KR930009946A - 표면이 잘고 거칠은 금속산화막 및 이것을 유리기판위에 형성하는 방법 - Google Patents

표면이 잘고 거칠은 금속산화막 및 이것을 유리기판위에 형성하는 방법 Download PDF

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KR930009946A
KR930009946A KR1019920022583A KR920022583A KR930009946A KR 930009946 A KR930009946 A KR 930009946A KR 1019920022583 A KR1019920022583 A KR 1019920022583A KR 920022583 A KR920022583 A KR 920022583A KR 930009946 A KR930009946 A KR 930009946A
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glass substrate
metal oxide
sol
film
compound
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KR1019920022583A
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KR950014694B1 (ko
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오사무 타카하시
히로아끼 아라이
세이지 야마사키
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와다 가꾸헤이
센트럴가라스 가부시기가이샤
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    • 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
    • C03C17/22—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
    • 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
    • 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
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/212—TiO2
    • 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
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/213—SiO2
    • 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
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/22—ZrO2
    • 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
    • C03C2217/77—Coatings having a rough surface
    • 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
    • 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
    • Y10T428/31—Surface property or characteristic of web, sheet or block
    • Y10T428/315—Surface modified glass [e.g., tempered, strengthened, etc.]

Abstract

본 발명은 졸-겔법으로 유리기판위에 형성된 금속산화막에 관한 것으로, 금속산화막을 잘고 거칠게 만들기 위해서는 금속알콕시드류 및 금속아세틸 아세토네이토류로 이루어지는 군에서 선택된 1종 이상의 화합물로부터 졸의 중합체의 평균분자량이 다르도록 각각2종 이상의 졸을 제조한 다음 2종 이상의 졸을 용매와 혼합하여 도료액을 제조하고, 도료액을 유리기판에 도포하여 졸막을 형성하고, 이렇게 도포된 유리기판을 가열하여 졸막을 겔막으로 변헝시키고 그 위에 다수의 마이카로피트를 형성한다.

Description

표면이 잘고 거칠은 금속산화막 및 이것을 유리기판위에 형성하는 방법
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
제1도는 본 발명에 따른 유리판위에 피복된 금속산화막의 표면상태를 도시하는, 터널형현미경을 통해 찍은 사진, 제2도는 본 발명에 따른 유리판위에 피복된 금속산화막의 표면상태를 도시하는, 주사형전자현미경을 통해 배율 10,000으로 찍은 사진, 제3도는 제2도와 유사한 사진이나, 종래방법으로 유리판위에 도포된 금속산화막의 표면상태를 도시.

Claims (12)

  1. (a) 1종 이상의 화합물로부터 각각 2종 이상의 졸을 제조하여 그 속에 1종 이상의 화합물의 2종 이상의 중합체를 분산시키고 (1종 이상의 화합물은 금속알콕시드류 및 금속아세틸아세토네이토류로 이루어진 군에서 선택되며, 2종 이상의 중합체는 평균분자량이 다르다), (b) 2종 이상의 졸을 용매와 혼합해서 도포액을 제조하고, (c) 도포액을 유리기판위에 도포하여 졸막을 형성하고, (d) 유리기판을 가열하여 졸막을 겔막으로 변형시키고 그 위에 다수의 마이크로피트를 형성하는 공정으로 이루어지는, 다수의 마이크로피트를 지닌 금속산화막을 유리기판위에 형성하는 방법.
  2. 제1항에 있어서, 상기 용매는 알콜용액인 것을 특징으로 하는 방법.
  3. 제1항에 있어서, 공정(d)에서 유리기판을 가열할 때 온도를 100℃이상으로 하는 것을 특징으로 하는 방법.
  4. 제1항에 있어서, 상기 1종 이상의 화합물은 Si, Ti 및 Zr의 알콕시드와 Si, Ti 및 Zn의 아세틸아세토네이토로 이루어지는 군에서 선택되는 것을 특징으로 하는 방법.
  5. 제1항에 있어서, 상기2종 이상의 중합체의 한쪽은 평균분자량이 800∼8,000이고, 다른 쪽은 10,000이상인 것을 특징으로 하는 방법.
  6. 제5항에 있어서, 상기 중합체의 다른 쪽의 평균분자량은 10,000∼70,000인 것을 특징으로 하는 방법.
  7. 제5항에 있어서, 상기 중합체의 다른 쪽의 평균분자량은 100,000∼400,000인 것을 특징으로 하는 방법.
  8. 제1항에 있어서, 공정(b)에서 상기 한쪽과 다른쪽의 중합체를 금속산화물로서 계산한 용질의 몰수로 표현하여 1:1∼8:1의 비율로 혼합하는 것을 특징으로 하는 방법.
  9. 제8항에 있어서, 공정(b)에서 상기 한쪽과 다른쪽의 중합체를 금속산화물로서 계산한 용질의 몰수로 표현하여 3:1∼6:1의 비율로 혼합하는 것을 특징으로 하는 방법.
  10. 제1항의 방법에 따라 제조된 금속산화막의 1층 이상으로 이루어진 다층막.
  11. 제1항에 있어서, 공정(b)에서 도료액의 점도를 1∼10cP로 조정하는 것을 특징으로 하는 방법.
  12. (a) 1종 이상의 화합물로부터 각각 2종 이상의 졸을 제조하여 그 속에 1종 이상의 화합물의 2종 이상의 중합체를 분산시키고(1종 이상의 화합물은 금속알콕시드류 및 금속아세틸아세토네이토류로 이루어진 군에서 선택되며, 2종 이상의 중합체는 평균분자량이 다르다), (b)2종 이상의 졸을 용매와 혼합해서 도포액을 제조하고, (c) 도포액을 유리기판위에 도포하여 졸막을 형성하고, (d) 유리기판을 가열하여 졸막을 겔막으로 변형시키고 그 위에 다수의 마이크로피트를 형성하는 공정으로 이루어지는 방법에 따라 유리기판위에 다수의 마이크로피트가 형성된 금속산화막.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019920022583A 1991-11-29 1992-11-27 표면이 잘고 거칠은 금속산화막 및 이것을 유리기판위에 형성하는 방법 KR950014694B1 (ko)

