JP5219805B2 - シリカフィルムの形態制御 - Google Patents
シリカフィルムの形態制御 Download PDFInfo
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- JP5219805B2 JP5219805B2 JP2008513867A JP2008513867A JP5219805B2 JP 5219805 B2 JP5219805 B2 JP 5219805B2 JP 2008513867 A JP2008513867 A JP 2008513867A JP 2008513867 A JP2008513867 A JP 2008513867A JP 5219805 B2 JP5219805 B2 JP 5219805B2
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- film
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- hydrolyzable
- silica
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 70
- 239000000377 silicon dioxide Substances 0.000 title claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 77
- 238000000034 method Methods 0.000 claims description 56
- 238000000576 coating method Methods 0.000 claims description 44
- 239000002243 precursor Substances 0.000 claims description 44
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 43
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- 239000000758 substrate Substances 0.000 claims description 31
- 239000011248 coating agent Substances 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000012298 atmosphere Substances 0.000 claims description 26
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 19
- 229910021529 ammonia Inorganic materials 0.000 claims description 19
- 238000006460 hydrolysis reaction Methods 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 19
- 239000011148 porous material Substances 0.000 claims description 18
- 239000003112 inhibitor Substances 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 12
- 230000007062 hydrolysis Effects 0.000 claims description 12
- 125000003118 aryl group Chemical group 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004528 spin coating Methods 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 125000003342 alkenyl group Chemical group 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000003618 dip coating Methods 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Chemical group 0.000 claims description 4
- 125000001424 substituent group Chemical group 0.000 claims description 4
- 150000005846 sugar alcohols Polymers 0.000 claims description 4
- 239000011593 sulfur Chemical group 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011253 protective coating Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229930013930 alkaloid Natural products 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002366 halogen compounds Chemical class 0.000 claims description 2
- 125000001072 heteroaryl group Chemical group 0.000 claims description 2
- 125000001624 naphthyl group Chemical group 0.000 claims description 2
- 150000007530 organic bases Chemical class 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 150000003141 primary amines Chemical class 0.000 claims description 2
- 150000003335 secondary amines Chemical class 0.000 claims description 2
- 229910052710 silicon Chemical group 0.000 claims description 2
- 239000010703 silicon Chemical group 0.000 claims description 2
- 150000003512 tertiary amines Chemical class 0.000 claims description 2
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 claims 2
- 230000002378 acidificating effect Effects 0.000 claims 1
- 125000005843 halogen group Chemical group 0.000 claims 1
- 230000003301 hydrolyzing effect Effects 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- -1 tetramethyl ester Chemical class 0.000 claims 1
- 239000010408 film Substances 0.000 description 71
- 238000001723 curing Methods 0.000 description 41
- 239000000203 mixture Substances 0.000 description 31
- 238000009472 formulation Methods 0.000 description 26
