EP2593302A1 - Procédé servant à améliorer des vitrages de protection thermique en empêchant la corrosion du verre due aux attaques alcalines et en fournissant un apprêt - Google Patents

Procédé servant à améliorer des vitrages de protection thermique en empêchant la corrosion du verre due aux attaques alcalines et en fournissant un apprêt

Info

Publication number
EP2593302A1
EP2593302A1 EP11731239.7A EP11731239A EP2593302A1 EP 2593302 A1 EP2593302 A1 EP 2593302A1 EP 11731239 A EP11731239 A EP 11731239A EP 2593302 A1 EP2593302 A1 EP 2593302A1
Authority
EP
European Patent Office
Prior art keywords
oxide
glass
zinc
aluminum
zirconium
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Withdrawn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
EP11731239.7A
Other languages
German (de)
English (en)
Inventor
Horst Seidel
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.)
Gevartis AG
Original Assignee
Gevartis AG
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 Gevartis AG filed Critical Gevartis AG
Publication of EP2593302A1 publication Critical patent/EP2593302A1/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Withdrawn legal-status Critical Current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
    • 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
    • C03C17/245—Oxides by deposition from the vapour phase
    • C03C17/2453—Coating containing SnO2
    • 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
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/069—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of intumescent 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
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/245—Oxides by deposition from the vapour 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
    • 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
    • C03C2217/211—SnO2
    • 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
    • C03C2217/216—ZnO
    • 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
    • C03C2217/23—Mixtures
    • 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
    • C03C2218/154—Deposition methods from the vapour phase by sputtering
    • C03C2218/155—Deposition methods from the vapour phase by sputtering by reactive sputtering

