) -2-(트리-sec-부톡시실릴)에탄, 1-(디-t-부톡시메틸실릴)-2-(트리-t-부톡시실릴)에탄, 비스(디메톡시메틸실릴)메탄, 비스(디에톡시메틸실릴)메탄, 비스(디-n-프로폭시메틸실릴)메탄, 비스(디-i-프로폭시메틸실릴)메탄, 비스(디-n-부톡시메틸실릴)메탄, 비스(디-sec-부톡시메틸실릴)메탄, 비스(디-t-부톡시메틸실릴)메탄, 1,2-비스(디메톡시메틸실릴)에탄, 1,2-비스(디에톡시메틸실릴)에탄, 1,2-비스(디-n-프로폭시메틸실릴)에탄, 1,2-비스(디-i-프로폭시메틸실릴)에탄, 1,2-비스(디-n-부톡시메틸실릴)에탄, 1,2-비스(디-sec-부톡시메틸실릴)에탄, 1,2-비스(디-t-부톡시메틸실릴)에탄, 1,2-비스(트리메톡시실릴)벤젠, 1,2-비스(트리에톡시실릴)벤젠, 1,2-비스(트리-n-프로폭시실릴)벤젠, 1,2-비스(트리-i-프로폭시실릴)벤젠, 1,2-비스(트리-n-부톡시실릴)벤젠, 1,2-비스(트리-sec-부톡시실릴)벤젠, 1,2-비스(트리-t-부톡시실릴)벤젠, 1,3-비스(트리메톡시실릴)벤젠, 1,3-비스(트리에톡시실릴)벤젠, 1,3-비스(트리-n-프로폭시실릴)벤젠, 1,3-비스(트리-i-프로폭시실릴)벤젠, 1,3-비스(트리-n-부톡시실릴)벤젠, 1,3-비스(트리-sec-부톡시실릴)벤젠, 1,3-비스(트리-t-부톡시실릴)벤젠, 1,4-비스(트리메톡시실릴)벤젠, 1,4-비스(트리에톡시실릴)벤젠, 1,4-비스(트리-n-프로폭시실릴)벤젠, 1,4-비스(트리-i-프로폭시실릴)벤젠, 1,4-비스(트리-n-부톡시실릴)벤젠, 1,4-비스(트리-sec-부톡시실릴)벤젠, 1,4-비스(트리-t-부톡시실릴)벤젠 등을 들 수 있다.
이들 중 비스(트리메톡시실릴)메탄, 비스(트리에톡시실릴)메탄, 1,2-비스(트리메톡시실릴)에탄, 1,2-비스(트리에톡시실릴)에탄, 1-(디메톡시메틸실릴)-1-(트리메톡시실릴)메탄, 1-(디에톡시메틸실릴)-1-(트리에톡시실릴)메탄, 1-(디메톡시메틸실릴)-2-(트리메톡시실릴)에탄, 1-(디에톡시메틸실릴)-2-(트리에톡시실릴)에탄, 비스(디메톡시메틸실릴)메탄, 비스(디에톡시메틸실릴)메탄, 1,2-비스(디메톡시메틸실릴)에탄, 1,2-비스(디에톡시메틸실릴)에탄, 1,2-비스(트리메톡시실릴)벤젠, 1,2-비스(트리에톡시실릴)벤젠, 1,3-비스(트리메톡시실릴)벤젠, 1,3-비스(트리에톡시실릴)벤젠, 1,4-비스(트리메톡시실릴)벤젠, 1,4-비스(트리에톡시실릴)벤젠 등을 바람직한 예로서 들 수 있다.
또한, 상기 화합물 (1) 내지 (4)의 군에서 선택된 1종 이상의 실란 화합물을 가수분해, 축합시킬 때, 화합물 (1) 내지 (4) 1 몰당 0.5 몰 초과 150 몰 이하의 물을 사용하는 것이 바람직하며, 0.5 몰 초과 130 몰의 물을 첨가하는 것이 특히 바람직하다. 첨가하는 물의 양이 0.5 몰 이하이면 도포막의 내균열성이 떨어지는 경우가 있고, 150 몰을 초과하면 가수분해 및 축합 반응 중의 중합체 석출 및 겔화가 발생하는 경우가 있다.
본 발명에 있어서, 상기 화합물 (1) 내지 (4)의 군에서 선택된 1종 이상의 실란 화합물을 가수분해, 축합시킬 때 촉매를 사용한다.
이 때 사용할 수 있는 촉매로서는 금속 킬레이트 화합물, 산 촉매, 알칼리 촉매를 들 수 있다.
