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EP2454211A1 - Procédé de production d'une vitre dotée d'un revêtement et antireflet - Google Patents

Procédé de production d'une vitre dotée d'un revêtement et antireflet

Info

Publication number
EP2454211A1
EP2454211A1 EP10729898A EP10729898A EP2454211A1 EP 2454211 A1 EP2454211 A1 EP 2454211A1 EP 10729898 A EP10729898 A EP 10729898A EP 10729898 A EP10729898 A EP 10729898A EP 2454211 A1 EP2454211 A1 EP 2454211A1
Authority
EP
European Patent Office
Prior art keywords
optically transparent
electrically conductive
conductive layer
glass substrate
layer
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Withdrawn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
EP10729898A
Other languages
German (de)
English (en)
Inventor
Marcus Neander
Katja Werner
Bianca Bergs
Marc Maurer
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 EP2454211A1 publication Critical patent/EP2454211A1/fr
Withdrawn legal-status Critical Current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
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • 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
    • 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
    • C03C2217/24—Doped oxides
    • C03C2217/241—Doped oxides with halides
    • 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
    • C03C2217/73—Anti-reflective coatings with specific characteristics
    • C03C2217/732—Anti-reflective coatings with specific characteristics made of a single 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
    • C03C2217/77—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

Definitions

  • the invention relates to a method for producing a coated and reflection-reduced disc, a disc produced by the method according to the invention and their use.
  • the reflection reduction of slices is in many cases based on the creation of a porous, structured layer on the glass surface.
  • This porous, structured layer can be produced by etching with a suitable acid or base.
  • a porous SiO 2 layer can be produced by deposition of SiO 2 on the glass surface, for example in a sol-gel process. Combinations of the two methods of etching and deposition are also possible.
  • the reflection-reducing properties are also of importance in the case of panes with optically transparent, electrically conductive coatings, such as, for example, transparent conductive oxides (TCO).
  • TCO transparent conductive oxides
  • the porous, structured layer on the glass surface often requires additional and adapted process steps.
  • the surface structure of a previously etched disk changes the deposition of the optically transparent, electrically conductive layer in many cases. This adjustment and, if necessary, amendment of Process conditions during the deposition of the optically transparent, electrically conductive coating make the production of the coated pane more expensive.
  • US 2,486,431 A discloses a method for producing a low-reflective glass surface.
  • the glass surface is etched with an H 2 SiF 6 solution. Depending on the duration of the etching process, the glass surface is removed to varying degrees and thus the optical properties of the surface are adjusted and varied.
  • DE 822 714 B discloses a method for producing a reflection-reducing film on the surface of a glass article.
  • the glass article is immersed in a solution of H 2 SiF 6 and colloidally dissolved SiO 2 .
  • the wafer surface is ablated (etched) and / or built up.
  • EP 1 056 136 B1 discloses a substrate for a solar cell comprising at least a glass plate, a first and second base coating film and a conductive film.
  • the first base coat film contains at least metal oxides such as tin oxide, titanium oxide, indium oxide or zinc oxide.
  • US2008 / 0314442 A1 discloses a transparent substrate with an optically transparent electrode consisting of at least two layers.
  • the first transparent, electrically conductive layer contains a non-doped metal oxide, such as tin oxide.
  • the second transparent, electrically conductive layer in contrast, contains a doped metal oxide.
  • US2008 / 0308146 A1 discloses a photovoltaic article having a front electrode on a textured glass substrate.
  • the texturing of the glass substrate is carried out before the application of the front electrode by a mechanical roller at 570 0 C to 750 0 C or by etching with an acid.
  • the front electrode is then applied via a pyrolysis process.
  • the object of the invention is to provide a method for producing a coated and reflection-reduced disc, which allows a coating of the disc with an optically transparent, electrically conductive coating regardless of the existing or later texturing of the disc.
  • the object of the present invention is achieved by an optically transparent glass pane, process for their preparation, and their use according to the independent claims 1, 13 and 15. Preferred embodiments will become apparent from the dependent claims.
  • the method for producing a coated, reflection-reduced pane comprises, in a first step, the application of an optically transparent, electrically conductive layer on at least a portion of the surface of a glass substrate.
  • This optically transparent, electrically conductive layer preferably has an average transmission of more than 75%, preferably more than 80% (as energy transmission according to DIN-EN 410: 1998) for light of wavelengths from 300 nm to 1300 nm.
