WO2016028013A1 - Structure de stratification de verre présentant une transparence élevée et une surface conductrice et procédé de production associé - Google Patents

Structure de stratification de verre présentant une transparence élevée et une surface conductrice et procédé de production associé Download PDF

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Publication number
WO2016028013A1
WO2016028013A1 PCT/KR2015/008116 KR2015008116W WO2016028013A1 WO 2016028013 A1 WO2016028013 A1 WO 2016028013A1 KR 2015008116 W KR2015008116 W KR 2015008116W WO 2016028013 A1 WO2016028013 A1 WO 2016028013A1
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WIPO (PCT)
Prior art keywords
glass
dielectric barrier
barrier layer
layer
transparent dielectric
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PCT/KR2015/008116
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English (en)
Korean (ko)
Inventor
류도형
박성환
김병종
김보민
진은주
Original Assignee
(주)솔라세라믹
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Publication of WO2016028013A1 publication Critical patent/WO2016028013A1/fr

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    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports

Definitions

  • the present invention relates to a glass substrate, and more particularly, to a glass laminated structure having a high transparency and a conductive surface and a method of manufacturing the same.
  • a transparent conductive film is a film having light transmittance and electric conductivity, and is used in display fields such as liquid crystal displays, organic light emitting displays (OLEDs), or plasma display devices, touch panel fields, solar cell fields, or condensation prevention or heating. It is widely used in the field of heat generating resistors.
  • a conductive metal oxide such as tin indium oxide (ITO), tin oxide, or fluorine-doped tin oxide (FTO) is typical.
  • ITO tin indium oxide
  • FTO fluorine-doped tin oxide
  • the FTO conductive film not only has a high transparency but also has almost no resistance change up to 500 ° C., and has excellent chemical resistance and abrasion resistance and is suitable for harsh external environments, so that it can be applied to various fields. It is attracting attention as.
  • the FTO conductive film is coated on a glass substrate such as soda lime and applied.
  • a glass substrate such as soda lime
  • alkali oxide such as Na 2 O or K 2 O
  • alkali metal ions such as Na + or K + diffuse from the inside of the glass substrate to the surface, thereby forming on the glass substrate.
  • the technical problem to be solved by the present invention when applying a transparent conductive film on a glass substrate, to protect the transparent conductive film from impurities of the glass substrate, without sacrificing the thickness of the transparent conductive film, the glass substrate and the transparent conductive
  • the glass laminated structure which can improve the light transmittance of the laminated structure of a film
  • Another technical problem to be solved by the present invention is to provide a method for producing a glass laminated structure that can efficiently and economically produce a glass laminated structure having the aforementioned advantages.
  • the glass substrate A transparent dielectric barrier layer formed on the first side of the glass substrate; A transparent conductive layer comprising fluorine doped tin oxide (FTO) formed on the transparent dielectric barrier layer; And a material formed on a second surface opposite to the first surface of the glass substrate on which the transparent dielectric barrier layer is formed, and the same material as the transparent dielectric barrier layer.
  • FTO fluorine doped tin oxide
  • the glass substrate may include soda lime glass or low iron glass including Na 2 O and K 2 O.
  • the glass laminate structure may be used as a glass of automobiles, general window glass, or greenhouse glass.
  • the transparent dielectric barrier layer and the refractive index control layer may include at least one of SiO 2 , CeO 2 , Al 2 O 3 , MnO 2 , Fe 2 O 3, and TiO 2 .
  • the transparent dielectric barrier layer and the refractive index control layer may include SiO 2 .
  • the average thickness of the transparent dielectric barrier layer and the refractive index control layer may be in the range of 60 nm to 120 nm.
  • the sheet resistance of the transparent conductive layer is in the range of 7 ohm / sq to 20 ohm / sq.
  • a method of manufacturing a glass laminate structure comprising: providing a glass substrate; Forming a transparent dielectric barrier layer on the first side of the glass substrate; Forming a transparent conductive layer including a fluorine doped tin oxide layer (FTO layer) on the dielectric barrier layer; And forming a refractive index control layer comprising the same material as the transparent dielectric barrier layer on a second side opposite the first side of the glass substrate on which the dielectric barrier layer is formed.
  • FTO layer fluorine doped tin oxide layer
  • the glass substrate comprises sodalime glass or low iron glass comprising Na 2 O and K 2 O.