금속 킬레이트 화합물로서는, 예를 들면 트리에톡시ㆍ모노(아세틸아세토네이토)티탄, 트리-n-프로폭시ㆍ모노(아세틸아세토네이토)티탄, 트리-i-프로폭시ㆍ모노(아세틸아세토네이토)티탄, 트리-n-부톡시ㆍ모노(아세틸아세토네이토)티탄, 트리-sec-부톡시ㆍ모노(아세틸아세토네이토)티탄, 트리-t-부톡시ㆍ모노(아세틸아세토네이토)티탄, 디에톡시ㆍ비스(아세틸아세토네이토)티탄, 디-n-프로폭시ㆍ비스(아세틸아세토네이토)티탄, 디-i-프로폭시ㆍ비스(아세틸아세토네이토)티탄, 디-n-부톡시ㆍ비스(아세틸아세토네이토)티탄, 디-sec-부톡시ㆍ비스(아세틸아세토네이토)티탄, 디-t-부톡시ㆍ비스(아세틸아세토네이토)티탄, 모노에톡시ㆍ트리스(아세틸아세토네이토)티탄, 모노-n-프로폭시ㆍ트리스(아세틸아세토네이토)티탄, 모노-i-프로폭시ㆍ트리스(아세틸아세토네이토)티탄, 모노-n-부톡시ㆍ트리스(아세틸아세토네이토)티탄, 모노-sec-부톡시ㆍ트리스(아세틸아세토네이토)티탄, 모노-t-부톡시ㆍ트리스(아세틸아세토네이토)티탄, 테트라키스(아세틸아세토네이토)티탄, 트리에톡시ㆍ모노(에틸아세토아세테이트)티탄, 트리-n-프로폭시ㆍ모노(에틸아세토아세테이트)티탄, 트리-i-프로폭시ㆍ모노(에틸아세토아세테이트)티탄, 트리-n-부톡시ㆍ모노(에틸아세토아세테이트)티탄, 트리-sec-부톡시ㆍ모노(에틸아세토아세테이트)티탄, 트리-t-부톡시ㆍ모노(에틸아세토아세테이트)티탄, 디에톡시ㆍ비스(에틸아세토아세테이트)티탄, 디-n-프로폭시ㆍ비스(에틸아세토아세테이트)티탄, 디-i-프로폭시ㆍ비스(에틸아세토아세테이트)티탄, 디-n-부톡시ㆍ비스 (에틸아세토아세테이트)티탄, 디-sec-부톡시ㆍ비스(에틸아세토아세테이트)티탄, 디-t-부톡시ㆍ비스(에틸아세토아세테이트)티탄, 모노에톡시ㆍ트리스(에틸아세토아세테이트)티탄, 모노-n-프로폭시ㆍ트리스(에틸아세토아세테이트)티탄, 모노-i-프로폭시ㆍ트리스(에틸아세토아세테이트)티탄, 모노-n-부톡시ㆍ트리스(에틸아세토아세테이트)티탄, 모노-sec-부톡시ㆍ트리스(에틸아세토아세테이트)티탄, 모노-t-부톡시ㆍ트리스(에틸아세토아세테이트)티탄, 테트라키스(에틸아세토아세테이트)티탄, 모노(아세틸아세토네이토) 트리스(에틸아세토아세테이트)티탄, 비스(아세틸아세토네이토) 비스(에틸아세토아세테이트)티탄, 트리스(아세틸아세토네이토) 모노(에틸아세토아세테이트)티탄 등의 티탄 킬레이트 화합물;
트리에톡시ㆍ모노(아세틸아세토네이토)지르코늄, 트리-n-프로폭시ㆍ모노(아세틸아세토네이토)지르코늄, 트리-i-프로폭시ㆍ모노(아세틸아세토네이토)지르코늄, 트리-n-부톡시ㆍ모노(아세틸아세토네이토)지르코늄, 트리-sec-부톡시ㆍ모노(아세틸아세토네이토)지르코늄, 트리-t-부톡시ㆍ모노(아세틸아세토네이토)지르코늄, 디에톡시ㆍ비스(아세틸아세토네이토)지르코늄, 디-n-프로폭시ㆍ비스(아세틸아세토네이토)지르코늄, 디- i-프로폭시ㆍ비스(아세틸아세토네이토)지르코늄, 디-n-부톡시ㆍ비스(아세틸아세토네이토)지르코늄, 디-sec-부톡시ㆍ비스(아세틸아세토네이토)지르코늄, 디-t-부톡시ㆍ비스 (아세틸아세토네이토)지르코늄, 모노에톡시ㆍ트리스(아세틸아세토네이토)지르코늄, 모노-n-프로폭시ㆍ트리스(아세틸아세토네이토)지르코늄, 모노-i-프로폭시ㆍ트리스(아세틸아세토네이토)지르코늄, 모노-n-부톡시ㆍ트리스(아세틸아세토네이토)지르코늄, 모노-sec-부톡시ㆍ트리스(아세틸아세토네이토)지르코늄, 모노-t-부톡시ㆍ트리스(아세틸아세토네이토)지르코늄, 테트라키스(아세틸아세토네이토)지르코늄, 트리에톡시ㆍ모노(에틸아세토아세테이트)지르코늄, 트리-n-프로폭시ㆍ모노(에틸아세토아세테이트)지르코늄, 트리-i-프로폭시ㆍ모노(에틸아세토아세테이트)지르코늄, 트리-n-부톡시ㆍ모노(에틸아세토아세테이트)지르코늄, 트리-sec-부톡시ㆍ모노(에틸아세토아세테이트)지르코늄, 트리-t-부톡시ㆍ모노(에틸아세토아세테이트)지르코늄, 