TW201402496A - 附有含無機微粒子之氧化矽膜的玻璃基板之製造方法 - Google Patents
附有含無機微粒子之氧化矽膜的玻璃基板之製造方法 Download PDFInfo
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- TW201402496A TW201402496A TW102114588A TW102114588A TW201402496A TW 201402496 A TW201402496 A TW 201402496A TW 102114588 A TW102114588 A TW 102114588A TW 102114588 A TW102114588 A TW 102114588A TW 201402496 A TW201402496 A TW 201402496A
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- inorganic fine
- fine particles
- oxide film
- glass substrate
- coating liquid
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- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- JGIATAMCQXIDNZ-UHFFFAOYSA-N calcium sulfide Chemical compound [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 description 1
- 229940023860 canarypox virus HIV vaccine Drugs 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 229960005215 dichloroacetic acid Drugs 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- QQBWQAURZPGDOG-UHFFFAOYSA-N ethyl hexanoate;zinc Chemical compound [Zn].CCCCCC(=O)OCC QQBWQAURZPGDOG-UHFFFAOYSA-N 0.000 description 1
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- YCWSUKQGVSGXJO-NTUHNPAUSA-N nifuroxazide Chemical group C1=CC(O)=CC=C1C(=O)N\N=C\C1=CC=C([N+]([O-])=O)O1 YCWSUKQGVSGXJO-NTUHNPAUSA-N 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- RCYJPSGNXVLIBO-UHFFFAOYSA-N sulfanylidenetitanium Chemical compound [S].[Ti] RCYJPSGNXVLIBO-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 description 1
- LTSUHJWLSNQKIP-UHFFFAOYSA-J tin(iv) bromide Chemical compound Br[Sn](Br)(Br)Br LTSUHJWLSNQKIP-UHFFFAOYSA-J 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- YUOWTJMRMWQJDA-UHFFFAOYSA-J tin(iv) fluoride Chemical compound [F-].[F-].[F-].[F-].[Sn+4] YUOWTJMRMWQJDA-UHFFFAOYSA-J 0.000 description 1
- QPBYLOWPSRZOFX-UHFFFAOYSA-J tin(iv) iodide Chemical compound I[Sn](I)(I)I QPBYLOWPSRZOFX-UHFFFAOYSA-J 0.000 description 1
- UBZYKBZMAMTNKW-UHFFFAOYSA-J titanium tetrabromide Chemical compound Br[Ti](Br)(Br)Br UBZYKBZMAMTNKW-UHFFFAOYSA-J 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 1