  • the forming of the transparent dielectric barrier layer and the forming of the refractive index control layer may be performed by immersing the glass substrate in a liquid raw material including the transparent dielectric barrier layer and the precursor of the refractive index adjusting layer. Coating the transparent dielectric barrier layer and the refractive index control layer on each side of the substrate; And drying and heat treating the coated result.
  • the thickness of the transparent dielectric barrier layer and the refractive index control layer may be controlled by adjusting the concentration of the precursor in the liquid raw material.
  • the transparent dielectric barrier layer and the refractive index control layer may include SiO 2 .
  • the liquid precursor of SiO 2 includes tetraethyl silicate ((C 2 H 5 ) 4 SiO 4 ), and an alcohol solvent.
  • the liquid raw material further includes nitric acid (HNO 3 ) as a catalyst.
  • the heat treatment may be performed in the range of 400 ° C to 550 ° C.
  • a transparent dielectric barrier layer on one main surface of the glass substrate to protect the transparent conductive film from impurities diffused out from the glass substrate, and the transparent dielectric barrier layer on the other main surface of the glass substrate
  • a refractive index adjusting layer including the same material as that, a glass laminate structure having improved light transmittance may be provided by symmetrically matching refractive indices on both sides of the glass substrate.
  • a method for producing a glass laminated structure that can efficiently and economically produce a glass laminated structure having the above-mentioned advantages by a liquid phase method.
  • FIG. 1 is a cross-sectional view of a glass laminate structure according to an embodiment of the present invention.
  • FIG. 2 is a graph illustrating a result of measuring light transmittance of a glass substrate having a transparent dielectric barrier layer of SiO 2 formed on both surfaces and a bare glass substrate and a glass laminate structure according to a comparative example, according to an embodiment of the present invention.
  • 3A shows the carrier concentration, mobility, and mobility of the transparent conductive film according to the sheet resistance of the transparent conductive layer of the FTO of the glass laminated structure according to the embodiment of the present invention, in which a dielectric barrier layer of SiO 2 is formed on both surfaces; And a graph showing resistivity.
  • 3B is a graph showing a measurement result of light transmittance of the glass laminate structure having various sheet resistances of FIG. 3A.
  • first, second, etc. are used herein to describe various members, parts, regions, layers, and / or parts, these members, parts, regions, layers, and / or parts are defined by these terms. It is obvious that not. These terms are only used to distinguish one member, part, region, layer or portion from another region, layer or portion. Thus, the first member, part, region, layer or portion, which will be discussed below, may refer to the second member, component, region, layer or portion without departing from the teachings of the present invention.
  • FIG. 1 is a cross-sectional view of a glass laminate structure 100 according to an embodiment of the present invention.
  • the glass laminate structure 100 includes a glass substrate 10, a transparent dielectric barrier layer 20 formed on a first surface of the glass substrate 10, for example, an upper surface, and a transparent dielectric barrier layer ( 20) and a transparent conductive layer 30 including fluorine doped tin oxide (hereinafter referred to as FTO) formed on.
  • the glass laminate structure 100 further includes a refractive index adjusting layer 40 formed on the second surface of the glass substrate 10, for example, the lower surface.
  • the glass laminated structure 100 is applicable to glass of a vehicle, general window glass, or greenhouse glass based on the electrical conductivity of the transparent conductive layer 30, the heat generating characteristic, and the high light transmittance accompanying it, as mentioned later.
  • the transparent conductive layer 30 may be patterned, and in this case, may be applied to a product such as a display glass or a touch panel.
  • the glass substrate 10 may be glass including an alkali metal oxide.
  • the glass substrate 10 may be, for example and not limited to, soda lime glass or low iron glass.
  • the alkali metal oxide may be Na 2 O or K 2 O, for example.
  • metal ions derived from the alkali metal oxide diffuse to the surface of the glass substrate 20 to resist the transparent conductive layer 20. Changes and deterioration of electrical durability may be caused, and the adhesion between the transparent conductive layer 20 and the glass substrate 20 may be weakened, resulting in a defect such as cracking or pill-off of the transparent conductive layer 20.