디에톡시ㆍ비스(에틸아세토아세테이트)지르코늄, 디-n-프로폭시ㆍ비스(에틸아세토아세테이트)지르코늄, 디-i-프로폭시ㆍ비스(에틸아세토아세테이트)지르코늄, 디-n-부톡시ㆍ비스(에틸아세토아세테이트)지르코늄, 디-sec-부톡시ㆍ비스(에틸아세토아세테이트)지르코늄, 디-t-부톡시ㆍ비스(에틸아세토아세테이트)지르코늄, 모노에톡시ㆍ트리스(에틸아세토아세테이트)지르코늄, 모노-n-프로폭시ㆍ트리스(에틸아세토아세테이트)지르코늄, 모노-i-프로폭시ㆍ트리스(에틸아세토아세테이트)지르코늄, 모노-n-부톡시ㆍ트리스(에틸아세토아세테이트)지르코늄, 모노-sec-부톡시ㆍ트리스(에틸아세토아세테이트)지르코늄, 모노-t-부톡시ㆍ트리스(에틸아세토아세테이트)지르코늄, 테트라키스(에틸아세토아세테이트)지르코늄, 모노(아세틸아세토네이토) 트리스(에틸아세토아세테이트)지르코늄, 비스(아세틸아세토네이토) 비스(에틸아세토아세테이트)지르코늄, 트리스(아세틸아세토네이토) 모노(에틸아세토아세테이트)지르코늄 등의 지르코늄 킬레이트 화합물;
트리스(아세틸아세토네이토)알루미늄, 트리스(에틸아세토아세테이트)알루미늄 등의 알루미늄 킬레이트 화합물 등을 들 수 있으며, 바람직하게는 티탄 및(또는) 알루미늄의 킬레이트 화합물, 특히 바람직하게는 티탄의 킬레이트 화합물을 들 수 있다.
이들 금속 킬레이트 화합물은 1종 또는 2종 이상을 동시에 사용할 수도 있다.
산 촉매로서는, 예를 들면 염산, 질산, 황산, 불산, 인산, 붕산, 옥살산 등의 무기산;
아세트산, 프로피온산, 부탄산, 펜탄산, 헥산산, 헵탄산, 옥탄산, 노난산, 데칸산, 옥살산, 말레산, 메틸말론산, 아디프산, 세바크산, 갈산, 부티르산, 멜리트산, 아라키돈산, 시킴산(shikimic acid), 2-에틸헥산산, 올레산, 스테아르산, 리놀산, 리놀레산, 살리실산, 벤조산, p-아미노벤조산, p-톨루엔술폰산, 벤젠술폰산, 모노클로로아세트산, 디클로로아세트산, 트리클로로아세트산, 트리플루오로아세트산, 포름산, 말론산, 술폰산, 프탈산, 푸마르산, 시트르산, 타르타르산, 숙신산, 이타콘산, 메사콘산, 시트라콘산, 말산, 글루타르산의 가수분해물, 말레산 무수물의 가수분해물, 프탈산 무수물의 가수분해물 등의 유기산을 들 수 있으며, 유기산을 보다 바람직한 예로서 들 수 있다.
이들 화합물은 1종 또는 2종 이상을 동시에 사용할 수도 있다.
알칼리 촉매로서는, 예를 들면 수산화나트륨, 수산화칼륨, 수산화리튬, 피리딘, 피롤, 피페라진, 피롤리딘, 피페리딘, 피콜린, 모노에탄올아민, 디에탄올아민, 디메틸 모노에탄올아민, 모노메틸 디에탄올아민, 트리에탄올아민, 디아자비시클로옥탄, 디아자비시클로노난, 디아자비시클로운데센, 테트라메틸암모늄히드록시드, 테트라에틸암모늄히드록시드, 테트라프로필암모늄히드록시드, 테트라부틸암모늄히드록시드, 암모니아, 메틸아민, 에틸아민, 프로필아민, 부틸아민, 펜틸아민, 헥실아민, 펜틸아민, 옥틸아민, 노닐아민, 데실아민, N,N-디메틸아민, N,N-디에틸아민, N,N-디프로필아민, N,N-디부틸아민, 트리메틸아민, 트리에틸아민, 트리프로필아민, 트리부틸아민, 시클로헥실아민, 트리메틸이미딘, 1-아미노-3-메틸부탄, 디메틸글리신 등을 들 수 있으며, 그 중 유기 아민이 보다 바람직하고, 암모니아, 알킬아민 및 테트라메틸암모늄히드록시드가 실리카계막의 기판에 대한 밀착성면에서 특히 바람직하다.
이들 알칼리 촉매는 1종 또는 2종 이상을 동시에 사용할 수도 있다.
상기 촉매의 사용량은, 화합물 (1) 내지 (4) 중의 R10-기, R2O-기, R3O-기, R5O-기 및 R6O-기로 표시되는 기의 총량 1 몰에 대하여 통상 0.00001 내지 10 몰, 바람직하게는 0.00005 내지 5 몰이다. 촉매의 사용량이 상기 범위 내이면, 반응 중의 중합체 석출 및 겔화의 우려가 적다.