Definitions

  • the present invention relates to a method for reducing or preventing alkaline glass attack by surface treatment, preferably while improving the properties in case of fire.
  • the aim of the present invention was therefore to reduce the glass corrosion in fire protection or heat protection glazings, without having to change to more expensive glasses, or the provision of such glazing.
  • This objective has been achieved by providing fire-resistant glazings or elements which are more corrosion-resistant or corrosion-resistant by the use of glass plates provided with a special surface treatment.
  • Another object of the invention is a method for producing such surface-modified glasses.
  • fire protection and heat protection are used interchangeably in the context of the present invention.
  • a translucent and preferably transparent fire protection element according to the invention has at least two glass panes, between which there is at least one transparent fire-resistant protective layer made of a hardened and water-containing alkali polysilicate.
  • a suitable protective layer usually an intumescent layer, has a SiC> 2: alkali metal oxide (Me 2 O) ratio of at least 2: 1 and a water content of up to 60% by weight.
  • the glass surface which is in contact with the alkali polysilicate layer is provided according to the invention with a coating (a blocking layer or diffusion barrier layer) consisting essentially of oxides of polyvalent cations and their reaction product with the silicate of the glass surface, both the oxides and the oxides Reaction products in the alkaline medium are sparingly soluble, and the alkali-resistant blocker layer has a thickness of less than 100 nm.
  • a coating consisting essentially of oxides of polyvalent cations and their reaction product with the silicate of the glass surface, both the oxides and the oxides Reaction products in the alkaline medium are sparingly soluble, and the alkali-resistant blocker layer has a thickness of less than 100 nm.
  • the oxides and / or their reaction products with the silicate of the glass surface are sparingly soluble compounds that the coated side of a glass sheet is left to stand for 24 hours at 60 ° C. can be exposed to medium of pH 12, in particular even pH 13, without subsequently a glass attack is detected by light microscopic observation.
  • the coating materials are also referred to as network formers or network converters. These are oxides of polyvalent cations which, as such, are sparingly soluble compounds in the alkaline range or form sparingly soluble compounds by reaction with the glass surface in the alkaline region and which act as blocking or diffusion barrier layers which are present in the glass / glass interface.
  • Protective layer preferably reduces or preferably prevents ion exchange of sodium and potassium ions for hydrogen ions or of sodium ions for potassium ions, and blocks competition adsorption of hydroxide ions and in particular of the foreign ions sodium and potassium.
  • CVD Chemical Vapor Deposition
  • sol-gel methods sol-gel methods
  • the coating is preferably carried out by immersion using a suitable precursor (eg for aluminum: aluminum (2-propylate), aluminum (2-butoxide), for zirconium: zirconium propylate or for titanium: Titanium ethylate, titanium (2-propylate), iCl2Et2), at a certain dip angle and at a certain speed and preferably at a temperature of about 25 ° C -30 ° C and a humidity of 8-10 g / cm ⁇ .
  • the metal alkoxides react with water to form M-OH groups, which crosslink with each other by dehydration condensation Kgs ⁇ NEN.
  • the coating process is followed by a drying at about 175 ° C, then an annealing at temperatures of about 450 ° C to a maximum of about 500 ° C, in particular up to a maximum of about 480 ° C with subsequent controlled cooling.
  • Both the CVD and the sol-gel process have the disadvantage that they depend on special output products, in the CVD method on volatile compounds, in the sol-gel process on hydroxy-convertible metal-containing precursors.
  • reactive sputtering allows virtually any composition, as it is primarily determined by the metal or the alloy of the target.
  • the coating method such as the reactive sputtering, CVD or 'sol-gel method, a heat treatment or a thermal tempering can downstream be turned on. These processes improve the adhesion, chemistry and cohesiveness of the blocker layer on the substrate and, at thermal tempering, improve the glass quality at the same time. Suitable conditions are:
  • Zinc oxide-containing mixed oxides such as zinc aluminum oxide (ZnAlO x ),
  • Zincates, stannates and zirconates particularly with more ⁇ valent cations selected from aluminum, boron, bismuth, titanium, zinc, tin and zirconium.
  • ZnA10 x Aluminum doped compounds such as Zn x Sny_
  • Preferred blocking layers include tin oxide
  • Sn02 alumina (Al2O3), bismuth oxide (B12O3), titanium oxide (T1O2), zinc oxide (ZnO), zirconium carbide (ZrC> 2), boron oxide (B2O3) or their mixtures, zinc oxide-containing mixed oxides, such as zinc aluminum oxides (ZnA10 x) , Aluminum-doped compounds such as Zn x SnyAl z O n , zinc stannates (ZnSnO x ), cerium aluminates, zirconium aluminates, zirconium borates and / or Zirkonzinkate.
  • Especially preferred blocker layers are layers of tin oxide (SnC> 2), alumina
  • Al2O3 bismuth oxide (B12O3), titanium oxide (Ti02), zinc oxide (ZnO), zirconium oxide (Zr02) and mixtures thereof, zinc oxide-containing mixed oxides and particularly aluminum doped compounds, such as Zn x SnyAl z O n, zirconates or Zinkstan- naten (ZnSnO x ).
  • Preferred overall layer thicknesses of one or more blocker layer (s) arranged one above the other are in the range from 10 to 100 nm, preferably from 10 to 60 nm and in particular from 10 to 30 nm.
  • the inventive fire-resistant glazings can be produced by either coating a glass sheet with a casting material which is curable to a water-containing alkali polysilicate having a SiC> 2: Me20 ratio of at least 2: 1 and a water content of up to 60% by weight, whereupon above this casting material before, during or after curing, a second glass pane is placed, or wherein two or more panes of glass are edge-sealed at a distance from each other (eg, except at least one fill opening), and the at least one space formed therein is filled with the hardenable casting material, and then cured;
  • the glass sheets are provided on at least one side and preferably at least on the air side with a blocking layer and the glass sheets are arranged such that their blocker layer provided side (s) in contact with the optionally cured to the protective layer casting material.
  • the air side is the side of the glass which has been turned away from the tin bath during manufacture.
  • the tin bath facing side is referred to as the bath side.
  • a protective layer together with the glasses provided with blocking layer (s) are layers which are produced from nanoparticulate SiO 2 in the form of dispersions of pyrogenic SiO 2, precipitated silica, silica sol and mixtures of 2 or all 3 of these SiO 2 s, and alkali metal hydroxide , especially potassium hydroxide.
  • layers are described in WO 2009/155719, the disclosure of which is included here in its entirety.
  • the blocking layer is applied by means of a reactive DC, HC and / or magnetron sputtering process and is especially preferably subsequently tempered.
  • Example 1 Preparation of a glass provided with a stannate layer
  • Blocker layer In a continuous flow industrial magnetron plant, a blocking layer was applied to the fire side by means of reactive sputtering (with the fire side the non-tin bath side facing away from the tin bath). Blocker layer can also be understood as a multilayer coating. According to prior art methods (e.g., EP 1 889 818), various layers were applied to 5mm thick float glass sheets, namely:
  • Ultra Turrax stirrer as disperser, which works according to a rotor / strator principle.
  • this solution was stirred for about 5 minutes until homogeneous. While dispersing with an Ultraturrax stirrer, 4.7 kg of silica powder was slowly added to the solution. The dispersion was continued until a homogeneous dispersion had formed.
  • silica sol BET 50 m 2 / g, primary particle size 55 nm, 50% S1O2 in water, adjusted to pH 9 to 11 with KOH
  • the mixture was stirred for about 5 minutes to homogeneity and then heated with further heating with the heating module to about 50 - 60 ° C. This temperature was maintained, the sol brought un ⁇ ter vacuum to boiling and 1.96 kg of water let ⁇ evaporated. Subsequently, the mixture was cooled down to 20 ° C without vacuum.
  • Example 3 Differences of properties with coated / uncoated glasses and with respect to the tin bath side.
  • a weight-loaded needle is pulled over the layer at a defined speed.
  • the weight at which scratch marks are visible serves as a measure of the scratch hardness.
  • the samples are exposed for 140 h at a temperature of 60 ° C at a relative humidity of 100%.
  • the measurement is carried out according to the plate method according to Kimmel et al. Z. Glastechnische Berichte 59 (1986) p. 252 et seq.
  • the glass sample is immersed for 8 min in 0.01 N HCl of 38 ° C and found the loss of emissivity in%.
  • the glass sample is immersed as in G in hydrochloric acid.
  • the assessment criterion is the visibility of the immersion edge.
  • the coated side of the samples is brought into contact with a thin film of water for 24 hours.
  • the test allows a statement about the storage behavior of coated and stacked glass panes when traces of water get between the panes of glass. The assessment is done visually. Examined samples:
  • Zinc stannate (ZnSnO x ) of 30 nm thickness obtained with target of the composition about 53 wt .-% zinc and 47 wt .-% tin.
  • Blocker or diffusion barrier layer Tin oxide (Sn.C> 2) of 40 nm thickness obtained with target of 100 wt .-% tin.
  • Blocker or Diffusion Barrier Layer Glass Side Tin oxide (SnO 2) of 40 nm obtained with target of 100 wt% tin and over it applied an additional barrier layer of 3 nm thickness of Zn x Sn y Al z O n obtained with a target of composition 68 % By weight of Zn, 30% by weight of Sn and 2% by weight of Al.
  • > 6 days refers to glass that is older than 6 days and has been stored and transported. The actual age is estimated at about 1 month previous trial period, trial continues
  • the alkaline glass attack by the heat / fire protection layer shows up in the form of white spots and bands (in the case of previously damaged glass surfaces) and less severe cloudiness and clouds on the surfaces