  • the transparent dielectric barrier layer 20 prevents alkali metal ions from diffusing into the transparent conductive layer 20, thereby providing electrical reliability of the transparent conductive layer 20 and a buffer layer between the transparent conductive layer 20 and the glass substrate 20. It also acts as a role to improve the interlayer adhesion.
  • the transparent dielectric barrier layer 20 is silicon oxide (SiO 2 ), ceria (CeO 2 ), aluminum oxide (Al 2 O 3 ) manganese oxide (MnO 2 ), iron oxide (Fe 2 O 3 ), It may include at least one of magnesium oxide (MgO) and titanium oxide (TiO 2 ).
  • the transparent dielectric barrier layer 20 may include silicon oxide (SiO 2 ), which is the same material as the refractive index control layer 40. These oxides are not necessarily stoichiometric and may lack or excess atomic ratios of oxygen relative to metallic elements.
  • the transparent dielectric barrier layer 20 can be formed by a liquid phase method.
  • the transparent dielectric barrier layer of SiO 2 includes, as starting material, a silicon precursor such as tetraethyl silicate ((C 2 H 5 ) 4 SiO 4 ) and an alcohol solvent for dispersion thereof.
  • the alcohol solvent is ethyl alcohol, methyl alcohol, glycerol, propylene glycol, isopropyl alcohol, isobutyl alcohol, polyvinyl alcohol, cyclohexanol, octyl alcohol, decanol, Hexatecanol, ethylene glycol, 1.2-octanediol, 1,2-dodecanediol, or 1,2-hexadecanediol, or mixtures thereof, preferably having a relatively low carbon content and nontoxic
  • water or distilled water may be further mixed in.
  • the concentration of the silicon precursor in the liquid solvent may be in the range of 0.1 to 0.4 mol%.
  • nitric acid HNO 3
  • the nitric acid catalyst promotes the oxidation reaction of silicon in the liquid phase method to improve the deposition rate of the transparent dielectric barrier layer 20 of SiO 2 .
  • the molar concentration of nitric acid in the liquid raw material may be about 0.1 mol% to 5 mol%.
  • a transparent dielectric barrier layer of SiO 2 may be formed by immersing a glass substrate in the liquid raw material, coating the liquid raw material on the glass substrate, and drying and sintering the liquid raw material.
  • the speed of immersing the glass substrate in the liquid raw material may be performed within a range of about 1 cm / min to about 10 cm / min.
  • the thickness of the transparent dielectric barrier layer 20 can be achieved by adjusting the concentration of the silicon precursor, eg, tetraethyl silicon oxide, in the liquid solution. As the concentration of the silicon precursor increases, the thickness of the transparent dielectric barrier layer 20 formed increases.
  • the molar concentration of the silicon precursor in the liquid raw material may be selected in the range of about 0.1 to 0.4 mol%.
  • the average thickness of the transparent dielectric barrier layer 20, preferably the transparent dielectric barrier layer of SiO 2 is in the range of 60 nm to 120 nm.
  • the transparent dielectric barrier layer 20, preferably, does not block the diffusion of the alkali metal ions when the average thickness of the transparent dielectric barrier layer of SiO 2 is less than 60 nm, and is deposited on top of it when it exceeds 120 nm. Cracks may occur in the transparent conductive layer 30 due to a difference between the transparent conductive layer 30 and the thermal expansion coefficient of the FTO, which may result in a defect.
  • the average thickness of the transparent dielectric barrier layer 20, preferably, the transparent dielectric barrier layer of SiO 2 is in the range of 80 nm to 100 nm.
  • Forming the transparent dielectric barrier layer of SiO 2 by immersing the glass substrate in the liquid raw material by the liquid phase method is the same component on both surfaces, that is, the first and second surfaces of the glass substrate 10, as described later.
  • the transparent dielectric barrier layer 20 and the refractive index control layer 40 having the same thickness can be simultaneously formed.
  • the transparent dielectric barrier layer 20 and the refractive index adjusting layer 40 having the same component can symmetrically match the refractive indices with respect to both surfaces of the glass substrate 10, thereby improving light transmittance of the glass laminate structure. It is a foundation.
  • the transparent conductive layer 30 of FTO on the transparent dielectric barrier layer 20 may have a crystalline (eg, polycrystalline), nanorod, nanowire or amorphous structure through a suitable deposition method and subsequent heat treatment process, The present invention is not limited to these examples.
  • Deposition of the transparent conductive layer 30 may be performed by spray pyrolysis deposition (SPD).
  • SPD spray pyrolysis deposition
  • the supply of the precursor for forming the transparent conductive layer may be made by ultrasonic spraying, spray spraying, or vaporization, but the present invention is not limited thereto.
  • the spray pyrolysis forms a droplet comprising a raw compound, and evaporation, high temperature reactions, thermal decomposition, reaction between carrier gas and precursor (e.g., a solvent contained in the droplet while the droplet is delivered through the droplet delivery flow path)