이 때, 막형성용 조성물의 반응에는, 비유전율 2.5 이하의 도포막을 쉽게 얻을 수 있다는 관점에서 화합물 (1) 내지 (4)에서 선택되는 화합물의 가수분해시의 촉매가 알칼리 촉매인 것이 바람직하다.
본 발명에서 사용하는 막형성용 조성물은 알콕시실란 가수분해 축합물을 통상 유기 용매에 용해 또는 분산시키며, 필요에 따라 첨가제를 첨가하여 이루어지는 막형성용 조성을 도포하고 가열하여 이루어지는 것이다.
유기 용매로서는 알콜계 용매, 케톤계 용매, 아미드계 용매, 에스테르계 용매 및 비양성자계 용매의 군에서 선택된 1종 이상을 들 수 있다.
이들 유기 용매 중에서 특히 하기 화학식 5로 표시되는 유기 용매가 특히 바람직하다.
<화학식 5>
R15O(CHCH3CH2O)gR16
식 중, R15및 R16은 각각 독립적으로 수소 원자, 탄소수 1 내지 4의 알킬기또는 CH3CO-로부터 선택되는 1가의 유기기이고, g는 1 내지 2의 정수이다.
이상의 유기 용매는 1종 또는 2종 이상을 혼합하여 사용할 수 있다.
본 발명에서 사용하는 막형성용 조성물은, 알콕시실란 가수분해 축합물을 구성하는 화합물 (1) 내지 (4)를 가수분해 및(또는) 축합할 때 동일한 용매를 사용할 수 있다.
구체적으로는 화합물 (1) 내지 (4)를 용해시킨 용매 중에 물 또는 용매로 희석한 물을 비연속적 또는 연속적으로 첨가한다. 이 때, 특정 염기성 화합물은 용매 중에 미리 첨가해 둘 수도 있고, 물 첨가시에 수중에 용해 또는 분산시켜 둘 수도 있다. 이 때의 반응 온도로서는 통상 0 내지 100 ℃, 바람직하게는 15 내지 90 ℃이다.
그 밖의 첨가제
본 발명에서 사용하는 막형성용 조성물에는 콜로이드형 실리카, 유기 중합체, 계면활성제, 실란 커플링제, 라디칼 발생제 등의 성분을 더 첨가할 수도 있다.
유기 중합체로서는, 예를 들면 당쇄 구조를 갖는 화합물, 비닐아미드계 중합체, (메트)아크릴계 중합체, 방향족 비닐 화합물, 덴드리머, 폴리이미드, 폴리아미드산, 폴리아릴렌, 폴리아미드, 폴리퀴녹살린, 폴리옥사디아졸, 불소계 중합체, 폴리알킬렌옥시드 구조를 갖는 화합물 등을 들 수 있다.
계면활성제로서는, 예를 들면 비이온계 계면활성제, 음이온계 계면활성제, 양이온계 계면활성제, 양쪽성 계면활성제 등을 들 수 있으며, 또한 불소계 계면활성제, 실리콘계 계면활성제, 폴리알킬렌옥시드계 계면활성제, 폴리(메트)아크릴레이트계 계면활성제 등을 들 수 있고, 바람직하게는 불소계 계면활성제, 실리콘계 계면활성제를 들 수 있다.
이와 같이 하여 얻어지는 본 발명에서 사용하는 막형성용 조성물의 전체 고형분 농도는 1 내지 30 중량%인 것이 바람직하며, 사용 목적에 따라 적절하게 조정된다. 조성물의 전체 고형분 농도가 1 내지 30 중량%이면, 도포막의 막 두께가 적당한 범위가 되어 보존 안정성도 보다 우수해진다.
또한, 이 전체 고형분 농도의 조정은, 필요하다면 농축 및 상기 유기 용매에 의한 희석에 의해 행할 수 있다.
본 발명의 층간 절연막은 CVD막과의 밀착성이 우수한 점에서 LSI, 시스템 LSI, DRAM, SDRAM, RDRAM, D-RDRAM 등의 반도체 소자용 층간 절연막 및 에칭 스토퍼막, 반도체 소자의 표면 코팅막 등의 보호막, 다층 레지스트를 이용한 반도체 제조 공정의 중간층, 다층 배선 기판의 층간 절연막, 액정 표시 소자용 보호막 및 절연막, 전기 발광 표시 소자용 보호막 및 절연막 등의 용도로 유용하다.
<실시예>
이하, 본 발명을 실시예를 들어 더욱 구체적으로 설명한다. 단, 이하의 기재는 본 발명의 태양예를 개괄적으로 나타내는 것으로, 특별한 이유없이 이들 기재에 의해 본 발명이 한정되는 것은 아니다.
또한, 실시예 및 비교예 중의 "부" 및 "%"는 특별히 기재하지 않는 한, 각각 "중량부" 및 "중량%"를 의미한다.
또한, 각종 평가는 다음과 같이 하여 행하였다.
관성 반경
하기 조건에 의한 겔 투과 크로마토그래피(GPC) (굴절률, 점도, 광산란 측정)법에 의해 측정하였다.
