CN103842307A - Glass plate fitted with transparent electroconductive film and glass plate for forming transparent electroconductive film - Google Patents

Glass plate fitted with transparent electroconductive film and glass plate for forming transparent electroconductive film Download PDF

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Publication number
CN103842307A
CN103842307A CN201280047009.7A CN201280047009A CN103842307A CN 103842307 A CN103842307 A CN 103842307A CN 201280047009 A CN201280047009 A CN 201280047009A CN 103842307 A CN103842307 A CN 103842307A
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Prior art keywords
sheet glass
nesa coating
glass
content
mass percent
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CN201280047009.7A
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Inventor
笹井淳
近藤裕己
林英明
广松邦明
中原阳
加藤利通
山本雄一
G·迪斯特法诺
土屋博之
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AGC Inc
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Asahi Glass Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
    • 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

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  • 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)
  • Glass Compositions (AREA)

Abstract

Provided are a glass plate fitted with a transparent conductive film and a glass plate for forming a transparent conductive film in which it is possible to inhibit separation of the transparent conductive film from an alkali barrier film. The glass plate fitted with the transparent conductive film is a glass plate (10) fitted with a transparent conductive film having an alkali barrier film (14) and a transparent conductive film (16) arranged from a glass plate (12) side in the stated order, wherein the glass plate (12) contains 60-75% of SiO2, 0-3% of Al2O3, 0-15% of CaO, 0-12% of MgO, 5-20% of Na2O, and 1.1-15% of K2O+SrO+BaO, and the total content expressed in terms of Fe2O3 being 0-0.06%.

Description

Sheet glass with nesa coating and nesa coating formation sheet glass
Technical field
The present invention relates to be formed with on surface the sheet glass with nesa coating and the nesa coating formation sheet glass of nesa coating.
Background technology
Be used as glass substrate for thin-film solar cells, low emissivity glass sheet (Low-E sheet glass) etc. with the sheet glass of nesa coating.For such sheet glass with nesa coating, conventionally require it to there is high light transmittance.
For example, for thin-film solar cells glass substrate, require its transmission of visible light (being denoted as below Tv) and solar radiation transmissivity (being denoted as below Te) enough high.Therefore, sheet glass as thin-film solar cells with the substrate of glass substrate, uses the content of coloring components (particularly iron) few and Tv and the high high transmission glass plate being made up of soda-lime-silica glass (so-called ultrawhite sheet glass) (with reference to patent documentation 1) of Te.
Prior art document
Patent documentation
Patent documentation 1: Japanese Patent Laid-Open 2007-112710 communique
Summary of the invention
Invent technical problem to be solved
, in the sheet glass with nesa coating, through time at the Na of the surperficial stripping of sheet glass +, in the time making Thinfilm solar cell component, there is Na +thermodiffusion, so the characteristic variation of the electric layer of Thinfilm solar cell component.Therefore, between sheet glass and nesa coating, be provided with SiO 2for the basic metal barrier film of principal constituent.
But, even basic metal barrier film is set known, if at long-term circulating current in the nesa coating of glass substrate for thin-film solar cells, contained Na in sheet glass +by electric attraction to nesa coating, Na +diffuse to the surface of basic metal barrier film, the phenomenon that nesa coating is peeled off occurs.
The invention provides a kind of sheet glass with nesa coating of peeling off and nesa coating formation sheet glass that has suppressed nesa coating.
The technical scheme that technical solution problem adopts
Sheet glass with nesa coating of the present invention is the sheet glass with nesa coating with sheet glass and nesa coating, wherein,
Described sheet glass, in the mass percent of oxide compound benchmark, comprises:
Figure BDA0000482584310000021
Described sheet glass is better in the mass percent of oxide compound benchmark, comprises:
Volume specific resistance (log (ρ [Ω cm])) when 150 ℃ of described sheet glass is better 8.8～12.0.Top temperature (the T that film in DHB test described later is not peeled off max) be better more than 150 ℃.