  • carrier gas e.g., a solvent contained in the droplet while the droplet is delivered through the droplet delivery flow path
  • the gas phase involves at least one or two or more steps of formation of clusters and formation of gas molecules (in this specification, intermediate products of each reaction step are collectively called gaseous precursors).
  • a precursor is a vapor deposition apparatus in which a thin film is formed by transferring a precursor onto a glass substrate on which a transparent dielectric barrier layer, which is a target object heated up to a deposition temperature, is formed.
  • the precursor solution for forming the FTO thin film is SnCl 4 5H 2 O, (C 4 H 9 ) 2 Sn (CH 3 COO) 2 , (CH 3 ) 2 SnCl 2 , or (C 4 H 9 ) 3 SnH as a tin precursor.
  • Compounds such as may be used.
  • the dopant fluorine precursor compounds such as NH 4 F, CF 3 Br, CF 2 Cl 2 , CH 3 CClF 2 , CF 3 COOH, or CH 3 CHF 2 can be used.
  • These precursors may be mixed with distilled water or alcohol to have a predetermined weight ratio F / Sn to prepare a liquid raw material, and then droplets may be generated.
  • the FTO thin film may be formed on the glass substrate by spraying a gaseous precursor onto the glass substrate after maintaining the temperature of the glass substrate as the workpiece.
  • the transparent conductive layer 30 of the FTO may be formed by a conventional atmospheric chemical vapor deposition method.
  • the refractive index adjusting layer 40 formed on the second surface of the glass substrate 10 may be formed of the same material as the transparent dielectric barrier layer 20.
  • the average thickness of the refractive index control layer 40 may be the same as the thickness of the transparent dielectric barrier layer 20.
  • the refractive index adjusting layer 40 having the same component as the transparent dielectric barrier layer 20 provides a layer having the same refractive index on both surfaces of the glass substrate 10, so that the refractive indices can be symmetrically matched. The light transmittance of the structure can be improved.
  • the red curve (E) is the measurement result of the glass substrate with the transparent dielectric barrier layer of SiO 2 formed on both sides
  • the blue curve (R1) is the measurement result of the bare glass substrate
  • the green curve (R2) is SiO 2 only on one surface. It is a measurement result of the glass substrate in which the transparent dielectric barrier layer of was formed.
  • the thickness of the glass substrate is about 0.7 mm and the thickness of the transparent dielectric barrier layer of SiO 2 has a thickness of about 100 nm.
  • the dielectric barrier layer of SiO 2 when the dielectric barrier layer of SiO 2 is formed on both sides of the glass substrate, an improvement in light transmittance may be obtained.
  • SiO 2 on both sides at a wavelength of 550 nm The layered glass substrate has a light transmittance of 94.1%, the bare glass substrate has a light transmittance of 90.7%, and the glass substrate having a transparent dielectric barrier layer of SiO 2 formed on only one surface has a light transmittance of 92.8%.
  • SiO 2 only on one side SiO 2 on both sides compared to forming a layer
  • an improvement in light transmittance of about 1.4% can be achieved. Referring to FIG. 2, it can be seen that the effect of improving the light transmittance obtained by forming the transparent dielectric barrier layer and the refractive index adjusting layer of the same material on both surfaces of the glass substrate is obtained in the entire visible light wavelength band.
  • FIG. 3A is a carrier concentration and hole mobility of a transparent conductive film according to sheet resistance of a transparent conductive layer of FTO having a glass laminated structure according to an embodiment of the present invention, in which dielectric barrier layers of SiO 2 are formed on both surfaces.
  • FIG. 3B is a graph showing a measurement result of light transmittance of the glass laminate structure having various sheet resistance of FIG. 3A.
  • the glass laminate structure having various sheet resistance structures has electrical property values as shown in Table 1 below.
  • Table 1 When the sheet resistance of the transparent conductive layer of FTO has a value in the range of about 7 ohm / sq to 20 ohm / sq, it can be seen that the light transmittance has a value of 80% or more at a wavelength of 550 nm (BL in FIG. 3B). .
  • Cotton Resistance (ohm / sq) Charge concentration (x10 20 cm-3) Hall mobility (cm2 / Vs) Resistivity (x10 - 4 ⁇ cm) Light transmittance (%, 550 nm) 3 2.8 45.74 4.87 67.5 5 6.84 43.33 2.11 77.7 7 4.09 41.61 3.62 83.7 10 3.38 41.71 4.43 85.5 20 5.39 26.91 4.31 86.6
  • the transparent conductive layer of the FTO of the glass laminate structure according to the above-described embodiment is formed or patterned entirely on a large area of glass to have an electrode structure suitable for the application.
  • a glass laminate structure having improved light transmittance may be provided by symmetrically matching refractive indices on both sides of a glass substrate.