- 230000008569 process Effects 0.000 description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 12
- 239000002585 base Substances 0.000 description 12
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 12
- 239000011521 glass Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 6
- 238000003980 solgel method Methods 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 239000006117 anti-reflective coating Substances 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 125000003158 alcohol group Chemical group 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 229920001519 homopolymer Polymers 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 230000003667 anti-reflective effect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 150000007529 inorganic bases Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 125000005233 alkylalcohol group Chemical group 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000005328 architectural glass Substances 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- VGWJKDPTLUDSJT-UHFFFAOYSA-N diethyl dimethyl silicate Chemical compound CCO[Si](OC)(OC)OCC VGWJKDPTLUDSJT-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- UYJOENUOBRUAJU-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC.CC[Si](OC)(OC)OC UYJOENUOBRUAJU-UHFFFAOYSA-N 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002367 halogens Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- XQMTUIZTZJXUFM-UHFFFAOYSA-N tetraethoxy silicate Chemical compound CCOO[Si](OOCC)(OOCC)OOCC XQMTUIZTZJXUFM-UHFFFAOYSA-N 0.000 description 1
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
Classifications
-
- 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
- C09D183/02—Polysilicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
- C03C1/008—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route for the production of films or 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
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/425—Coatings comprising at least one inhomogeneous layer consisting of a porous layer
-
- 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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/75—Hydrophilic and oleophilic 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
-
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes
-
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
-
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Wood Science & Technology (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Paints Or Removers (AREA)
- Silicon Compounds (AREA)
- Surface Treatment Of Optical Elements (AREA)
Description
(ここで、Xは少なくとも三つのXが加水分解性基でなければならないという条件でそれぞれ独立的に加水分解性基又は非加水分解性基から選択される。)
前駆体製剤のコーティングを基板上に形成し、その後、塩基と水と加水分解性ケイ酸塩オリゴマーの加水分解を抑制する抑制剤とを含む気体雰囲気(vapourous environment)においてコーティングを加水分解および縮合を行うことによりコーティングを硬化すること、を含む基板上を覆うシリカ又はシリカ様フィルムを形成する方法に属する。
ここで、少なくとも三つのX基は、加水分解性基である。X基の選択は特に限定されないが、以下に説明する。これらの物質の特定の例は、オルトケイ酸塩テトラメチル及びオルトケイ酸塩テトラエチルのオリゴマー型であるケイ酸メチル、ケイ酸エチルをそれぞれ有する。これらの物質はまた、テトラメトキシシラン及びテトラエトキシシランとしても知られる。
ケイ酸塩エチル40(ケイ酸テトラエチルエステルホモポリマー94%より多く(>94%)、テトラエトキシシラン4%未満(<4%)、エタノール4%未満(<4%)を含む){コルコート株式会社製:日本国143−0015東京都大田区大森西3−28−6}50mlをエタノール又はメタノール100mlに加えて、前駆体製剤を作製する。
単量体のエチルトリメトキシシラン(ethyltrimethoxysilane:ETOS){Sigma−Aldrich社製:Castle Hill,NSW Australia}を水と、2部の水に対して1部のETOSのモル比で混合する。ここで、水にはETOSを溶かすためのエタノールが十分に加えられている。この混合物は、反応してケイ酸塩オリゴマーを生成する。
単量体のメチルトリメトキシシラン(methyltrimethoxysilane:MTOS){Sigma−Aldrich社製:Castle Hill,NSW Australia}を水と、3部の水に対して1部のMTOSのモル比で混合する。ここで、水にはMTOSを溶かすためのエタノールが十分に加えられている。この混合物は、反応してケイ酸塩オリゴマーを生成する。他の比率、2部の水に対して1部のMTOS、4部の水に対して1部のMTOSでも適切であるということが認められている。
2 台状のもの
3 基板
4 容器
5 雰囲気
6 ポート
Claims (21)
- 以下の構造式で表わされる加水分解性ケイ酸塩オリゴマーを溶媒に溶解させることによりシリカ前駆体溶液を調整し、