Sheet glass with nesa coating of the present invention is better to have the basic metal barrier film being arranged between described sheet glass and described nesa coating.
In addition, nesa coating formation of the present invention is better in the mass percent of following oxide-base standard with sheet glass, comprises:
Figure BDA0000482584310000031
In addition, nesa coating formation of the present invention is better in the mass percent of following oxide-base standard with sheet glass, comprises:
Figure BDA0000482584310000032
In addition, nesa coating formation of the present invention is better in the mass percent of following oxide-base standard with sheet glass, comprises:
Figure BDA0000482584310000041
In addition, the sheet glass with nesa coating of the present invention is the sheet glass with nesa coating with sheet glass and nesa coating, wherein,
Described sheet glass, in the mass percent of oxide compound benchmark, comprises:
For "～" of above-mentioned expression numerical range, to comprise that the numerical value being recorded in before and after it uses as the connotation of lower value and higher limit, as long as no specifically definition, following in specification sheets, also use "～" with same connotation.
The effect of invention
Sheet glass with nesa coating of the present invention is the sheet glass of peeling off that can suppress nesa coating
Accompanying drawing explanation
Fig. 1 is the sectional view that represents an example of the sheet glass with nesa coating of the present invention.
Fig. 2 is the sectional view that represents an example of thin-film solar cells.
Fig. 3 is the sectional view that represents an example of double glazing.
Embodiment
The sheet glass > of < with nesa coating
Sheet glass with nesa coating of the present invention has sheet glass and nesa coating, better also has the basic metal barrier film being arranged between sheet glass and nesa coating.Other film also can be set between sheet glass and basic metal barrier film, between basic metal barrier film and nesa coating and/or on the surface of the sheet glass of the opposition side of nesa coating side.
Fig. 1 is the sectional view that represents an example of the sheet glass with nesa coating of the present invention.Sheet glass 10 with nesa coating has sheet glass 12, the basic metal barrier film 14 forming on a surface of sheet glass 12 and the nesa coating 16 forming on the surface of basic metal barrier film 14.
(nesa coating formation sheet glass)
Sheet glass as the substrate of the sheet glass with nesa coating has following composition (I).Sheet glass is better to have following composition (II), is more preferably and has following composition (III), particularly preferably has following composition (IV).
Below, in this specification sheets, " nesa coating formation sheet glass " also notes by abridging as " sheet glass ".Be denoted as the sheet glass with nesa coating with the sheet glass of nesa coating.
(I) in the mass percent of following oxide-base standard, comprise:
Figure BDA0000482584310000051
(II) in the mass percent of following oxide-base standard, comprise:
Figure BDA0000482584310000052
Figure BDA0000482584310000061
(III) in the mass percent of following oxide-base standard, comprise:
Figure BDA0000482584310000062
(IV) in the mass percent of following oxide-base standard, comprise:
Figure BDA0000482584310000063
Sheet glass in the present invention adopts following composition: in the mass percent of oxide compound benchmark, K 2the total content of O, SrO and BaO is than contained K in common soda-lime-silica glass (comprising common high transmission glass plate) 2the total content (being for example, below 0.4% in the situation of high transmission glass plate) of O, SrO and BaO is more.
If K/Na is than increasing, due to the effect of mixed alkali metal, the volume specific resistance of sheet glass raise (, specific conductivity reduction).In addition, for the ratio of alkaline-earth metal/Na, also find the tendency same with K/Na, in the Sr that atomic radius is large, the situation of Ba, this tendency is remarkable especially.Therefore, if K 2content (or the K of O 2the total content of O, SrO and BaO) more than common soda-lime-silica glass (comprising common high transmission glass plate), the volume specific resistance of sheet glass rising (, specific conductivity reduces), even so in the nesa coating of the sheet glass with nesa coating long-term circulating current, contained Na in sheet glass +also be difficult for by electric attraction to nesa coating, Na +be not easy to diffuse to the surface of basic metal barrier film, therefore can suppress nesa coating peeling off from basic metal barrier film.