시료 용액: 알콕시실란 가수분해 축합물을 고형분 농도가 0.25 %가 되도록 10 mM의 LiBr을 포함하는 메탄올로 희석하고, GPC (굴절률, 점도, 광산란 측정)용 시료 용액으로 사용하였다.
장치: 도소(주) 제조, GPC 시스템 모델 GPC-8020
도소(주) 제조, 칼럼 Alpha5000/3000
비스코텍사 제조, 점도 검출기 및 광산란 검출기
모델 T-60 듀얼미터
캐리어 용액: 10 mM의 LiBr을 포함하는 메탄올
캐리어 송액 속도: 1 ㎖/min
칼럼 온도: 40 ℃
도포막의 비유전율
8인치 실리콘 웨이퍼 상에 스핀 코팅법을 이용하여 조성물 시료를 도포하고, 핫 플레이트 상에서 80 ℃로 1분간, 질소 분위기에서 200 ℃로 1분간 기판을 건조하였다. 또한, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다. 얻어진 막에 대하여 증착법에 의해 알루미늄 전극 패턴을 형성시켜 비유전율 측정용 샘플을 제조하였다. 이 샘플을 100 kHz의 주파수로 요꼬가와ㆍ휴렛팩커드(주)제조의 HP16451B 전극 및 HP4284A 프리시젼 LCR 미터를 이용하여 CV법에 의해 해당 도포막의 비유전율을 측정하였다.
적층막의 밀착성
적층막을 설치한 기판을 60 ℃의 온수 중에서 50시간 침지하고, 100 ℃의 핫 플레이트에서 10분간 기판을 건조하였다. 얻어진 기판의 최상층에 에폭시 수지를 사용하여 스터드 핀 10개를 고정하고, 150 ℃에서 1시간 건조시켰다. 이 스터드 핀에 대하여 세바스챤법을 이용하여 인취 시험을 행하고, 이하의 기준으로 밀착성을 평가하였다.
○: 스터드 핀 10개 모두 CVD막과 도포막의 계면에서 박리없음
×: CVD막과 도포막의 계면에서 박리 발생
<합성예 1>
석영제 세퍼러블 플라스크에 증류 에탄올 570 g, 이온 교환수 160 g, 10 % 수산화테트라메틸암모늄 수용액 30 g을 넣고 균일하게 교반하였다. 이 용액에 메틸 트리메톡시실란 136 g과 테트라에톡시실란 209 g의 혼합물을 첨가하였다. 용액을 60 ℃로 유지한 채 5시간 동안 반응시켰다. 이 용액에 프로필렌글리콜 모노프로필에테르 300 g을 첨가하고, 그 후, 50 ℃의 증발기를 이용하여 용액을 10 % (완전 가수분해 축합물 환산)가 될 때까지 농축하고, 그 후 아세트산의 10 % 프로필렌글리콜 모노프로필에테르 용액 10 g을 첨가하여 반응액 ①을 얻었다.
이와 같이 하여 얻어진 축합물 등의 관성 반경은 17.8 nm이고, 비유전율은 2.21이었다.
<합성예 2>
석영제 세퍼러블 플라스크에 증류 에탄올 470.9 g, 이온 교환수 226.5 g, 10 % 수산화칼륨 수용액 10.2 g을 넣고 균일하게 교반하였다. 이 용액에 메틸 트리메톡시실란 44.9 g과 테트라에톡시실란 68.6 g의 혼합물을 30분 동안 첨가하였다. 용액을 55 ℃로 유지한 채 2시간 동안 반응시켰다. 이 용액에 20 % 말레산 수용액 80 g을 첨가하여 충분히 교반한 후, 실온까지 냉각하였다. 이 용액에 프로필렌글리콜 모노프로필에테르 400 g을 첨가하고, 그 후, 50 ℃의 증발기를 이용하여 용액을 10 % (완전 가수분해 축합물 환산)가 될 때까지 농축하고, 그 후 말레산의 10 % 프로필렌글리콜 모노프로필에테르 용액 10 g을 첨가하여 반응액 ②를 얻었다.
이와 같이 하여 얻어진 축합물 등의 관성 반경은 23.4 nm이고, 비유전율은 2.11이었다.
<합성예 3>
석영제 세퍼러블 플라스크 중에서 메틸 트리메톡시실란 324.40 g과 트리에톡시실란 123.64 g을 프로필렌글리콜 모노에틸에테르 298 g에 용해시킨 후, 쓰리 원 모터로 교반시키고, 용액 온도를 50 ℃로 안정시켰다. 이어서, 프탈산 0.20 g을 용해시킨 이온 교환수 254 g을 1시간 동안 용액에 첨가하였다. 그 후, 50 ℃에서 3시간 동안 반응시킨 후, 프로필렌글리콜 모노에틸에테르 502 g을 첨가하여 반응액을 실온까지 냉각하였다. 50 ℃에서 반응액으로부터 메탄올과 에탄올을 포함하는 용액 502 g을 증발 제거하고, 반응액 ③을 얻었다.
이와 같이 하여 얻어진 축합물 등의 관성 반경은 0.2 nm이고, 비유전율은 2.72였다.