塩基と水と前記加水分解性ケイ酸塩オリゴマーの加水分解を抑制する抑制剤とが含まれる気体雰囲気において前記コーティングを加水分解及び縮合することにより前記シリカ前駆体溶液の前記コーティングを硬化すること、
を含み、
Xは少なくとも三つのXが加水分解性基であり、且つそれぞれ独立的に加水分解性基又は非加水分解性基から選択され、前記加水分解性ケイ酸塩オリゴマーは、ケイ酸テトラメチルエステルホモポリマーではなく、前記シリカ前駆体溶液は、5体積%未満の水を含み、且つ酸性ではないことを特徴とする基板上にコーティングされたシリカ又はシリカ様フィルムの作製方法。 - 前記硬化することが、
前記コーティングされた基板を気体の前記抑制剤が備えられたチャンバーに配置し、
前記チャンバーに前記水と塩基とを順次に導入すること、
を含むことを特徴とする請求項1に記載の方法。 - Xが加水分解性基である場合、C1〜C10のアルキル基、フェニル基又はナフチル基を含めたアリール基、置換されたC1〜C10のアルキル基又はアリール基を含むグループから選択されることを特徴とする請求項1に記載の方法。
- Xが非加水分解性基である場合、アルキル基、アルケニル基及びアリール基、又はハロゲン、窒素、酸素、硫黄又はケイ素で置換されたアルキル基、アルケニル基及びアリール基を含むグループから選択されることを特徴とする請求項1に記載の方法。
- Xが、ハロゲン化合物、アリール基、ヘテロアリール基、あるいは窒素、酸素又は硫黄といったシリカフィルムの構造に干渉しない置換基を有する一つ以上の不活性な置換基に置換されることを特徴とする請求項1に記載の方法。
- 前記塩基は、アンモニア、第1級アミン、第2級アミン、第3級アミンを含めた揮発性アミノ−アルカン、又はアルカロイドなどの揮発性アミノ−アルケンを含むグループから選択される揮発性の有機塩基であることを特徴とする請求項1に記載の方法。
- 前記塩基がアンモニアであることを特徴とする請求項1に記載の方法。
- 前記フィルムにおける孔の大きさを制御するために前記溶媒を選択することをさらに含むことを特徴とする請求項1に記載の方法。
- 前記加水分解性ケイ酸塩オリゴマーは、以下に表される分子前駆体から適宜誘導されることを特徴とする請求項1に記載の方法。
- 前記気体雰囲気における前記塩基、前記抑制剤及び前記水のそれぞれの分圧を制御することによる前記フィルムの形態制御をさらに含むことを特徴とする請求項1に記載の方法。
- 前記溶媒がメタノール、エタノール、イソプロピルアルコール、ブタノール、ペンタノール及び多価アルコールを含むグループから選択されることを特徴とする請求項8に記載の方法。
- 前記フィルムにおける前記孔の密度を制御するために前記溶媒の濃度を選択することをさらに含むことを特徴とする請求項1に記載の方法。
- 前記フィルムにおける孔の密度を制御するために前記気体雰囲気における前記抑制剤の濃度を選択することをさらに含むことを特徴とする請求項1に記載の方法。
- スピンコーティング又はディップコーティングを行うことによって前記コーティングを形成することを特徴とする請求項1に記載の方法。
- 前記コーティング条件は、最終的なフィルムの膜厚に影響することを特徴とする請求項14に記載の方法。
- 前記硬化は、常温及び常圧又はその付近で行われることを特徴とする請求項1に記載の方法。
- 前記フィルムは、1.1〜1.56の屈折率と100μm未満の膜厚とを有することを特徴とする請求項1に記載の方法。
- 前記水と塩基とを前記チャンバーに導入する前に、前記コーティングによって前記気体の抑制剤を平衡にすることをさらに含むことを特徴とする請求項2に記載の方法。
- 透明基板上にコーティングされて反射防止コーティング及び/又は曇り防止コーティング及び/又は保護コーティングとして使用されることを特徴とする請求項1の方法により作製されたフィルム。
- 親水性であることを特徴とする請求項1の方法により作製されたフィルム。
- 高表面積を有することを特徴とする請求項1の方法により作製されたフィルム。
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AU2005902785A AU2005902785A0 (en) | 2005-05-31 | Control of morphology of silica films | |
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PCT/AU2006/000733 WO2006128232A1 (en) | 2005-05-31 | 2006-05-31 | Control of morphology of silica films |
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US (2) | US8007868B2 (ja) |
EP (2) | EP1734016B1 (ja) |
JP (2) | JP5219805B2 (ja) |
CN (1) | CN101203581B (ja) |
CA (1) | CA2610643C (ja) |
MX (1) | MX2007014980A (ja) |
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-
2006
- 2006-05-31 MX MX2007014980A patent/MX2007014980A/es active IP Right Grant
- 2006-05-31 WO PCT/AU2006/000733 patent/WO2006128232A1/en active Application Filing
- 2006-05-31 CN CN2006800194462A patent/CN101203581B/zh not_active Expired - Fee Related
- 2006-05-31 US US11/921,124 patent/US8007868B2/en not_active Expired - Fee Related
- 2006-05-31 EP EP06011146.5A patent/EP1734016B1/en not_active Not-in-force
- 2006-05-31 JP JP2008513867A patent/JP5219805B2/ja not_active Expired - Fee Related
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- 2006-05-31 EP EP06741150A patent/EP1920023A4/en not_active Ceased
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Publication number | Publication date |
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NZ563647A (en) | 2010-01-29 |
CN101203581B (zh) | 2012-09-05 |
US7642199B2 (en) | 2010-01-05 |
CN101203581A (zh) | 2008-06-18 |
US20080292889A1 (en) | 2008-11-27 |
JP2008542009A (ja) | 2008-11-27 |
JP2013039570A (ja) | 2013-02-28 |
EP1734016B1 (en) | 2017-01-04 |
CA2610643C (en) | 2014-07-29 |
WO2006128232A1 (en) | 2006-12-07 |
EP1734016A1 (en) | 2006-12-20 |
EP1920023A4 (en) | 2009-08-19 |
CA2610643A1 (en) | 2006-12-07 |
EP1920023A1 (en) | 2008-05-14 |
US20060286813A1 (en) | 2006-12-21 |
US8007868B2 (en) | 2011-08-30 |
MX2007014980A (es) | 2008-04-08 |
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