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)
  • Joining Of Glass To Other Materials (AREA)

Abstract

L'invention concerne un élément pare-feu translucide et de préférence transparent, comportant au moins deux vitres entre lesquelles se trouve au moins une couche de protection transparente, résistante au feu, constitué d'un polysilicate alcalin aqueux durci, la surface de verre respective en contact avec la couche de protection étant pourvue d'un revêtement résistant aux alcalins (couche de blocage) d'une épaisseur inférieure à 100 nm, constitué sensiblement d'oxydes de cations polyvalents et de leur produit de réaction avec le silicate de la surface de verre. Ces couches sont de préférence appliquées par pulvérisation cathodique réactive et servent d'une part à réduire (voire empêcher) la corrosion du verre, et d'autre part d'apprêt améliorant le comportement de cassure en cas d'incendie et donc augmentant la capacité de résistance au feu.
EP11731239.7A 2010-07-16 2011-06-16 Procédé servant à améliorer des vitrages de protection thermique en empêchant la corrosion du verre due aux attaques alcalines et en fournissant un apprêt Withdrawn EP2593302A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH11642010 2010-07-16
PCT/CH2011/000148 WO2012006748A1 (fr) 2010-07-16 2011-06-16 Procédé servant à améliorer des vitrages de protection thermique en empêchant la corrosion du verre due aux attaques alcalines et en fournissant un apprêt

Publications (1)

Publication Number Publication Date
EP2593302A1 true EP2593302A1 (fr) 2013-05-22

Family

ID=44343001

Family Applications (1)