<합성예 4>
석영제 세퍼러블 플라스크 중에서 증류 트리메톡시실란 77.04 g과 증류 테트라키스(아세틸아세토네이토)티탄 0.48 g을 증류 프로필렌글리콜 모노프로필에테르 290 g에 용해시킨 후, 쓰리 원 모터로 교반시키고, 용액 온도를 60 ℃로 안정시켰다. 이어서, 이온 교환수 84 g을 1시간 동안 용액에 첨가하였다. 그 후, 60 ℃에서 2시간 동안 반응시킨 후, 증류 아세틸아세톤 25 g을 첨가하여 30분간 더 반응시키고, 반응액을 실온까지 냉각하였다. 50 ℃에서 반응액으로부터 메탄올과 물을 포함하는 용액 149 g을 증발 제거하고, 반응액 ④를 얻었다.
이와 같이 하여 얻어진 축합물 등의 관성 반경은 0.3 nm이고, 비유전율은 2.96이었다.
<실시예 1>
8인치 실리콘 웨이퍼 상에 어플라이드 마테리얼(Applied Material) 제조의 Producer S를 이용하여 테트라메틸실란의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (26 원자%), O (3 원자%), C (26 원자%), H (45 원자%)였다.
이 기판에 대하여, 우시오 덴끼 제조의 UVS-4200을 사용하여 10초간 파장 172 nm의 광을 조사하였다. 얻어진 기판 상에 반응액 ①을 5000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 도포막의 계면에서 박리는 확인되지 않았다.
<실시예 2>
8인치 실리콘 웨이퍼 상에 어플라이드 마테리얼 제조의 Producer S를 이용하여 테트라메틸실란의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (26 원자%), O (3 원자%), C (26 원자%), H (45 원자%)였다.
이 기판을 히따찌 세이사꾸쇼 제조의 RE-654X-II 중에 넣고, 챔버 내에 산소 를 도입하여 2 mTorr로 하였다. 이 챔버 내에서 400 W의 플라즈마 처리를 60초간 행하였다. 얻어진 기판 상에 반응액 ②를 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 도포막의 계면에서 박리는 확인되지 않았다.
<실시예 3>
8인치 실리콘 웨이퍼 상에 네벨러스(Nevellus) 제조의 Sequel Express를 이용하여 트리메틸실란의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (25 원자%), O (4 원자%), C (21 원자%), N (14 원자%), H (36 원자%)였다.
이 기판을 히따찌 세이사꾸쇼 제조의 RE-654X-II 중에 넣고, 챔버 내에 질소를 도입하여 2 mTorr로 하였다. 이 챔버 내에서 400 W의 플라즈마 처리를 60초간 행하였다. 얻어진 기판 상에 반응액 ①을 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 도포막의 계면에서 박리는 확인되지 않았다.
<실시예 4>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 실란과 암모니아의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (50 원자%), O (4 원자%), C (3 원자%), N (40 원자%), H (4 원자%)였다.
이 기판을 히따찌 세이사꾸쇼 제조의 RE-654X-II 중에 넣고, 챔버 내에 아르곤을 도입하여 2 mTorr로 하였다. 이 챔버 내에서 400 W의 플라즈마 처리를 60초간 행하였다. 얻어진 기판 상에 반응액 ② 50 g과 반응액 ③ 5 g의 혼합물을 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 도포막의 계면에서 박리는 확인되지 않았다.
<실시예 5>
8인치 실리콘 웨이퍼 상에 어플라이드 마테리얼사 제조의 Producer S를 이용하여 테트라메틸실란의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (26 원자%), O (3 원자%), C (26 원자%), H (45 원자%)였다.
이 기판을 히따찌 세이사꾸쇼 제조의 RE-654X-II 중에 넣고, 챔버 내에 헬륨을 도입하여 2 mTorr로 하였다. 이 챔버 내에서 400 W의 플라즈마 처리를 60초간 행하였다. 얻어진 기판 상에 반응액 ① 30 g과 반응액 ④ 5 g의 혼합물을 5000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하고, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 도포막의 계면에서 박리는 확인되지 않았다.
<실시예 6>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 트리메틸실란의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (25 원자%), O (4 원자%), C (21 원자%), N (14 원자%), H (36 원자%)였다.
이 기판을 히따찌 세이사꾸쇼 제조의 RE-654X-II 중에 넣고, 챔버 내에 수소를 도입하여 2 mTorr로 하였다. 이 챔버 내에서 400 W의 플라즈마 처리를 60초간 행하였다. 얻어진 기판 상에 반응액 ①을 5000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하고, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 도포막의 계면에서 박리는 확인되지 않았다.
<실시예 7>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 트리메틸실란의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (25 원자%), O (4 원자%), C (21 원자%), N (14 원자%), H (36 원자%)였다.
이 기판을 히따찌 세이사꾸쇼 제조의 RE-654X-II 중에 넣고, 챔버 내에 암모니아를 도입하여 2 mTorr로 하였다. 이 챔버 내에서 400 W의 플라즈마 처리를 60초간 행하였다. 얻어진 기판 상에 반응액 ①을 5000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하고, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 도포막의 계면에서 박리는 확인되지 않았다.
