EP2694448A1 - Glassubstrat mit leicht rauer schicht - Google Patents

Glassubstrat mit leicht rauer schicht

Info

Publication number
EP2694448A1
EP2694448A1 EP12718284.8A EP12718284A EP2694448A1 EP 2694448 A1 EP2694448 A1 EP 2694448A1 EP 12718284 A EP12718284 A EP 12718284A EP 2694448 A1 EP2694448 A1 EP 2694448A1
Authority
EP
European Patent Office
Prior art keywords
glass substrate
layer
crystallites
substrate according
zno
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP12718284.8A
Other languages
English (en)
French (fr)
Inventor
Alexandre Popoff
Bernard Nghiem
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Saint Gobain Glass France SAS
Compagnie de Saint Gobain SA
Original Assignee
Saint Gobain Glass France SAS
Compagnie de Saint Gobain SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Saint Gobain Glass France SAS, Compagnie de Saint Gobain SA filed Critical Saint Gobain Glass France SAS
Publication of EP2694448A1 publication Critical patent/EP2694448A1/de
Withdrawn legal-status Critical Current

Links

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
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • 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
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • 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
    • C03C17/3429—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 at least one of the coatings being a non-oxide coating
    • C03C17/3441—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 at least one of the coatings being a non-oxide coating comprising carbon, a carbide or oxycarbide
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24—HEATING; RANGES; VENTILATING
    • F24C—DOMESTIC STOVES OR RANGES ; DETAILS OF DOMESTIC STOVES OR RANGES, OF GENERAL APPLICATION
    • F24C15/00—Details
    • F24C15/02—Doors specially adapted for stoves or ranges
    • F24C15/04—Doors specially adapted for stoves or ranges with transparent panels
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/90—Other aspects of coatings
    • C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating
    • 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
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/152—Deposition methods from the vapour phase by cvd
    • C03C2218/1525—Deposition methods from the vapour phase by cvd by atmospheric CVD
    • 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
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the present invention relates to the coating of a rough inorganic layer and / or having surface irregularities with acute angles and / or spikes and deposited on a particular glass substrate, by an amorphous or nanocrystalline layer, in order to reduce or eliminate the surface roughness and / or rounding or softening surface irregularities.
  • the assembly constituted by the substrate and the layers is in particular transparent, the layers conferring on the whole of the properties for example optical (blur, diffusion, absorption of light, coloration %) and / or thermal (low-emissivity, control solar -reflection of part of solar radiation -%) and / or electrical (conductivity %) and / or catalytic (self-cleaning ).
  • TCO transparent conductive oxide
  • CVD chemical vapor deposition
  • the disadvantage of the thermal CVD comes from the fact that, since the glass is hot, the layer obtained is generally well crystallized, that is to say predominantly contains relatively large crystallites, and thus has a non-zero roughness on the surface.
  • Roughness here refers, in common, the height between the highest points of an irregular surface (vertices) and the lowest (valleys). This surface roughness results in a high blur value that is sought to avoid in certain applications, in which it is considered aesthetically unpleasant or visually troublesome.
  • the well-crystallized layer obtained has surface irregularities forming sharp-edged asperities which may hinder or even prevent cleaning of the surface.
  • the invention which relates to a glass substrate, characterized in that it is provided with a layer consisting of crystallites of at least 25 nm, directly covered with a layer consisting of crystallites of at most 10 nm.
  • a layer consisting of crystallites of at least 25 nm, or at most 10 nm is mainly composed of crystallites whose largest dimension is such.
  • a layer consisting of crystallites of at least 25 nm results from thermal CVD deposition on glass usually at about 600 ° C.
  • the two layers of the glass substrate of the invention consist of identical or different materials.
  • the size of the crystallites is here determined from the X-ray diffraction measurements (XRD) carried out on the crystallized layers.
  • XRD X-ray diffraction measurements
  • the X-ray diffraction apparatus is used in theta-theta mode on a plane parallel to the surface of the sample.
  • the indicated size is the minimum size for 25 nm, respectively maximum for 10 nm, among the sizes obtained for each of the diffraction peaks.
  • the thickness of the layer consisting of crystallites of at most 10 nm can reach values of 700 nm, or even up to 2 ⁇ .