  • an antireflection layer is formed on the uncoated surface of the glass substrate by applying a solution of an acid and / or base to the surface of the glass substrate.
  • the solution of an acid and / or base is preferably also applied to the surface of the glass substrate on the surface of the glass substrate provided with an optically transparent, electrically conductive layer.
  • the acid and / or alkali is preferably selected so that the glass surface is etched, but at the same time the optically transparent, electrically conductive layer is not attacked by the acid and / or alkali.
  • Metal oxides have, in particular, depending on their redox potential, a sufficient stability to acids and bases. This property can also be exploited for metallic layers which form corresponding passivated surfaces.
  • the antireflection layer is preferably produced by completely immersing the glass substrate containing the optically transparent electrically conductive layer in a solution of an acid and / or base. Completely includes in the context of the invention also not treated contact points of holding devices on the glass substrate with a.
  • the antireflection layer can alternatively also be produced in that a solution of an acid and / or base is sprayed onto the glass substrate with the optically transparent, electrically conductive layer.
  • the acid and / or base applied to the surface of the glass substrate preferably contains HF, H 2 SiF 6 , (SiO 2 ) m * nH 2 O, HCl, H 2 SO 4 , H 3 PO 4 , HNO 3 , CF 3 COOH, CCI 3 COOH, HCOOH, CH 3 COOH, NaOH, KOH, Ca (OH) 2 and / or mixtures thereof.
  • the acid and / or base applied to the surface of the glass substrate particularly preferably contains HF and / or H 2 SiF 6 . With these acids, particularly good results are achieved in the dipping process.
  • the optically transparent, electrically conductive layer is preferably applied by CVD (chemical vapor deposition), CLD (chemical liquid deposition), PVD (physical vapor deposition) and / or combinations thereof on the glass substrate.
  • the optically transparent, electrically conductive layer is particularly preferably applied by spraying method, pyrolysis method, sputtering, magnetron sputtering, sol-gel method, ion beam method, electron beam method, vapor deposition and / or combinations thereof on the glass substrate.
  • the optically transparent, electrically conductive layer preferably has a sheet resistance of ⁇ 20 ⁇ /, more preferably of ⁇ 15 ⁇ /, and most preferably of ⁇ 10 ⁇ / ⁇ .
  • the optically transparent, electrically conductive layer preferably has a haze of ⁇ 20%, preferably ⁇ 10%, particularly preferably ⁇ 5%, after the generation of the antireflection layer.
  • the optically transparent, electrically conductive layer preferably has a R.M.S roughness depth of 3 nm to 50 nm, preferably 5 nm to 20 nm, after the generation of the antireflection layer.
  • the R.M.S roughness (Root Mean Square) describes the root mean square of the roughness depth.
  • the R.M.S roughness depth is preferably determined using an AFM (Atomic Force Microscope) microscope.
  • the optically transparent, electrically conductive layer is preferably applied to the glass substrate with a layer thickness of 10 nm to 1500 nm, particularly preferably with a layer thickness of 400 nm to 800 nm.
  • the optically transparent, electrically conductive layer is preferably by application of tin-doped indium oxide (ITO), aluminum-doped zinc oxide (AZO), fluorine-doped tin oxide (FTO, SnO 2 : F), antimony-doped tin oxide (ATO, SnO 2 : Sb), silver, gold, tin, Tungsten, copper, silicon, carbon nanotubes and / or optically transparent, electrically conductive polymers and / or mixtures thereof.
  • ITO tin-doped indium oxide
  • AZO aluminum-doped zinc oxide
  • FTO, SnO 2 : F fluorine-doped tin oxide
  • ATO, SnO 2 : Sb antimony-doped tin oxide
  • silver gold, tin, Tungsten, copper, silicon, carbon nanotubes and / or optically transparent, electrically conductive polymers and / or mixtures thereof.
  • optically transparent, electrically conductive polymers preferably contain poly (3,4-ethylenedioxythiophene), polystyrene sulfonate, poly (4,4-dioctylcylopentadithiophene), iodo, 2,3-dichloro-5,6-dicyano-1,4-benzoquinone, mixtures and / or copolymers thereof.
  • the glass substrate preferably has an average transmission in the wavelength range from 300 nm to 1300 nm of> 80%, preferably of> 90%.
  • the antireflection layer preferably has an average transmission in the wavelength range from 300 nm to 1300 nm of> 80%, preferably of> 90%.
  • the antireflection layer is preferably produced with a layer thickness of 10 nm to 1000 nm, particularly preferably 50 nm to 200 nm. Good results are achieved in this layer thickness range.
  • the glass substrate preferably contains flat glass (float glass), quartz glass, borosilicate glass, soda lime glass and / or mixtures thereof. Good results are achieved with these glasses.
  • the glass substrate preferably contains 0.001% by weight to 0.05% by weight of Fe (III) as Fe 2 O 3 and / or 0.0005% by weight to 0.005% by weight of Fe (II) as FeO. These Fe (III) and Fe (II) concentrations are particularly advantageous.
  • a cover layer is preferably applied to the optically transparent, electrically conductive layer.
  • the cover layer may contain scratch-resistant layers such as Si 3 N 4 and / or acids and / or bases resistant polymers such as epoxy resins, etching and / or etching.
  • the glass substrate is preferably biased after the formation of the antireflection layer.