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 description 1
- WYKQDEPZMVTTSJ-UHFFFAOYSA-J titanium(4+);tetrabenzoate Chemical compound [Ti+4].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 WYKQDEPZMVTTSJ-UHFFFAOYSA-J 0.000 description 1
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 229940102001 zinc bromide Drugs 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011576 zinc lactate Substances 0.000 description 1
- 229940050168 zinc lactate Drugs 0.000 description 1
- 235000000193 zinc lactate Nutrition 0.000 description 1
- JDLYKQWJXAQNNS-UHFFFAOYSA-L zinc;dibenzoate Chemical compound [Zn+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 JDLYKQWJXAQNNS-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
-
- 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
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
- B05D3/104—Pretreatment of other substrates
-
- 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
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
- B05D3/107—Post-treatment of applied coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
-
- 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
-
- 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
- C23C18/1216—Metal oxides
-
- 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
-
- 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
- C23C18/1225—Deposition of multilayers of inorganic material
-
- 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
- C23C18/1229—Composition of the substrate
- C23C18/1245—Inorganic substrates other than metallic
-
- 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
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
-
- 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
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
- C23C18/127—Preformed particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/048—Encapsulation of modules
-
- 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
- B05D2203/00—Other substrates
- B05D2203/30—Other inorganic substrates, e.g. ceramics, silicon
- B05D2203/35—Glass