K 2the content of O counts 0～5% with the mass percent of oxide compound benchmark.If K 2the content of O exceedes 5%, causes raw materials cost significantly to rise, or viscosity under high temperature rises, solvability variation.K 2the content of O, in the mass percent of oxide compound benchmark, is preferably 1.1～4.5%, and more preferably 1.3～4.0%.
The content of SrO counts 0～5% with the mass percent of oxide compound benchmark.If the content of SrO exceedes 5%, devitrification characteristic (, being not easy to occur the characteristic of devitrification in the time of glass-pane shaping) variation.The content of SrO, in the mass percent of oxide compound benchmark, is preferably 0～4%, and more preferably 0～2%.
The content of BaO counts 0～5% with the mass percent of oxide compound benchmark.If the content of BaO exceedes 5%, devitrification characteristic variation.The content of BaO, in the mass percent of oxide compound benchmark, is preferably 0～4.5%, and more preferably 0～4%.
K 2the total content of O, SrO and BaO (is also denoted as " K by this total amount in this specification sheets below, 2o+SrO+BaO ") count 1.1～15% with the mass percent of oxide compound benchmark.If K 2o+SrO+BaO, lower than 1.1%, can not fully suppress nesa coating peeling off from basic metal barrier film.If K 2o+SrO+BaO exceedes 15%, and liquidus temperature rises, and the possibility of devitrification characteristic variation increases.K 2o+SrO+BaO, in the mass percent of oxide compound benchmark, is preferably 1.4～13%, and more preferably 1.4～12%.
Fe 2o 3it is the coloring components of inevitably sneaking on manufacturing.
Be scaled Fe 2o 3the content of the full iron of meter counts 0～0.06% with the mass percent of oxide compound benchmark.If be scaled Fe 2o 3the content of the full iron of meter is below 0.06%, and the reduction of Tv can be inhibited.Be scaled Fe 2o 3the content of the full iron of meter, in the mass percent of oxide compound benchmark, is preferably 0～0.05%, and more preferably 0～0.03%.Be particularly below 0.01% by making the content of this full iron, can easily make the Te (thickness of slab 4mm thickness conversion) of sheet glass reach more than 90%, and can easily make the Tv (thickness of slab 4mm thickness conversion) of sheet glass reach more than 90%, thereby preferably.
In this specification sheets, the content of full iron according to standard method of analysis with Fe 2o 3amount represent, be not all to exist as 3 valency iron but be present in iron in glass.Conventionally, in glass, there is divalent iron.Divalent iron mainly has absorption peak near wavelength 1000～1100nm, also has absorption at the wavelength place shorter than wavelength 800nm, and 3 valency iron mainly have absorption peak near wavelength 400nm.The increase of divalent iron means the increase of the absorption of the near infrared range before and after 1000nm, if it is described with Te, for Te reduces.Therefore,, in the situation that being conceived to Tv, Te, be scaled Fe by inhibition 2o 3the content of the full iron of meter, can suppress the decline of Tv, by making 3 valency iron more than divalent iron, can suppress the decline of Te.Therefore, suppress Tv, Te decline aspect, preferably reduce full iron amount, will be scaled Fe 2o 3in the full iron of meter, be scaled Fe 2o 3the mass ratio (being designated as below Redox) of the divalent iron of meter is suppressed at low-level.
The Redox of sheet glass is preferably below 35%.If Redox is below 35%, can suppress the decline of Te.Redox is more preferably below 30%.
SiO 2it is the principal constituent of glass.
SiO 2content count 60～75% with the mass percent of oxide compound benchmark.If SiO 2content lower than 60%, the stability decreases of glass.If SiO 2content exceed 75%, the temperature of fusion of glass raise, likely cannot melt.SiO 2content in the mass percent of oxide compound benchmark, be preferably 62～73%, more preferably 62～72%.In addition SiO, 2content can be also 68～75%, preferably 69～75%, more preferably 69.3～73%.
Al 2o 3it is the composition that weathering resistance is improved.