<실시예 8>
8인치 실리콘 웨이퍼 상에 어플라이드 마테리얼 제조의 Producer S를 이용하여 테트라에톡시실란의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (32 원자%), O (64 원자%), H (4 원자%)였다.
이 막 위에 3-글리시독시프로필 트리에톡시실란을 농도 2 %로 용해시킨 프로필렌글리콜 모노프로필에테르를 회전수 1500 rpm으로 20초간 도포하고, 이 기판을 80 ℃에서 1분간, 200 ℃에서 1분간 건조하였다. 또한, 이 기판 상에 반응액 ①을 5000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 막의 계면에서 박리는 확인되지 않았다.
<실시예 9>
8인치 실리콘 웨이퍼 상에 어플라이드 마테리얼 제조의 Producer S를 이용하여 테트라메틸실란의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (26 원자%), O (3 원자%), C (26 원자%), H (45 원자%)였다.
이 막 위에 N-[2-(비닐벤질아미노)]-3-아미노프로필 트리메톡시실란을 농도 2 %로 용해시킨 프로필렌글리콜 모노프로필에테르를 회전수 1500 rpm으로 20초간 도포하고, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판 상에 반응액 ②를 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 막의 계면에서 박리는 확인되지 않았다.
<실시예 10>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 트리메틸실란의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (25 원자%), O (4 원자%), C (21 원자%), N (14 원자%), H (36 원자%)였다.
이 막 위에 3-이소시아네이토프로필 트리에톡시실란을 농도 2 %로 용해시킨 프로필렌글리콜 모노프로필에테르를 회전수 1500 rpm으로 20초간 도포하고, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판 상에 반응액 ①을 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 막의 계면에서 박리는 확인되지 않았다.
<실시예 11>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 실란과 암모니아의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (50원자%), O (4 원자%), C (3 원자%), N (40 원자%), H (4 원자%)였다.
이 막 위에 N-(히드록시에틸)-N-메틸프로필 트리메톡시실란을 농도 2 %로 용해시킨 프로필렌글리콜 모노프로필에테르를 회전수 1500 rpm으로 20초간 도포하고, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판 상에 반응액 ②를 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 막의 계면에서 박리는 확인되지 않았다.
<실시예 12>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 트리메틸실란의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (25 원자%), O (4 원자%), C (21 원자%), N (14 원자%), H (36 원자%)였다.
이 막 위에 아세톡시메틸 트리에톡시실란을 농도 2 %로 용해시킨 프로필렌글리콜 모노프로필에테르를 회전수 1500 rpm으로 20초간 도포하고, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판 상에 반응액 ① 20 g과 반응액 ③ 20 g의 혼합액을 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
<실시예 13>
8인치 실리콘 웨이퍼 상에 어플라이드 마테리얼 제조의 Producer S를 이용하여 테트라메틸실란의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (26 원자%), O (3 원자%), C (26 원자%), H (45 원자%)였다.
이 막 위에 N-(2-아미노에틸)-3-아미노프로필 트리메톡시실란을 농도 2 %로 용해시킨 프로필렌글리콜 모노프로필에테르를 회전수 1500 rpm으로 20초간 도포하고, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판 상에 반응액 ② 20 g과 반응액 ④ 20 g의 혼합액을 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 막의 계면에서 박리는 확인되지 않았다.
<실시예 14>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 트리메틸실란의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (25 원자%), O (4 원자%), C (21 원자%), N (14 원자%), H (36 원자%)였다.
이 막 위에 3-머캅토프로필 트리에톡시실란을 농도 2 %로 용해시킨 프로필렌글리콜 모노프로필에테르를 회전수 1500 rpm으로 20초간 도포하고, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판 상에 반응액 ①을 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 막의 계면에서 박리는 확인되지 않았다.
<실시예 15>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 실란과 암모니아의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (50 원자%), O (4 원자%), C (3 원자%), N (40 원자%), H (4 원자%)였다.
이 막 위에 합성예 5에서 얻어진 반응액 ⑤를 회전수 1500 rpm으로 20초간 도포하고, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판 상에 반응액 ①을 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 막의 계면에서 박리는 확인되지 않았다.
<실시예 16>
8인치 실리콘 웨이퍼 상에 네벨러스 제조의 Sequel Express를 이용하여 트리메틸실란의 CVD막을 1000 Å 형성하였다. 이 막의 원소 조성은 Si (25 원자%), O (4 원자%), C (21 원자%), N (14 원자%), H (36 원자%)였다.
이 막 위에 합성예 6에서 얻어진 반응액 ⑥을 회전수 1500 rpm으로 20초간 도포하고, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판 상에 반응액 ②를 4000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 405 ℃의 질소 분위기의 핫 플레이트에서 30분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, CVD막과 막의 계면에서 박리는 확인되지 않았다.
<비교예 1>
8인치 실리콘 웨이퍼 상에 어플라이드 마테리얼 제조의 Producer S를 이용하여 테트라에톡시실란의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (32 원자%), O (64 원자%), H (4 원자%)였다.