-
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Abstract
提供一種附有含無機微粒子之氧化矽膜的玻璃基板之製造方法,其可因應目標光學特性使用期望粒徑的無機微粒子,且無機微粒子的選擇幅度廣。將含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者的塗敷液塗佈於玻璃基板上而形成含無機微粒子之氧化矽膜;或在將熔融玻璃成形為玻璃帶並將玻璃帶徐冷接著切斷來製造玻璃基板時,將含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者的塗敷液塗佈於玻璃帶上而形成含無機微粒子之氧化矽膜。
Description
發明領域
本發明係有關於一種附有含無機微粒子之氧化矽膜的玻璃基板之製造方法。
發明背景
表面具有凹凸之玻璃基板從可使入射光散射一點看來,可作為具有防眩效果之窗玻璃、具有光擷取效果之有機EL元件用玻璃基板、及具有光侷限效果之太陽電池用蓋玻璃等使用。
作為表面具有凹凸之玻璃基板,周知有一種使玻璃基板上之氧化矽膜含有無機微粒子者。作為該玻璃基板之製造方法,例如有提出下述方法。
(1)藉由使用金屬氯化物為原料之熱分解法,於玻璃基板上形成金屬氧化物粒子後進一步形成氧化矽膜之方法(參照專利文獻1)。
(2)於溫度範圍在400~650℃之玻璃基板上塗佈含有有機聚矽氧烷、無機微粒子及液狀介質之塗敷液,而形成含無機微粒子之氧化矽膜之方法(參照專利文獻2)。
專利文獻1:國際公開第03/080530號
專利文獻2:國際公開第2011/155545號
但,在(1)之方法中很難控制金屬氧化物粒子之粒徑。所以,難以製得具有目標光學性能之玻璃基板。
在(2)之方法中,雖可配合目標光學性能使用期望粒徑的無機微粒子,但由於有機聚矽氧烷為非極性,因此塗敷液之液狀介質被侷限在非極性者。所以,無機微粒子也為了避免在非極性液狀介質中凝聚,亦被侷限在已另外施行疏水化等表面處理者。
本發明提供一種附有含無機微粒子之氧化矽膜的玻璃基板之製造方法,其可因應目標光學特性使用期望粒徑的無機微粒子,且無機微粒子的選擇幅度很廣。
本發明係下述[1]、[2]之發明。
[1]一種附有含無機微粒子之氧化矽膜的玻璃基板之製造方法,係將塗敷液塗佈於玻璃基板上而形成含無機微粒子之氧化矽膜者,該塗敷液含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者。以下,該[1]之製造方法亦稱為本發明第1實施態樣之相關方法。
在[1]之發明中,塗佈前述塗敷液時之玻璃基板
溫度以200~650℃為佳。
又,以更於前述含無機微粒子之氧化矽膜上形成折射率與前述無機微粒子相異之金屬氧化物膜為佳。
[2]一種附有含無機微粒子之氧化矽膜的玻璃基
板之製造方法,具有下述步驟:於由熔融玻璃所成形之玻璃帶上塗佈塗敷液而形成含無機微粒子之氧化矽膜之步驟,該塗敷液含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者;及其後將玻璃帶切斷之步驟。
以下,該[2]之製造方法亦稱為關於本發明第2實施態樣之相關方法。
在[2]之發明中,塗佈前述塗敷液時之玻璃帶溫
度以200~650℃為佳。
又,以在浮浴中將熔融玻璃成形為玻璃帶,並在浮浴與徐冷步驟之間或在徐冷步驟中塗佈前述塗敷液為佳。
又,以更於玻璃帶上之前述含無機微粒子之氧化矽膜上,形成折射率與前述無機微粒子相異之金屬氧化物膜為佳。
依據本發明之附有含無機微粒子之氧化矽膜的玻璃基板之製造方法,可使用期望粒徑的無機微粒子,且無機微粒子之選擇幅度較廣。
1‧‧‧附有含無機微粒子之氧化矽膜的玻璃基板
10‧‧‧玻璃基板
12‧‧‧含無機微粒子之氧化矽膜
14‧‧‧無機微粒子
16‧‧‧氧化矽膜
18‧‧‧金屬氧化物膜
20‧‧‧玻璃製造裝置
22‧‧‧熔解窯
24‧‧‧熔融錫
26‧‧‧浮浴
28‧‧‧徐冷窯
30‧‧‧熔融玻璃
32‧‧‧玻璃帶
34‧‧‧第1噴槍
36‧‧‧第2噴槍
圖1係顯示藉由本發明製造方法而製得之附有含無機微粒子之氧化矽膜的玻璃基板一例的概略截面圖。
圖2係顯示藉由本發明製造方法而製得之附有含無機微粒子之氧化矽膜的玻璃基板其他例的概略截面圖。
圖3係顯示玻璃製造裝置一例的概略圖。
本說明書中之(聚)乙二醇表示乙二醇或聚乙二醇。
本說明書中之玻璃基板及玻璃帶之溫度係塗佈塗敷液之側的表面溫度。
本說明書中之折射率係波長550nm之光的折射率。
本說明書中之含無機微粒子之氧化矽膜膜厚係從以掃描型電子顯微鏡觀察附有含無機微粒子之氧化矽膜的玻璃基板截面而得之像進行計測,乃是自玻璃基板上起至無機微粒子頂點為止之距離的平均值。本說明書中之金屬氧化物膜的膜厚係從以掃描型電子顯微鏡觀察具有金屬氧化物膜之附有含無機微粒子之氧化矽膜的玻璃基板截面而得之像進行計測者。