Al 2o 3content count 0～3% with the mass percent of oxide compound benchmark.If Al 2o 3content exceed 3%, the remarkable variation of melting, or volume resistance becomes too low.Al 2o 3content in the mass percent of oxide compound benchmark, be preferably 0～2.8%, more preferably 0～2.5%.In addition Al, 2o 3content can be also 0.3～2.3%, preferably 0.5～2.1%.
CaO is the composition that promotes the melting of frit and adjust viscosity, thermal expansivity etc.
The content of CaO counts 0～15% with the mass percent of oxide compound benchmark.If the content of CaO exceedes 15%, devitrification temperature rises.The content of CaO, in the mass percent of oxide compound benchmark, is preferably 3～12%, and more preferably 3～11%.In addition, the content of CaO can be also 5～10%.
MgO is the composition that promotes the melting of frit and adjust viscosity, thermal expansivity etc.
The content of MgO counts 0～12% with the mass percent of oxide compound benchmark.If the content of MgO exceedes 12%, devitrification temperature rises.The content of MgO, in the mass percent of oxide compound benchmark, is preferably 2～12%, and more preferably 2～6%.In addition, the content of MgO can be also 1～10%, preferably 3～8%.
Na 2o is the essential composition that promotes frit melting.
Na 2the content of O counts 5～20% with the mass percent of oxide compound benchmark.If Na 2the content of O is lower than 5%, and the fusing of frit becomes difficulty.If Na 2the content of O exceedes 20%, the weathering resistance of sheet glass and bad stability.Na 2the content of O, in the mass percent of oxide compound benchmark, is preferably 7～19%, and more preferably 9～17%.Na 2the content of O can be also 9～15%.
In sheet glass of the present invention, although optional, can also comprise TiO 2, ZrO 2, Li 2o and B 2o 3.
Contain TiO 2situation under, TiO 2content in the mass percent of oxide compound benchmark, be preferably 0～2%.If TiO 2content exceed 2%, sheet glass is painted, Tv and Te decline.
ZrO 2it is the composition that can improve the chemical durability of glass and improve the physical strengths such as Young's modulus, hardness.
Contain ZrO 2situation under, ZrO 2content in the mass percent of oxide compound benchmark, be preferably 0～3%.If ZrO 2content exceed 3%, melting characteristic variation, devitrification temperature rise.
Li 2o is the melting that can promote frit, the composition that reduces temperature of fusion.
Contain Li 2in the situation of O, Li 2the content of O, in the mass percent of oxide compound benchmark, is preferably 0～3%.If Li 2the content of O exceedes 3%, the bad stability of glass.In addition, cause raw materials cost significantly to increase.
B 2o 3the composition that promotes frit melting, if but add in soda-lime-silica glass, the unfavorable condition such as generation, erosion furnace wall of the brush line (ream) that mostly can occur to be caused by volatilization, inapplicable on manufacturing.
Contain B 2o 3situation under, B 2o 3content in the mass percent of oxide compound benchmark, be preferably below 1%, more preferably in fact containing B 2o 3.Here do not contain in fact the amount that can sneak into impurity levels that refers to.
Sheet glass preferably comprises the SO using as finings 3.Be scaled SO 3the content of the full sulphur of meter, in the mass percent of oxide compound benchmark, is preferably 0.01～0.5%.If be scaled SO 3the content of the full sulphur of meter exceedes 0.5%, occurs to boil in the process being cooled at melten glass again, and bubble quality may variation.If be scaled SO 3the content of the full sulphur of meter, lower than 0.01%, cannot obtain sufficient clarifying effect.Be scaled SO 3the content of the full sulphur of meter, in the mass percent of oxide compound benchmark, is preferably 0.05～0.5%, and more preferably 0.2～0.4%.
Sheet glass also can contain the SnO using as finings 2.Be scaled SnO 2the content of the full tin of meter, in the mass percent of oxide compound benchmark, is preferably 0～1%.In addition, can will be laminated with SnO on the top layer of glass substrate as transparent electrode material 2the fragment of the glass with nesa coating of film is as SnO 2the frit of composition.