  • the biasing is preferably carried out as described in DE10 2009 025 788 A1.
  • the disc is heated to a temperature of 500 0 C to 800 0 C.
  • the heating of the disk is followed by rapid cooling (quenching, for example by a cold jet of air) the heated, etched disk.
  • the surface of the disk cools faster than the core zone, so that tensions form in the glass. The tensions increase the stability and strength of the glass. Heating and rapid cooling together form the tempering process of the process according to the invention.
  • the invention further relates to an optically transparent glass pane having an electrically conductive layer and an antireflection layer.
  • the glass pane comprises at least one optically transparent, electrically conductive layer on at least a portion of the surface of a glass substrate and an antireflection layer on the non-coated surface of the glass substrate.
  • the antireflection layer has a minimum light reflection of 0.5% to 7%, preferably 1% to 5%. The light reflection is determined at a wavelength of 300 nm to 1300 nm and a reflection angle of 1 ° to 40 °.
  • the optically transparent glass pane has the properties described above. The minimum light reflection of less than 7% and light reflection angle of less than 40 ° allow a high light transmission.
  • the invention further relates to an optically transparent glass pane obtained by the method according to the invention with an electrically conductive layer and an antireflection layer.
  • the invention further relates to the use of an optically transparent glass pane having an electrically conductive layer and an antireflection layer in photovoltaics, preferably in solar cells, screens, vehicle glazing and / or structural glazing.
  • FIG. 1 shows a cross section of the optically transparent glass pane according to the invention with an antireflection coating (1), glass substrate (2) and an optically transparent, electrically conductive layer (3) and
  • Figure 2 is a flow diagram of a preferred embodiment of the method according to the invention.
  • Figure 1 shows a cross section of the glass substrate (2) with the applied electrically conductive layer (3) and the anti-reflection layer (1).
  • the antireflection coating (1) lowers the proportion of the light reflected on the glass surface. This increases the proportion of light (transmission) which can pass through the glass substrate (2) and then the optically transparent, electrically conductive layer (3).
  • FIG. 2 shows a flow chart of a preferred embodiment of the method according to the invention.
  • the glass substrate (2) is provided on one side with an optically transparent, electrically conductive layer (3), in this case an optically transparent, conductive oxide (TCO).
  • TCO can be applied by various methods such as CVD or PVD, for example sputtering.
  • the layer thickness of the TCO is preferably 400 nm to 800 nm.
  • the TCO coating can be provided with an acid-resistant covering layer (4) depending on the acid used.
  • the glass substrate (2) with the TCO coating (3) is completely immersed in a hydrofluoric acid bath.
  • the hydrofluoric acid etches the uncoated glass surface of the glass substrate (2) and generates an antireflection coating (1) thereon.
  • the TCO layer (3) is not or only slightly attacked by the relatively weak acid HF, so that the TCO layer (3) shows no significant changes in its physical or chemical properties.
  • the now coated glass substrate (2) is then rinsed with distilled water and dried.
  • Example 1 In two series of experiments, the transmission, turbidity, efficiency increase and the sheet resistance of a disk produced by the process according to the invention (Example 1) and a comparative example (Example 2) were compared. Both discs (Example 1 and 2) containing a diamond ® glass (2) from Saint-Gobain Glass having a thickness of 3.2 mm. Both disks (Examples 1 and 2) contained on one side an optically transparent, electrically conductive SnO 2 : F layer (3) with a layer thickness of approximately 500 nm. The SnO 2 : F layer (3) was applied as in US2008 / 0314442 A1 described.
  • the disc produced by the process according to the invention was then precessed with an HF solution (2 wt.%) For 1 to 10 min, rinsed with deionized water and with H 2 SiF 6 (1, 25 mol / l) for Etched in a dip bath for 30 minutes to 120 minutes.
  • the pane according to the invention Example 1 was also completely immersed in the acid with the optically transparent, electrically conductive coating.
  • T ref transmission reference glass
  • T AR transmission of the disc according to the invention
  • N number of incident photons in the wavelength range ⁇ from 300 nm to 1300 nm.
  • the haze was determined using a Haze-Gard Plus (BYK Gardner GmbH, 82538 Geretsried, Germany).
  • the sheet resistance (rsq) was determined by the 4 point method.
  • the pane of the invention (Example 1) had a significantly higher transmission (T) and a significantly lower proportion of scattered light (R) than the comparative example (Example 2).
  • a high efficiency increase (E.I.) dependent on these quantities, was found to be 3.64%.
  • This Efficiency Increase (E.I) for example, has a direct effect on the efficiency of a solar module which uses a glass substrate according to the invention.
  • the constant sheet resistance (rsq) and the barely changing haze showed that the optically transparent, electrically conductive layer (3) was not attacked or abraded by the acid treatment.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