本說明書中之分散液中的平均一次粒徑係藉由動態散射法測定之平均一次粒徑(中值粒徑:50%粒徑)。
<附有含無機微粒子之氧化矽膜的玻璃基板>
圖1係顯示藉由本發明製造方法製得之附有含無機微粒子之氧化矽膜的玻璃基板一例的概略截面圖。附有含無機微粒子之氧化矽膜的玻璃基板1具有玻璃基板10及含無機微粒子之氧化矽膜12,其形成於玻璃基板10表面且表面
具有凹凸。
(玻璃基板)
作為玻璃基板10之材料,可舉如鈉鈣矽玻璃、硼矽酸玻璃、及矽酸鋁玻璃等。
使用附有含無機微粒子之氧化矽膜的玻璃基板1作為有機EL元件用玻璃基板時,作為玻璃基板10以在無鹼玻璃、或鈉鈣矽玻璃已有氧化矽塗覆者為佳。
玻璃基板10亦可為基板本體表面具有功能層者。作為功能層,可舉如底塗層、密著改善層、保護層等。底塗層具有作為鹼阻障層或寬頻帶之低折射率層的功能。作為底塗層,以藉由將含有烷氧矽烷或其水解物(溶膠凝膠矽)之底塗用塗敷液塗佈於基板本體表面而形成之層為佳。
又,在本發明第2實施態樣之相關方法中,在玻璃帶上形成含無機微粒子之氧化矽膜之前,亦可形成如上述之底塗層、密著改善層、保護層等功能層。
(含無機微粒子之氧化矽膜)
含無機微粒子之氧化矽膜12係藉由塗佈後述塗敷液(即第1塗敷液)而形成之膜。具體而言,含無機微粒子之氧化矽膜12係由配置在玻璃基板10表面的複數個無機微粒子14及薄薄地覆蓋在無機微粒子14與玻璃基板10表面的氧化矽膜16構成,且表面具有源自於無機微粒子14形狀的凹凸。含無機微粒子之氧化矽膜12可有效地作為窗玻璃之防眩膜、有機EL元件用玻璃基板之光擷取層、及太陽電池用蓋玻璃之光侷限層使用。
含無機微粒子之氧化矽膜12之厚度在100~
5000nm為佳,且在200~1000nm較佳。含無機微粒子之氧化矽膜12之厚度只要在100nm以上,藉光散射獲致的防眩效果、光擷取效果、及光侷限效果等即佳。含無機微粒子之氧化矽膜12之厚度只要在5000nm以下,製膜時即不會過剩地耗費時間,在生產面上不會產生問題。
玻璃基板10上之無機微粒子14的被覆率在1~
100%為佳,且在5~100%較佳。無機微粒子14之被覆率係無機微粒子14之著膜效率的指標。無機微粒子14之被覆率只要在1%以上,藉光散射獲致的防眩效果、光擷取效果、及光侷限效果等即佳。
無機微粒子14之被覆率係以下述方法求算。
使用接觸段差計,在測定長度1mm下測定含無機微粒子之氧化矽膜12表面的凹凸形狀,並從測定結果抽出存在有無機微粒子14之部分的長度,從下式求算被覆率。
被覆率(%)=100×存在有無機微粒子14之部分的長度(mm)/測定長度(1mm)。
附有含無機微粒子之氧化矽膜的玻璃基板1之霧
度在0.5~100%為佳,且在2~100%較佳。附有含無機微粒子之氧化矽膜的玻璃基板1之霧度係光散射之指標。附有含無機微粒子之氧化矽膜的玻璃基板1之霧度只要在0.5%以上,藉光散射獲致的防眩效果、光擷取效果、及光侷限效果等即佳。
(無機微粒子)
作為無機微粒子14,可舉如金屬氧化物粒子(亦包含複合金屬氧化物粒子)及金屬粒子。因應對附有含無機微粒子之氧化矽膜的玻璃基板1要求之功能,適宜地選擇無機微粒子14之種類即可。
僅考慮光散射的情況下,作為無機微粒子14之材
料,從較廉價一點看來以氧化矽為佳。
加上光散射另對附有含無機微粒子之氧化矽膜的玻璃基板1追加其他功能的情況下,作為無機微粒子14之材料,依功能別可舉如下述者。
紫外線遮蔽:氧化鋅、氧化鈰等。
紅外線遮蔽:氧化銦錫(ITO)、氧化銻錫(ATO)、氧化鎢、鉺等。
抗靜電:ITO、ATO、銀等。
光觸媒:氧化鈦等。
波長轉換:氧化鋅、銪摻雜氧化鋅、硫化鋅、銪摻雜硫化鋅、磷化銦、鉍摻雜硫化鈣、銪摻雜氟化鈣、銪摻雜釩酸釔等。
作為無機微粒子14之形狀,可舉如球狀、粒狀、
棒狀、念珠狀、纖維狀、片狀、中空狀、凝聚物狀、及不定形狀等。無機微粒子14亦可為某一成分被另一成分被覆之核殼型粒子。又,無機微粒子14亦可藉由界面活性劑、高分子分散劑、矽烷耦合劑等進行表面處理。又,無機微粒子14亦可係對400~650℃之熱呈惰性者,亦即在僅使用無機微粒子14之分散液作為塗敷液的情況下不會形成膜、
或是著膜效率顯著低者。
(氧化矽膜)
氧化矽膜16係後述塗敷液中含有之烷氧矽烷之水解物的燒成物,可發揮作為將無機微粒子14固定於玻璃基板10表面的黏結劑之功用。
(金屬氧化物膜)
如圖2顯示,附有含無機微粒子之氧化矽膜的玻璃基板1亦可在含無機微粒子之氧化矽膜12上更具有折射率與無機微粒子14相異之金屬氧化物膜18。金屬氧化物膜18於表面具有源自於無機微粒子14之凹凸。
作為金屬氧化物膜18,可舉如氧化鈦膜(折射