  • the thickness of the crystallite layer of at least 25 nm is not limited; it is for example at most equal to 2, preferably 1, 5 ⁇ ; and a minimum average thickness of the order of the size of the crystallites (from 25 nm) is conceivable.
  • the thickness of the layer of crystallites of at most 10 nm is at most equal to 350, preferably 250 nm; the inventors have found that a maximum thickness of 350 nm of coating consisting of crystallites of at most 10 nm provides a desired effective smoothing of an underlying functional layer deposited by thermal CVD, by decreasing or even eliminating the surface roughness and / or rounding out small pointed growths with possible maintenance of the roughness in this case; this effect is still obtained at thicknesses of this layer of 100 nm, and even up to thicknesses of this layer of 10 or even 5 nm;
  • the glass substrate is directly covered with a barrier layer vis-à-vis the migration of alkali glass;
  • the barrier layer is therefore under the layer consisting of crystallites of at least 25 nm, either directly or with the interposition of one or more other layers;
  • the function of the barrier layer is to prevent the contamination of the upper layers by the sodium ions of the glass, when the glass is in particular conditions, especially at elevated temperature; it may consist of silica or silicon oxycarbide SiOC;
  • the layer of crystallites of at least 25 nm on the one hand, of at most 10 nm on the other hand, is a transparent oxide layer, electroconductive or not; examples of transparent conductive oxides Sn0 2 : F, SnO 2 : Sb, ZnO: Al, ZnO: Ga, InO: Sn, ZnO: 1n, and examples of non-conductive transparent oxides Sn0 2 , ZnO, InO; the transparent oxide constituting these layers can be photocatalytic, such as Ti0 2 , that is to say have properties of radical oxidizing initiator under solar radiation (hydrocarbon degradation properties, self-cleaning).
  • the invention also relates to
  • a method of manufacturing a glass substrate defined above in which the layers consisting of crystallites of at least 25 nm, respectively at most 10 nm, are formed by chemical vapor deposition at a temperature of the substrate relatively high (especially at least 500, preferably 550 ° C), respectively relatively low (in particular at least equal to 300 ° C and at most equal to 550, preferably 500 ° C);
  • a glass substrate described above in a photovoltaic cell electrode in which the layer composed of crystallites of at most 10 nm rounds and / or softens the surface irregularities with acute angles and / or spikes the layer consisting of crystallites of at least 25 nm, but without necessarily reducing its roughness, and is coated with amorphous or microcrystalline silicon as an absorbent;
  • the crystallite layer of at most 10 nm has a flat surface (zero roughness), and is coated with CdTe as absorbent;
  • the relatively conductive layer such as Sn0 2 : F consisting of crystallites of at least 25 nm is then covered with the layer of crystallites of at most 10 nm, necessarily non-conductive (in English "buffer layer"), such as Sn0 2 , which is advantageously flat and smooth because CdTe, absorbing relatively large amounts of light, does not require light trapping by the underlying layers; and
  • the substrate consists of 4 mm thick float soda-lime glass sold under the registered trade name Planilux® by Saint-Gobain Glass France, provided with a 25 nm SiOC layer constituting a barrier against the migration of alkaline glass.
  • the first deposit is made under the following conditions:
  • Substrate running speed (direction perpendicular to the width): 12 m / min
  • Air flow (80% nitrogen, 20% oxygen by volume) total: 1,195 l / min.
  • a 400 nm thick layer consisting of Sn0 2 crystallites of at least 25-30 nm is obtained.
  • the blur of the coated substrate is 17%.
  • the second deposit is made under the following conditions:
  • Substrate temperature 450 ° C
  • a second 150 nm thick layer consisting of Sn0 2 crystallites of about 6 nm is obtained.
  • the blur of the substrate coated with the layers of the first and second deposits is 17.1%.
  • the layer of the second deposit maintained the properties of the substrate before it was deposited.
  • the only modification was the smoothing of the surface facilitating its cleaning; it is found that a cloth-type cleaning means is no longer hooked by the asperities with sharp corners of the surface, which have been more or less covered and / or rounded.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • General Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Surface Treatment Of Glass (AREA)
  • Photovoltaic Devices (AREA)
  • Laminated Bodies (AREA)
EP12718284.8A 2011-04-04 2012-03-30 Glassubstrat mit leicht rauer schicht Withdrawn EP2694448A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1152873A FR2973366A1 (fr) 2011-04-04 2011-04-04 Substrat verrier a couche faiblement rugueuse
PCT/FR2012/050690 WO2012136919A1 (fr) 2011-04-04 2012-03-30 Substrat verrier a couche faiblement rugueuse

Publications (1)