Applications Claiming Priority (2)

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JP3316992A JP2716302B2 (ja) 1991-11-29 1991-11-29 マイクロピット状表層を有する酸化物薄膜および該薄膜を用いた多層膜、ならびにその形成法
JP91-316992 1991-11-29

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KR930009946A true KR930009946A (ko) 1993-06-21
KR950014694B1 KR950014694B1 (ko) 1995-12-13

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US (1) US5403368A (ko)
EP (1) EP0545258B1 (ko)
JP (1) JP2716302B2 (ko)
KR (1) KR950014694B1 (ko)
CA (1) CA2084045C (ko)
DE (1) DE69201856T2 (ko)

Families Citing this family (29)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2716330B2 (ja) * 1992-11-13 1998-02-18 セントラル硝子株式会社 低反射ガラスおよびその製法
DE4331082C1 (de) * 1993-09-13 1995-04-13 Schott Glaswerke Brandsichere Glasscheibe und Verfahren zur Herstellung einer solchen Glasscheibe
US5674625A (en) * 1993-11-10 1997-10-07 Central Glass Company, Limited Multilayered water-repellent film and method of forming same on glass substrate
US5733660A (en) * 1994-05-20 1998-03-31 Central Glass Company, Limited Glass pane with reflectance reducing coating
DE4429533A1 (de) * 1994-08-19 1996-02-22 Cerdec Ag Wasser- und hydroxylgruppenfreie Gele und Xerogele, Verfahren zu deren Herstellung und deren Verwendung
EP0748775A3 (en) * 1995-05-30 1998-11-25 Central Glass Company, Limited Water-repellent glass plate having minutely roughed metal-oxide base film
WO1997006896A1 (en) * 1995-08-14 1997-02-27 Central Glass Company Limited Porous metal-oxide thin film and method of forming same on glass substrate
EP0763504B1 (en) * 1995-09-14 1999-06-02 Heraeus Quarzglas GmbH Silica glass member and method for producing the same
US6130152A (en) * 1995-11-16 2000-10-10 Texas Instruments Incorporated Aerogel thin film formation from multi-solvent systems
JPH09208266A (ja) * 1996-01-29 1997-08-12 Du Pont Kk ガラス表面への有機系ポリマコーティング方法および有機系ポリマをコーティングしたガラス
JP3488965B2 (ja) * 1996-05-21 2004-01-19 日本山村硝子株式会社 ゾル−ゲル法による独立膜の製造方法
JP2901550B2 (ja) * 1996-07-26 1999-06-07 株式会社村上開明堂 防曇素子
JPH10237078A (ja) 1996-10-14 1998-09-08 Dainippon Printing Co Ltd 金属錯体溶液、感光性金属錯体溶液及び金属酸化物膜の形成方法
FR2756276B1 (fr) * 1996-11-26 1998-12-24 Saint Gobain Vitrage Substrat a proprietes hydrophiles ou hydrophobes ameliorees, comportant des irregularites
JP3700358B2 (ja) * 1996-12-18 2005-09-28 日本板硝子株式会社 防曇防汚ガラス物品
JPH10259038A (ja) 1997-01-24 1998-09-29 Samsung Corning Co Ltd 耐久性撥水ガラス及びその製造方法
KR100281993B1 (ko) * 1997-06-26 2001-04-02 박영구 내구성 발수유리와 그 제조방법
US6394613B1 (en) * 1997-08-07 2002-05-28 Canon Kabushiki Kaisha Anti-fogging and anti-reflection optical article
JP3456396B2 (ja) * 1997-12-25 2003-10-14 日本板硝子株式会社 透光性着色膜付きガラス基板の製造方法
DE69926093T2 (de) 1998-02-13 2006-05-11 Central Glass Co., Ltd., Ube Wasserabweisende Lösung und Verfahren zur Herstellung einer wasserabweisenden Schicht auf einem Substrat mittels dieser Lösung
DE19829172A1 (de) * 1998-06-30 2000-01-05 Univ Konstanz Verfahren zur Herstellung von Antireflexschichten
DE19845291A1 (de) * 1998-10-01 2000-04-13 Fraunhofer Ges Forschung Verfahren zur Abscheidung von Titanoxid-Schichten unter Verwendung von löslichen Pulvern
DE19943789A1 (de) * 1999-09-13 2001-03-15 Fraunhofer Ges Forschung Verfahren zur Abscheidung von Zirkonoxid-Schichten unter Verwendung von löslichen Pulvern
EP1873126A1 (en) * 2006-02-22 2008-01-02 Central Glass Co., Ltd. Anti-Glare Glass Substrate
DE102007053839B4 (de) * 2007-11-12 2009-09-24 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verwendung eines beschichteten, transparenten Substrats zur Beeinflussung der menschlichen Psyche
US20130309613A1 (en) * 2012-05-16 2013-11-21 Corning Incorporated Liquid Based Films
EP2880474A4 (en) * 2012-08-01 2016-03-23 Ferro Corp LIGHT-INFLUENCING NANOSCREEN
US20140186613A1 (en) * 2012-12-27 2014-07-03 Guardian Industries Corp. Anti-reflection coatings with self-cleaning properties, substrates including such coatings, and related methods
EP3619175A1 (en) * 2017-05-04 2020-03-11 AGC Glass Europe Coated substrate