率:2.5)、氧化鋅膜(折射率:2.0)、氧化錫膜(折射率:2.0)、氧化矽膜(折射率:1.5)、及氧化鋁(折射率:1.8)等,作為無機微粒子14使用氧化矽粒子時,從藉光散射獲致之防眩效果、光擷取效果、光侷限效果等可充分發揮之觀點看來,以氧化鈦膜、氧化鋅膜、氧化錫膜為佳。又,將金屬氧化物膜18作成氟摻雜氧化錫(FTO)、銻摻雜氧化錫(ATO)、錫摻雜氧化銦(ITO)、鋁摻雜氧化鋅(AZO)、鎵摻雜氧化鋅(GZO)等透明導電膜,藉此可作成具有光侷限效果之透明導電膜。上述效果可藉由使用折射率比無機微粒子14高的金屬氧化物膜18而有效地發揮。當外部介質為空氣(折射率=1)時,在金屬氧化物膜18之折射率高於無機微粒子14的情況下,散射特性會增加。另一方面,由於在金屬氧化物膜18之折射率低於無機微粒子14的情況下會成為折射率傾斜結
構,因此穿透率會提升。如此一來,藉由使金屬氧化物膜之折射率改變,可依照用途來調整光學特性。
金屬氧化物膜18之厚度在100~5000nm為佳,且
在200~1000nm較佳。金屬氧化物膜18之厚度只要在100nm以上,藉光散射獲致之防眩效果、光擷取效果、光侷限效果等即佳。金屬氧化物膜18之厚度只要在5000nm以下,製膜時即不會耗費過剩的時間,且在生產面上不會產生問題。膜厚係使用掃描型電子顯微鏡(日立先端科技公司製S-4300)進行膜之截面觀察,在面外方向10μm的範圍測定3點的膜厚,並以其平均值而求出。
<附有含無機微粒子之氧化矽膜的玻璃基板之製
造方法>
本發明之附有含無機微粒子之氧化矽膜的玻璃基板之製造方法係將含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者的第1塗敷液,塗佈於玻璃基板或成為玻璃基板之玻璃帶,並將烷氧矽烷之水解物燒成,而於玻璃基板或玻璃帶上形成含無機微粒子之氧化矽膜之方法。
於玻璃帶上形成含無機微粒子之氧化矽膜的情
況下,具體上可舉如具有下述步驟之方法。
即,具有:於由熔融玻璃所成形之玻璃帶上塗佈塗敷液而形成含無機微粒子之氧化矽膜之步驟、及其後將玻璃帶切斷之步驟的方法,該塗敷液含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者。
在本發明之附有含無機微粒子之氧化矽膜的玻
璃基板之製造方法中,亦可於玻璃基板或玻璃帶上之含無機微粒子之氧化矽膜上塗佈第2塗敷液而形成金屬氧化物膜,該第2塗敷液含有折射率與無機微粒子相異之金屬氧化物的前驅物。
(玻璃基板)
作為玻璃基板之材料,可舉如上述者。又,作為玻璃基板方面,在將熔融玻璃成形為玻璃帶並將玻璃帶徐冷再予以切斷來製造玻璃基板的玻璃基板之製造方法中,為了使之適用對玻璃帶塗佈塗敷液而於玻璃帶上形成含無機微粒子之氧化矽膜之方法,以未經強化的生板玻璃基板為佳。
(第1塗敷液)
第1塗敷液係含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者。
(無機微粒子)
無機微粒子係在預先將上述之無機微粒子分散於水或(聚)乙二醇之分散液的狀態下使用。
分散液中之無機微粒子的平均一次粒徑以100~
1000nm為佳,且以300~500nm較佳。分散液中之無機微粒子的平均一次粒徑只要在100~1000nm,即可發揮藉光散射獲致的防眩效果、光擷取效果、及光侷限效果等。
(烷氧矽烷之水解物)
烷氧矽烷之水解物係藉由水及觸媒將烷氧矽烷水解而製得者。烷氧矽烷之水解物亦可含有未反應的烷氧矽烷。
作為烷氧矽烷,可舉如四烷氧矽烷(四甲氧矽
烷、四乙氧矽烷、四丙氧矽烷、四丁氧矽烷等)、單烷基三烷氧矽烷(甲基三甲氧矽烷、甲基三乙氧矽烷、乙基三甲氧矽烷、乙基三乙氧矽烷、丙基三甲氧矽烷、丙基三乙氧矽烷等)、二烷基二烷氧矽烷(二甲基二甲氧矽烷、二甲基二乙氧矽烷、二乙基二甲氧矽烷、二乙基二乙氧矽烷、二丙基二甲氧矽烷、二丙基二乙氧矽烷等)、三烷基單烷氧矽烷(三甲基甲氧矽烷、三甲基乙氧矽烷、三乙基甲氧矽烷、三乙基乙氧矽烷、三丙基甲氧矽烷、三丙基乙氧矽烷等)、單芳基三烷氧矽烷(苯基三甲氧矽烷、苯基三乙氧矽烷等)、二芳基二烷氧矽烷(二苯基二甲氧矽烷、二苯基二乙氧矽烷等)、三芳基單烷氧矽烷(三苯基甲氧矽烷、三苯基乙氧矽烷等)、具全氟聚醚基之烷氧矽烷(全氟聚醚三乙氧矽烷等)、具全氟烷基之烷氧矽烷(全氟乙基三乙氧矽烷等)、具乙烯基之烷氧矽烷(乙烯基三甲氧矽烷、乙烯基三乙氧矽烷等)、具環氧基之烷氧矽烷(2-(3,4-環氧環己基)乙基三甲氧矽烷、3-環氧丙氧基丙基三甲氧矽烷、3-環氧丙氧基丙基甲基二乙氧矽烷、3-環氧丙氧基丙基三乙氧矽烷等)、及具丙烯醯基氧基之烷氧矽烷(3-丙烯醯基氧基丙基三甲氧矽烷等)等。
作為烷氧矽烷,從水解速度快且生產性高等之觀
點看來,以四烷氧矽烷為佳,且以四乙氧矽烷、四甲氧矽烷較佳。
烷氧矽烷之水解係使用水及作為觸媒的酸或鹼
進行。以酸而言,可舉如無機酸(硝酸、硫酸、鹽酸等)、及
有機酸(甲酸、草酸、酒石酸、檸檬酸、單氯乙酸、二氯乙酸、三氯乙酸等)。以鹼而言可舉如氨、氫氧化鈉、及氫氧化鉀等。作為觸媒,從長期保存性之觀點看來,以酸為佳,又,作為觸媒以不會妨礙無機微粒子之分散者為佳。
(液狀介質)
作為第1塗敷液之液狀介質係使用水及(聚)乙二醇中之任一者或兩者。使用水及(聚)乙二醇以外之液狀介質時,含無機微粒子之氧化矽膜不會著膜於玻璃基板上或含無機微粒子之氧化矽膜的著膜效率顯著降低。