Procédé de production d'une vitre optiquement transparente, comprenant une couche électroconductrice et une couche antireflet, a- une couche électroconductrice (3) optiquement transparente étant appliquée sur au moins une zone partielle de la surface d'un substrat de verre (2) et b- une couche antireflet (1) étant produite sur la surface dépourvue de revêtement du substrat en verre (2), une solution d'un acide et/ou d'une base étant appliquée(s) sur la surface du substrat en verre (2).
EP10729898A 2009-07-17 2010-07-08 Procédé de production d'une vitre dotée d'un revêtement et antireflet Withdrawn EP2454211A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200910026197 DE102009026197B4 (de) 2009-07-17 2009-07-17 Optisch transparente Glasscheibe und deren Verwendung
PCT/EP2010/059805 WO2011006829A1 (fr) 2009-07-17 2010-07-08 Procédé de production d'une vitre dotée d'un revêtement et antireflet

Publications (1)

Publication Number Publication Date
EP2454211A1 true EP2454211A1 (fr) 2012-05-23

Family

ID=42799581

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10729898A Withdrawn EP2454211A1 (fr) 2009-07-17 2010-07-08 Procédé de production d'une vitre dotée d'un revêtement et antireflet

Country Status (4)

Country Link
EP (1) EP2454211A1 (fr)
CN (1) CN102471141A (fr)
DE (1) DE102009026197B4 (fr)
WO (1) WO2011006829A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103183480A (zh) * 2011-12-28 2013-07-03 上海北玻玻璃技术工业有限公司 Azo镀膜玻璃的制备方法
CN102795785B (zh) * 2012-09-10 2015-04-22 刘立强 减反射玻璃及二次酸腐蚀制备减反射玻璃的方法
CN109148608A (zh) * 2017-06-16 2019-01-04 联相光电股份有限公司 低反射率太阳能天窗装置及其制造方法
CN110981208A (zh) * 2019-12-17 2020-04-10 河南豫科光学科技股份有限公司 一种超白玻璃基板的制备工艺

Family Cites Families (9)

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Publication number Priority date Publication date Assignee Title
US2486431A (en) 1944-08-18 1949-11-01 Rca Corp Method of producing low-glare coatings
USB490662I5 (fr) 1946-09-21
JPS57210676A (en) * 1981-06-22 1982-12-24 Hoya Corp Substrate for electrode
CA2342910C (fr) * 1998-09-04 2008-08-05 Nippon Sheet Glass Co., Ltd. Verre de couleur claire a haute transmission et methode de fabrication connexe, vitre a film conductif utilisant ce verre et methode de fabrication connexe et article en verre
JP3227449B2 (ja) 1999-05-28 2001-11-12 日本板硝子株式会社 光電変換装置用基板とその製造方法、およびこれを用いた光電変換装置
FR2891269B1 (fr) 2005-09-23 2007-11-09 Saint Gobain Substrat transparent muni d'une electrode
US20080308146A1 (en) 2007-06-14 2008-12-18 Guardian Industries Corp. Front electrode including pyrolytic transparent conductive coating on textured glass substrate for use in photovoltaic device and method of making same
DE102008051730A1 (de) * 2008-10-15 2010-04-22 Saint-Gobain Sekurit Deutschland Gmbh & Co. Kg Transparenter Gegenstand mit einem örtlich begrenzten, strukturierten, elektrisch beheizbaren, transparenten Bereich, Verfahren zu seiner Herstellung und seine Verwendung
DE102009025788A1 (de) 2009-05-13 2010-11-25 Saint-Gobain Sekurit Deutschland Gmbh & Co. Kg Verfahren zur Herstellung einer reflexionsverminderten Scheibe

Non-Patent Citations (1)

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Title
See references of WO2011006829A1 *

Also Published As

Publication number Publication date
DE102009026197A1 (de) 2011-01-27
CN102471141A (zh) 2012-05-23
WO2011006829A1 (fr) 2011-01-20
DE102009026197B4 (de) 2013-05-02

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