Application Number Title Priority Date Filing Date
EP11731239.7A Withdrawn EP2593302A1 (fr) 2010-07-16 2011-06-16 Procédé servant à améliorer des vitrages de protection thermique en empêchant la corrosion du verre due aux attaques alcalines et en fournissant un apprêt

Country Status (3)

Country Link
EP (1) EP2593302A1 (fr)
TW (1) TW201213260A (fr)
WO (1) WO2012006748A1 (fr)

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2557141B1 (fr) 2011-08-10 2015-04-08 AMATO GmbH Brandschutzsysteme Elément anti-incendie formé de manière plate, son procédé de fabrication et son utilisation
DE102012200799A1 (de) * 2011-09-26 2013-03-28 Interpane Entwicklungs-Und Beratungsgesellschaft Mbh Brandschutzelement mit Schutzbeschichtung und dessen Herstellungsverfahren
US11497681B2 (en) 2012-02-28 2022-11-15 Corning Incorporated Glass articles with low-friction coatings
US10737973B2 (en) 2012-02-28 2020-08-11 Corning Incorporated Pharmaceutical glass coating for achieving particle reduction
SG11201405220WA (en) 2012-02-28 2014-09-26 Corning Inc Glass articles with low-friction coatings
US9988174B2 (en) 2012-06-07 2018-06-05 Corning Incorporated Delamination resistant glass containers
US10273048B2 (en) 2012-06-07 2019-04-30 Corning Incorporated Delamination resistant glass containers with heat-tolerant coatings
US9034442B2 (en) 2012-11-30 2015-05-19 Corning Incorporated Strengthened borosilicate glass containers with improved damage tolerance
US10117806B2 (en) * 2012-11-30 2018-11-06 Corning Incorporated Strengthened glass containers resistant to delamination and damage
WO2014086570A1 (fr) * 2012-12-06 2014-06-12 Saint-Gobain Glass France Vitre dotée d'au moins une couche de protection contenant de l'oxyde d'étain et de zinc
HUE030780T2 (en) 2012-12-06 2017-06-28 Saint Gobain Fire protection plate and fire protection glazing
EP2949463A1 (fr) * 2014-05-28 2015-12-02 Saint-Gobain Glass France Vitre de protection contre l'incendie et vitrage de protection contre l'incendie
DE102014108372A1 (de) * 2014-06-13 2015-12-17 Promat Gmbh Brandschutzscheibe und Verfahren zu deren Fertigung
CA2959666C (fr) 2014-09-05 2021-03-16 Corning Incorporated Articles en verre et procedes pour ameliorer la fiabilite d'articles en verre
MX2017006945A (es) 2014-11-26 2017-08-16 Corning Inc Metodos para producir recipientes de vidrio fortalecidos y durables.
EP3150564B1 (fr) 2015-09-30 2018-12-05 Corning Incorporated Compositions chimiques à base de polyimide-siloxane halogéné et articles en verre avec des revêtements à faible frottement en polylmide-siloxane halogéné
CN113214740B (zh) * 2021-06-03 2022-07-26 亚士漆(上海)有限公司 光反射透明隔热涂料及制备方法和光反射隔热罩面

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DE19731416C1 (de) 1997-07-22 1998-09-17 Vetrotech Saint Gobain Int Ag Brandschutzverglasung
GB9721812D0 (en) * 1997-10-15 1997-12-17 Glaverbel Transparent heat-swellable material
EP1398147A1 (fr) * 2002-09-13 2004-03-17 Scheuten Glasgroep Unité de vitrage pare-feu
BE1016494A3 (fr) * 2005-04-15 2006-12-05 Glaverbel Vitrage anti-feu.
DE502006008443D1 (de) 2006-08-08 2011-01-13 Scheuten Glasgroep Bv Temperbares Low-e-Schichtsystem; Verfahren zur Herstellung und Low-e-Glasprodukt mit Schichtsystem
EP1961555A1 (fr) * 2007-02-21 2008-08-27 AGC Flat Glass Europe SA Vitrage pare-flamme
WO2009155714A1 (fr) 2008-06-26 2009-12-30 Gevartis Ag Matériaux pour la fabrication d'éléments de protection thermique transparents, éléments de protection contre la lumière produits avec de tels matériaux et procédé de fabrication

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Also Published As

Publication number Publication date
TW201213260A (en) 2012-04-01
WO2012006748A1 (fr) 2012-01-19

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