作為第1塗敷液之液狀介質,從烷氧矽烷之水解
需要水一點看來,以僅只水或水與(聚)乙二醇之混合物為佳。又,從含無機微粒子之氧化矽膜的著膜效率佳之觀點看來,以(聚)乙二醇與所需最小限度之水的混合物尤佳。
作為(聚)乙二醇,可舉如乙二醇、二乙二醇、三
乙二醇、四乙二醇、及分子量300以下之聚乙二醇等,從含無機微粒子之氧化矽膜的著膜效率佳之觀點看來,以三乙二醇、四乙二醇為佳,且以四乙二醇尤佳。
第1塗敷液可在不損及本發明效果之範圍內含有
水及(聚)乙二醇以外之液狀介質。
(第1塗敷液之組成)
從含無機微粒子之氧化矽膜的著膜效率及第1塗敷液之黏度(處理性)的觀點看來,第1塗敷液之固體成分濃度(第1塗敷液中之無機微粒子及烷氧矽烷之水解物的合計濃度)以0.3~70質量%為佳,且以3~25質量%較佳。
在第1塗敷液之固體成分(第1塗敷液中之無機微
粒子及烷氧矽烷之水解物的合計)100質量%中,無機微粒子之比率佔1~60質量%為佳,且以佔3~30質量%較佳。無機微粒子之比率只要在1質量%以上,即可充分地發揮源自於無機微粒子之功能。無機微粒子之比率只要在60質量%以下,即可抑制無機微粒子凝聚而製得無機微粒子均勻分散之膜。
在第1塗敷液之固體成分(第1塗敷液中之無機微
粒子及烷氧矽烷之水解物的合計)100質量%中,烷氧矽烷之水解物(SiO2換算固體成分)之比率佔40~99質量%為佳,且以佔70~97質量%較佳。烷氧矽烷之水解物之比率只要在40質量%以上,即可使無機微粒子以高效率進行著膜。烷氧矽烷之水解物的比率只要在99質量%以下,即可充分地發揮源自於無機微粒子之功能。
(第1塗敷液之塗佈)
作為第1塗敷液之塗佈方法,從可生產效率良好地製造附有含無機微粒子之氧化矽膜的玻璃基板之觀點看來,以使用噴嘴(例如噴槍等)來噴霧第1塗敷液的噴霧法為佳。
作為噴霧法的具體塗佈方法,可舉如下述方法(i)、(ii)、(iii)等,從步驟數少且可以較佳的生產效率來製造附有含無機微粒子之氧化矽膜的玻璃基板之觀點看來,以方法(ii)為佳。
(i)在經固定之玻璃基板上方一邊使噴嘴移動一
邊從噴嘴對玻璃基板噴霧第1塗敷液之方法。
(ii)從噴嘴對朝一方向移動中的玻璃帶噴霧第1塗敷液之方法。
(iii)在移動中的玻璃基板上方,一邊使噴嘴移動一邊從噴嘴對玻璃基板噴霧第1塗敷液;或將噴嘴固定而從噴嘴對玻璃基板噴霧第1塗敷液之方法。
塗佈第1塗敷液時的玻璃基板或玻璃帶之溫度以
200~650℃為佳,且以300~600℃較佳。在處於該溫度範圍的玻璃基板或玻璃帶上將烷氧矽烷之水解物燒成而成為氧化矽。玻璃基板或玻璃帶之溫度只要在200℃以上,即可在短時間內燒成玻璃基板或玻璃帶上的烷氧矽烷之水解物,因此生產性佳。在本發明第2實施態樣中,利用以浮製玻板法所行之玻璃基板的製造方法時,玻璃帶之溫度只要在650℃以下,玻璃帶即不會存在浮浴內,因此少有在噴霧中污染浴內環境之虞。
在本發明第2實施態樣中,利用以浮製玻板法所
行之玻璃基板的製造方法時,對已在浮浴中將熔融玻璃成形而製得之玻璃帶,在浮浴與徐冷步驟之間或在徐冷步驟中玻璃帶處於200~650℃之溫度範圍的位置噴霧第1塗敷液為佳。以浮製玻板法來製造玻璃基板時,浮浴瞬後之位置的玻璃帶溫度雖依玻璃基板之玻璃組成而異但通常在650℃左右,因此塗佈第1塗敷液之位置的玻璃帶溫度超過650℃乃不切實際。離開浮浴的玻璃帶在徐冷步驟中被徐冷,並在徐冷步驟中冷卻至400℃以下。
(第2塗敷液)
第2塗敷液係含有金屬氧化物之前驅物及因應需求之液狀介質者。
(金屬氧化物之前驅物)
作為金屬氧化物之前驅物,可舉如下述者。
氧化鈦之前驅物:鈦烷氧化物、醇鈦、乙酸鈦、氧乙醯丙酮鈦、乙醯丙酮鈦、乙二胺四乙酸鈦、乙基己酸鈦、苯甲酸鈦、乳酸鈦、硫化鈦、氟化鈦、氯化鈦、溴化鈦、碘化鈦等。
氧化鋅之前驅物:乙酸鋅、乙醯丙酮鋅、乙二胺四乙酸鋅、乙基己酸鋅、十八酸鋅、苯甲酸鋅、環烷酸鋅、乳酸鋅、硫化鋅、硼酸鋅、碳酸鋅、氟化鋅、氯化鋅、溴化鋅、碘化鋅等。
氧化錫之前驅物:乙酸錫、二乙酸二丁錫、乙醯丙酮錫、乙二胺四乙酸錫、乙基己酸錫、硫化錫、氟化錫、氯化錫、溴化錫、碘化錫等。
氧化矽之前驅物:烷氧矽烷之水解物、有機聚矽氧烷(矽酮油等)等。
(液狀介質)
第2塗敷液之液狀介質因應金屬氧化物之前驅物適當選擇即可。
(第2塗敷液之組成)
第2塗敷液之固體成分濃度(第2塗敷液中之金屬氧化物之前驅物濃度)因應金屬氧化物之前驅物適當選擇即可。
(第2塗敷液之塗佈)
作為第2塗敷液之塗佈方法,從可生產效率良好地製造附有含無機微粒子之氧化矽膜的玻璃基板之觀點看來,以使用噴嘴(例如噴槍等)來噴霧第2塗敷液的噴霧法為佳。
作為噴霧法的具體塗佈方法,可舉如上述方法(i)、(ii)、(iii)等,從步驟數少且可以較佳的生產效率製造附有含無機微粒子之氧化矽膜的玻璃基板之觀點看來,以方法(ii)為佳。