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  • Laminated Bodies (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

La présente invention concerne une structure de stratification de verre ayant une transparence élevée et une surface conductrice, et un procédé de production associé. Une structure de stratification de verre selon un mode de réalisation de la présente invention comprend : un substrat de verre; une couche barrière diélectrique transparente qui est formée sur une première surface du substrat de verre ; une couche conductrice transparente qui est formée sur la couche barrière diélectrique transparente et comprend de l'oxyde d'étain dopé au fluor (FTO) ; et une couche de contrôle d'indice de réfraction qui est formée sur une seconde surface opposée à la première surface du substrat de verre sur lequel la couche barrière diélectrique transparente est formée, et qui comprend les mêmes matériaux que la couche barrière diélectrique transparente.
PCT/KR2015/008116 2014-08-21 2015-08-04 Structure de stratification de verre présentant une transparence élevée et une surface conductrice et procédé de production associé WO2016028013A1 (fr)

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KR1020140109302A KR101633987B1 (ko) 2014-08-21 2014-08-21 고투명도 및 도전성 표면을 갖는 유리 적층 구조 및 이의 제조 방법
KR10-2014-0109302 2014-08-21

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020021610A (ko) * 2000-09-14 2002-03-21 세야 히로미치 적층 유리
JP2003322702A (ja) * 2002-04-30 2003-11-14 Hamamatsu Photonics Kk 反射防止膜の製造方法並びに反射防止膜、空間光変調素子及び空間光変調装置
KR20080110756A (ko) * 2006-02-22 2008-12-19 쌩-고벵 글래스 프랑스 유기 발광 장치 및 유기 발광 장치의 투명 전기 전도층의 용도
JP4406237B2 (ja) * 2003-07-30 2010-01-27 株式会社ニデック 導電性を有する多層膜付透明基板の製造方法。
JP2013101309A (ja) * 2011-10-12 2013-05-23 Canon Inc エレクトロクロミック材料を用いた透過率可変素子、光学系および光学機器

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020021610A (ko) * 2000-09-14 2002-03-21 세야 히로미치 적층 유리
JP2003322702A (ja) * 2002-04-30 2003-11-14 Hamamatsu Photonics Kk 反射防止膜の製造方法並びに反射防止膜、空間光変調素子及び空間光変調装置
JP4406237B2 (ja) * 2003-07-30 2010-01-27 株式会社ニデック 導電性を有する多層膜付透明基板の製造方法。
KR20080110756A (ko) * 2006-02-22 2008-12-19 쌩-고벵 글래스 프랑스 유기 발광 장치 및 유기 발광 장치의 투명 전기 전도층의 용도
JP2013101309A (ja) * 2011-10-12 2013-05-23 Canon Inc エレクトロクロミック材料を用いた透過率可変素子、光学系および光学機器

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