Publication Number Publication Date
EP2694448A1 true EP2694448A1 (de) 2014-02-12

Family

ID=46025772

Family Applications (1)

Application Number Title Priority Date Filing Date
EP12718284.8A Withdrawn EP2694448A1 (de) 2011-04-04 2012-03-30 Glassubstrat mit leicht rauer schicht

Country Status (10)

Country Link
US (1) US20140116412A1 (de)
EP (1) EP2694448A1 (de)
JP (1) JP5992993B2 (de)
KR (1) KR20140009431A (de)
CN (1) CN103459344B (de)
BR (1) BR112013023979A2 (de)
EA (1) EA025612B1 (de)
FR (1) FR2973366A1 (de)
MX (1) MX347045B (de)
WO (1) WO2012136919A1 (de)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105408270B (zh) * 2013-03-08 2018-10-09 康宁公司 分层透明导电氧化物薄膜

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5900275A (en) * 1992-07-15 1999-05-04 Donnelly Corporation Method for reducing haze in tin oxide transparent conductive coatings

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2738813B1 (fr) * 1995-09-15 1997-10-17 Saint Gobain Vitrage Substrat a revetement photo-catalytique
US6596398B1 (en) * 1998-08-21 2003-07-22 Atofina Chemicals, Inc. Solar control coated glass
JP2001002449A (ja) * 1999-04-22 2001-01-09 Nippon Sheet Glass Co Ltd 低放射ガラスと該低放射ガラスを使用したガラス物品
US6171646B1 (en) * 1999-12-09 2001-01-09 Engineered Glass Products, Llc Method for making an abrasion and scratch resistant coated glass article
FR2838735B1 (fr) * 2002-04-17 2005-04-15 Saint Gobain Substrat a revetement auto-nettoyant
CN102311236B (zh) * 2003-12-26 2015-02-04 积水化学工业株式会社 夹层玻璃用中间膜和夹层玻璃
FR2944148B1 (fr) * 2009-04-02 2012-03-02 Saint Gobain Procede de fabrication d'une structure a surface texturee pour dispositif a diode electroluminescente organique et structure a surface texturee obtenue par ce procede

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5900275A (en) * 1992-07-15 1999-05-04 Donnelly Corporation Method for reducing haze in tin oxide transparent conductive coatings

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
THANGARAJU B ED - AOUADI SAMIR BROITMAN ESTEBAN FIGUEROA CARLOS FRANZ ROBERT VEPREK STAN STÜBER MICHAEL: "Structural and electrical studies on highly conducting spray deposited fluorine and antimony doped SnO2 thin films from SnCl2 precursor", THIN SOLID FILMS, ELSEVIER-SEQUOIA S.A. LAUSANNE, CH, vol. 402, no. 1-2, 1 January 2002 (2002-01-01), pages 71 - 78, XP004329936, ISSN: 0040-6090, DOI: 10.1016/S0040-6090(01)01667-4 *
XIAO ZHI ET AL: "The morphological, optical and electrical properties of SnO2:F thin films prepared by spray pyrolysis", SURFACE AND INTERFACE ANALYSIS., vol. 40, no. 2, 1 February 2008 (2008-02-01), GB, pages 67 - 70, XP055252593, ISSN: 0142-2421, DOI: 10.1002/sia.2693 *
YADAV A A ET AL: "Electrical, structural and optical properties of SnO2:F thin films: Effect of the substrate temperature", JOURNAL OF ALLOYS AND COMPOUNDS, ELSEVIER SEQUOIA, LAUSANNE, CH, vol. 488, no. 1, 20 November 2009 (2009-11-20), pages 350 - 355, XP026783646, ISSN: 0925-8388, [retrieved on 20090901], DOI: 10.1016/J.JALLCOM.2009.08.130 *

Also Published As

Publication number Publication date
JP5992993B2 (ja) 2016-09-14
US20140116412A1 (en) 2014-05-01
EA201391462A1 (ru) 2014-02-28
WO2012136919A1 (fr) 2012-10-11
EA025612B1 (ru) 2017-01-30
JP2014511817A (ja) 2014-05-19
CN103459344B (zh) 2017-03-01
MX347045B (es) 2017-04-10
MX2013011446A (es) 2013-10-17
FR2973366A1 (fr) 2012-10-05
BR112013023979A2 (pt) 2016-12-13
CN103459344A (zh) 2013-12-18
KR20140009431A (ko) 2014-01-22

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