塗佈第2塗敷液時的玻璃基板或玻璃帶之溫度在
200~650℃為佳,且在300~600℃較佳。
在本發明第2實施態樣中,利用以浮製玻板法所行之玻璃基板的製造方法時,作為第2塗敷液之塗佈方法,宜對已在浮浴中將熔融玻璃成形而製得之玻璃帶,在浮浴與徐冷步驟之間或在徐冷步驟中,於玻璃帶處於200~650℃之溫度範圍的位置噴霧第2塗敷液。
(玻璃製造裝置)
圖3係顯示玻璃製造裝置一例的概略圖。
玻璃製造裝置20具備:熔解窯22,將玻璃原料熔解而製成熔融玻璃30;浮浴26,藉由使從熔解窯22供給的熔融玻璃30浮在熔融錫24表面上,而將熔融玻璃30成形為後續成為玻璃基板的玻璃帶32;徐冷窯28,將該玻璃帶32徐冷;及空氣式第1噴槍34,係設置在浮浴26之出口與徐冷窯28之入口間且在玻璃帶32上方高度570mm處,以塗佈第1塗敷液。又,亦宜於第1噴槍34之後段設置塗佈第2塗敷液的第2噴槍36。
對以預定搬送速度移動的玻璃帶32,在浮浴26
與徐冷窯28之間,於玻璃帶32之表面溫度處於200~650℃之位置從第1噴槍34噴霧第1塗敷液而於玻璃帶32上形成含無機微粒子之氧化矽膜,接著從第2噴槍36噴霧第2塗敷液至含無機微粒子之氧化矽膜上而於含無機微粒子之氧化矽膜上形成金屬氧化物膜。
離開徐冷窯28的玻璃帶32會藉由未圖示的切斷裝置切斷而成為玻璃基板。
以上所說明之本發明之附有含無機微粒子之氧化矽膜的玻璃基板之製造方法中,由於係在玻璃基板或玻璃帶上塗佈含有無機微粒子之塗敷液,因此可因應目標的光學特性使用期望粒徑的無機微粒子。其結果可製得具有目標光學性能的附有含無機微粒子之氧化矽膜的玻璃基板。
又,由於以上所說明之本發明之附有含無機微粒
子之氧化矽膜的玻璃基板之製造方法中,作為塗敷液所含之氧化矽之前驅物係使用烷氧矽烷之水解物來取代習知的有機聚矽氧烷,因此作為液狀介質可使用極性者。與可分散於非極性液狀介質之無機微粒子相比,可分散於極性液狀介質之無機微粒子其種類較多,且無須施行疏水化等表面處理,因此無機微粒子的選擇幅度變廣。
而,與習知的有機聚矽氧烷相較下,氧化矽之前
驅物即烷氧矽烷的水解物較容易在高溫下氣化,且有對玻璃基板或玻璃帶上之著膜效率較差的傾向,但由於在本發
明中作為液狀介質係使用水及(聚)乙二醇中之任一者或兩者,因此含無機微粒子之氧化矽膜於玻璃基板或玻璃帶上之著膜效率佳。
又,藉由於含無機微粒子之氧化矽膜上形成金屬氧化物膜,可製造藉光散射獲致之防眩效果、光擷取效果、及光侷限效果等獲提高的附有含無機微粒子之氧化矽膜的玻璃基板。
以下藉由實施例進一步詳細說明本發明,惟本發明不受該等實施例限定。
例8~19係實施例,例1~7係比較例。
(被覆率)
作為著膜效率之指標,以如下述的方法求出無機微粒子在玻璃基板上之被覆率。
使用接觸段差計(ALVAC公司製、DEKTAK150),以測定長度1mm測定含無機微粒子之氧化矽膜的表面凹凸形狀。從測定結果抽出存在有無機微粒子之部分的長度,並從下式求算被覆率。
被覆率(%)=100×存在有無機微粒子之部分的長度(mm)/測定長度(1mm)。
(霧度)
作為光散射之指標,使用霧度計(BYK-Gardner公司製、HAZE-GARD PLUS E-4725型)測定附有含無機微粒子之氧化矽膜的玻璃基板之霧度。
[例1~11]
於表1顯示之液狀介質加入四乙氧矽烷(關東化學公司製、SiO2換算固體成分:99.9質量%)使其在第1塗敷液中成為30質量%,再加入硝酸(70質量%水溶液)使其在第1塗敷液中成為0.35質量%,並攪拌1小時。接下來,加入矽溶膠(日產化學工業製、MP-4540M、平均一次粒徑:450nm、固體成分:40.7質量%、介質:水)使其在第1塗敷液中成為2.5質量%並攪拌5~10分,而製得例1~例11之第1塗敷液,其SiO2換算固體成分濃度為9.65質量%,固體成分中之氧化矽粒子比率為10.4質量%,且固體成分中之烷氧矽烷之水解物(SiO2換算固體成分)比率為89.6質量%。
作為塗佈裝置係使用KM-100(SPD研究所公司
製)。作為玻璃基板係使用10cm×10cm×4mm之高穿透玻璃(旭硝子公司製)。
將玻璃基板載置於工作台上,並於工作台背面側以與工作台非接觸的方式設置加熱器。藉由加熱器之放射熱,隔著工作台將玻璃基板加熱至600℃。玻璃基板之溫度係藉由使玻璃基板之一側面接觸熱電耦而測定。由於以噴槍噴霧第1塗敷液之前已將玻璃基板加熱充分的時間,因此在此所測定之溫度可視為與玻璃基板之表面溫度大致相同。
將玻璃基板升溫至600℃後,從配置在玻璃基板上方之噴槍噴霧第1塗敷液至玻璃基板上。從噴槍噴霧第1塗敷液時,調節對噴槍之送液壓力使送液速度為0.3~0.6mL/秒,且噴霧壓力設為0.1MPa。塗佈時間設為15秒。而,工作台、
玻璃基板、噴槍係在被防爆裝置包圍的狀態下進行噴霧,未調整環境溫度。
製得之例1~11之附有含氧化矽粒子之氧化矽膜的玻璃基板的被覆率及霧度顯示於表1。
以水或(聚)乙二醇作為主要液狀介質使用的本