이 퇴적막 상에 반응액 ①을 5000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, 스터드 핀 8개에서 CVD막과 도포막 계면에서의 박리가 확인되었다.
<비교예 2>
8인치 실리콘 웨이퍼 상에 어플라이드 마테리얼 제조의 Producer S를 이용하여 테트라에톡시실란의 CVD막을 1000 Å 형성하였다. 이 퇴적막의 원소 조성은 Si (32 원자%), O (64 원자%), H (4 원자%)였다.
이 퇴적막 상에 반응액 ②를 5000 Å 도포한 후, 80 ℃에서 1분간, 200 ℃에서 1분간 기판을 건조하였다. 또한, 이 기판을 430 ℃의 질소 분위기의 퍼니스에서 18분간 소성하였다.
이 적층막의 밀착성을 평가한 결과, 스터드 핀 8개에서 CVD막과 도포막 계면에서의 박리가 확인되었다.
본 발명에 따르면, 기판을 (A-1) 자외선 조사, 산소 플라즈마 처리, 질소 플라즈마 처리, 헬륨 플라즈마 처리, 아르곤 플라즈마 처리, 수소 플라즈마 처리, 암모니아 플라즈마 처리에서 선택되는 1종 이상의 처리, 또는 (A-2) 반응성기를 갖는 알콕시실란 화합물, 및 그의 가수분해 축합물 또는 그 중 어느 하나의 처리 또는 그 중 어느 하나의 처리를 행하는 공정을 수행한 후, 알콕시실란의 가수분해 축합물을 적층하는 막형성 방법을 적용함으로써 CVD막과의 밀착성이 우수한 층간 절연막 (반도체용 기판)을 제공할 수 있다.
Claims (6)
- (A) 기판에, (A-1) 자외선 조사 처리, 산소 플라즈마 처리, 질소 플라즈마 처리, 헬륨 플라즈마 처리, 아르곤 플라즈마 처리, 수소 플라즈마 처리, 암모니아 플라즈마 처리에서 선택되는 1종 이상의 처리 및 (A-2) 반응성기를 갖는 알콕시실란 화합물 및 그의 가수분해 축합물 또는 그 중 어느 하나의 처리, 또는 그 중 어느 하나의 처리를 행하는 공정, (B) 하기 화학식 1 내지 4로 표시되는 화합물로 이루어지는 군에서 선택된 1종 이상의 화합물, 및 이 화합물을 가수분해, 축합하여 얻어지는 가수분해 축합물 또는 그 중 어느 하나 및 유기 용매를 포함하는 막형성용 조성물을 도포하여 가열하는 공정을 포함하는 것을 특징으로 하는 막형성 방법.<화학식 1>HSi(OR1)3<화학식 2>RaSi(OR2)4-a<화학식 3>Si(OR3)4<화학식 4>R4 b(R5O)3-bSi-(R8)d-Si(OR6)3-cR7 c식 중, R1은 1가의 유기기이고, R은 불소 원자 또는 1가의 유기기이고, R2는 1가의 유기기이고, a는 1 내지 2의 정수이고, R3은 1가의 유기기이고, R4내지 R7은 동일하거나 또는 상이하며 각각 1가의 유기기이고, b 및 c는 동일하거나 또는 상이하며 0 내지 2의 정수이고, R8은 산소 원자, 페닐렌기 또는 -(CH2)n-으로 표시되는 기 (여기서, n은 1 내지 6의 정수임)이며, d는 0 또는 1이다.
- 제1항에 있어서, 공정 (A-2)에 있어서 알콕시실란 화합물이 갖는 반응성기가 에폭시기, 이소시아네이트기, 비닐기, 수산기, 아세톡시기, 아미노기, 머캅토기의 군에서 선택되는 1종 이상인 것을 특징으로 하는 막형성 방법.
- 제3항에 있어서, 공정 (B)에 있어서 실란 화합물의 가수분해 축합시의 촉매가 알칼리 촉매인 것을 특징으로 하는 막형성 방법.
- 제1항에 있어서, 기판이 Si를 함유하며, 동시에 O, C, N, H의 군에서 선택되는 1종 이상의 원소를 더 함유하는 CVD (Chemical Vapor Deposition) 퇴적막인 것을 특징으로 하는 막형성 방법.
- 제1항에 기재된 막형성 방법에 의해 얻어지는 절연막.
- 제5항에 기재된 절연막을 사용한 반도체용 기판.
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JP2001307909A JP2003115485A (ja) | 2001-10-03 | 2001-10-03 | 膜形成方法、積層膜、絶縁膜ならびに半導体用基板 |
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EP (1) | EP1296365B1 (ko) |
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EP1670049A4 (en) * | 2003-09-17 | 2008-06-04 | Tokyo Electron Ltd | PREPARATION OF A LOW DIELECTRICITY CONSTANT INSULATION FILM |
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EP1679184A4 (en) * | 2003-10-31 | 2009-02-18 | Jsr Corp | LAMINATE AND METHOD FOR THE PRODUCTION THEREOF, INSULATING FILM, SEMICONDUCTOR DEVICE AND COMPOSITION FOR PRODUCING THE FILM |
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