Family Cites Families (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR751917A (fr) * 1932-01-26 1933-09-12 Eclipse Machine Co Mécanisme de démarrage pour moteurs à combustion interne
FR1596613A (ko) * 1967-11-20 1970-06-22
US4129434A (en) * 1971-07-08 1978-12-12 Glaverbell Process for forming a metal oxide coating
US3850665A (en) * 1971-07-08 1974-11-26 Glaverbel Process for forming a metal oxide coating on a substrate and resulting products
US4160061A (en) * 1975-03-29 1979-07-03 Central Glass Company, Limited Heat-reflecting glass plate and method of producing same
JPS5332806A (en) * 1976-09-08 1978-03-28 Hitachi Ltd Production of damping material
US4100330A (en) * 1977-03-28 1978-07-11 Ppg Industries, Inc. Method for coating glass with silicon and a metal oxide and resulting product
JPS5424A (en) * 1977-06-03 1979-01-05 Asahi Glass Co Ltd Method of forming titanium oxide coating layer on glass surface
JPS5422426A (en) * 1977-07-22 1979-02-20 Asahi Glass Co Ltd Method of forming titanium oxide coating layer on glass surface
BE879189A (fr) * 1978-10-19 1980-04-04 Bfg Glassgroup Procede de formation d'un revetement d'oxyde d'etain sur un support de verre chaud et produits ainsi obtenus
US4719126A (en) * 1983-02-02 1988-01-12 Ppg Industries, Inc. Pyrolytic deposition of metal oxide film from aqueous suspension
US4719127A (en) * 1983-02-02 1988-01-12 Ppg Industries, Inc. Aqueous chemical suspension for pyrolytic deposition of metal-containing film
US4596745A (en) * 1984-05-04 1986-06-24 Cotek Company Non-glare coating
US4830879A (en) * 1986-09-25 1989-05-16 Battelle Memorial Institute Broadband antireflective coating composition and method
FR2621030B1 (fr) * 1987-09-29 1990-11-16 Centre Nat Rech Scient Procede de preparation d'oxydes metalliques
JPH01239024A (ja) * 1988-03-18 1989-09-25 Giken Kagaku Kk 酸化チタン被膜形成方法
JPH0637283B2 (ja) * 1989-12-20 1994-05-18 セントラル硝子株式会社 酸化物薄膜の成膜方法
US5137560A (en) * 1990-03-09 1992-08-11 Asahi Glass Company, Inc. Process for manufacturing glass with functional coating
JP3300382B2 (ja) * 1991-05-20 2002-07-08 眞一 平野 βーＢａＢ２Ｏ４薄膜の製造方法
US5219611A (en) * 1991-09-30 1993-06-15 Cornell Research Foundation, Inc. Preparing densified low porosity titania sol gel forms
JPH05170486A (ja) * 1991-12-25 1993-07-09 Central Glass Co Ltd ガラス表面用撥水処理剤およびその撥水処理ガラス

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JPH05147976A (ja) 1993-06-15
DE69201856D1 (de) 1995-05-04
EP0545258B1 (en) 1995-03-29
JP2716302B2 (ja) 1998-02-18
DE69201856T2 (de) 1995-07-27
US5403368A (en) 1995-04-04
CA2084045C (en) 1996-07-30
KR950014694B1 (ko) 1995-12-13
EP0545258A1 (en) 1993-06-09
CA2084045A1 (en) 1993-05-30

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