發明實施例之例8~11中,與使用其他液狀介質之例1~7相較下顯示出高粒子被覆率。又,隨之,霧度亦上升,並顯示出高光散射特性。
[例12~14]
除了將玻璃基板之溫度如表2變更成300℃、400℃、500℃以外,使用例10之液狀介質,以與例1~11同樣的方式製得附有含氧化矽粒子之氧化矽膜的玻璃基板。製得之附有含氧化矽粒子之氧化矽膜的玻璃基板之被覆率及霧度顯示於表2。
[表2]
[例15~19]
於三乙二醇加入四乙氧矽烷(關東化學公司製、SiO2換算固體成分:99.9質量%)使其在第1塗敷液中成為30質量%,再加入硝酸(70質量%水溶液)使其在第1塗敷液中成為0.35質量%,並攪拌1小時。接下來,加入矽溶膠(日產化學工業製、MP-2040、平均一次粒徑:190nm、固體成分:40質量%、介質:水)使其在第1塗敷液中成為2.5質量%並攪拌5~10分,而製得例15~例19之第1塗敷液,其SiO2換算固體成分濃度為9.65質量%,固體成分中之氧化矽粒子比率為10.4質量%,且固體成分中之烷氧矽烷之水解物(SiO2換算固體成分)比率為89.6質量%。
於正癸烷加入矽酮油(信越有機矽公司製、
X-22-7322)使其在第2塗敷液中成為70質量%並攪拌10分鐘,而製得例16之第2塗敷液。
於乙醯丙酮加入四丁氧化鈦使其在第2塗敷液中
成為20質量%並攪拌1小時,而製得例17之第2塗敷液。
於N,N-二甲基甲醯胺加入二氫化乙酸鋅使其在
第2塗敷液中成為20質量%並攪拌30分鐘,而製得例18之第2塗敷液。
於N,N-二甲基甲醯胺加入二乙酸二丁錫(氧化錫
前驅物)使其在第2塗敷液中成為20質量%並攪拌10分鐘,而製得例19之第2塗敷液。
與例1同樣地將玻璃基板升溫至600℃後,從配置
在玻璃基板上方之噴槍噴霧第1塗敷液至玻璃基板上。從噴槍噴霧第1塗敷液時,調節對噴槍的送液壓力以使送液速度成為0.3~0.6mL/秒,且將噴霧壓力設為0.1MPa。塗佈時間係設為15~30秒。
針對例15,就僅形成有含有氧化矽粒子之氧化矽
膜的玻璃基板進行評估。霧度顯示於表3。
針對例16~19,於含有氧化矽粒子之氧化矽膜之形成緊接著使用上述之各個第2塗敷液,以下述方式進一步形成金屬氧化物膜。
將剛形成含有氧化矽粒子之氧化矽膜的玻璃基
板維持在600℃的狀態下,從配置在玻璃基板上方之噴槍噴霧第2塗敷液至含有氧化矽粒子之氧化矽膜上。從噴槍噴霧第2塗敷液時,調節對噴槍的送液壓力以使送液速度成為0.3~0.6mL/秒,並將噴霧壓力設為0.1MPa。塗佈時間係設為15~30秒。
針對於含有氧化矽粒子之氧化矽膜上形成有金屬氧化物膜之例16~例19的玻璃基板進行評估。霧度顯示於表3。
[表3]
與僅形成有含有氧化矽粒子之氧化矽膜的玻璃
基板(例15)相較下,進一步形成有折射率與氧化矽粒子相異之金屬氧化物膜的玻璃基板(例17~19)霧度有大幅提升。
而,在進一步形成有折射率與氧化矽粒子相同之氧化矽膜的玻璃基板(例16)中,未見霧度提升。
以本發明製造方法製得之附有含無機微粒子之氧化矽膜的玻璃基板可有效地作為具有防眩效果之窗玻璃、具有光擷取效果之有機EL元件用玻璃基板、及具有光侷限效果之太陽電池用蓋玻璃等使用。
而,在此係引用已於2012年4月24日提出申請之日本專利申請案2012-099166號之說明書、申請專利範圍、圖式及摘要的全部內容,並納入作為本發明揭示。
1‧‧‧附有含無機微粒子之氧化矽膜的玻璃基板
10‧‧‧玻璃基板
12‧‧‧含無機微粒子之氧化矽膜
14‧‧‧無機微粒子
16‧‧‧氧化矽膜
Claims (7)
- 一種附有含無機微粒子之氧化矽膜的玻璃基板之製造方法,係將塗敷液塗佈於玻璃基板上而形成含無機微粒子之氧化矽膜者,該塗敷液含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者。
- 如申請專利範圍第1項之製造方法,其塗佈前述塗敷液時之玻璃基板溫度為200~650℃。
- 如申請專利範圍第1或2項之製造方法,其更於前述含無機微粒子之氧化矽膜上形成折射率與前述無機微粒子相異之金屬氧化物膜。
- 一種附有含無機微粒子之氧化矽膜的玻璃基板之製造方法,具有下述步驟:於由熔融玻璃所成形之玻璃帶上塗佈塗敷液而形成含無機微粒子之氧化矽膜之步驟,該塗敷液含有無機微粒子、烷氧矽烷之水解物、水及(聚)乙二醇中之任一者或兩者;及其後將玻璃帶切斷之步驟。
- 如申請專利範圍第4項之製造方法,其塗佈前述塗敷液時之玻璃帶溫度為200~650℃。
- 如申請專利範圍第4或5項之製造方法,其係在浮浴中將熔融玻璃成形為玻璃帶,並在浮浴與徐冷步驟之間或在徐冷步驟中塗佈前述塗敷液。
- 如申請專利範圍第4至6項中任一項之製造方法,其更於 玻璃帶上之前述含無機微粒子之氧化矽膜上,形成折射率與前述無機微粒子相異之金屬氧化物膜。
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