Sheet glass also can contain the Sb using as finings 2o 3.Be scaled Sb 2o 3the content of the full antimony of meter is preferably 0～0.5%.If be scaled Sb 2o 3the content of full antimony of meter exceedes 0.5%, the in the situation that of float glass process, and the sheet glass generation gonorrhoea after shaping.Be scaled Sb 2o 3the content of the full antimony of meter, in the mass percent of oxide compound benchmark, is preferably 0～0.1%.
Sheet glass is better in fact not containing S, NiO, MoO as coloring components 3, CoO, Cr 2o 3, V 2o 5, or MnO.In fact not containing S, NiO, MoO 3, CoO, Cr 2o 3, V 2o 5or MnO refers to: completely not containing S, NiO, MoO 3, CoO, Cr 2o 3, V 2o 5or MnO; Or can be used as the impurity of inevitably sneaking in manufacture and contain S, NiO, MoO 3, CoO, Cr 2o 3, V 2o 5, MnO.If in fact not containing S, NiO, MoO 3, CoO, Cr 2o 3, V 2o 5or MnO, can suppress the decline of Tv, Te.
The Te of sheet glass (4mm thickness conversion, convert by the thickness of slab of sheet glass as 4mm) is preferably more than 80%, more preferably more than 82.7%.The solar radiation transmissivity of Te for utilizing spectrophotometric determination transmissivity to calculate according to JIS R3106 (1998) (being designated hereinafter simply as JIS R3106).
In addition the Fe as coloring components in composition, 2o 3content is in the situation below 0.01%, and Te (4mm thickness conversion) is preferably more than 90%, more preferably more than 91%, further preferably more than 91.5%.
The Tv (4mm thickness conversion) of sheet glass is preferably more than 80%, more preferably more than 82%.Tv is the transmission of visible light that utilizes spectrophotometric determination transmissivity to calculate according to JIS R3106.The value at coefficients by using standard light A, 2 degree visual angles.
In addition the Fe as coloring components in composition, 2o 3content is in the situation below 0.01%, and Tv (4mm thickness conversion) is preferably more than 90%, more preferably more than 91%.
Volume specific resistance (log (ρ [Ω cm])) when 150 ℃ of sheet glass is preferably 9.0～12, and more preferably 9.1～12.If volume specific resistance when 150 ℃ of sheet glass is more than 9.0, can suppress more reliably nesa coating peeling off from basic metal barrier film.Similarly, the volume specific resistance (log (ρ [Ω cm])) when 200 ℃ of sheet glass is preferably 7.8～12, and more preferably 7.9～11.If volume specific resistance when 200 ℃ of sheet glass is more than 7.8, can suppress more reliably nesa coating peeling off from basic metal barrier film.
Here, the volume specific resistance of sheet glass can be measured by the method based on ASTM C657-78.
Sheet glass can be successively through for example following operation (i)～(V) manufacture.
(i) mix various glass chief component raw materials, fragment, finings etc. according to target composition, thereby prepare frit.
(ii) make frit melting to make melten glass.
(iii) by after melten glass clarification, utilize float glass process or glass tube down-drawing (scorification) to be configured as the sheet glass of specific thickness.
(iv) cooled glass plate.
(V) sheet glass is cut into the size of regulation.
In addition, in above-mentioned operation (iii) afterwards, also can be attached to the operation (iii-1) that glass pane surface forms basic metal barrier film, or stop that at the basic metal of this sheet glass face forms the operation (iii-2) of nesa coating.By additional these operations (iii-1) and (iii-2), can utilize sheet glass manufacturing process to manufacture online the sheet glass with nesa coating.
As glass chief component raw material, can exemplify the material that the common raw material as soda-lime glass such as silica sand, rhombspar, SODA ASH LIGHT 99.2 uses.
As finings, can exemplify SO 3, SnO 2or Sb 2o 3deng.
The melting of frit can, by for example frit being supplied to continuously to glass melting furnace (melting kiln), be heated to approximately 1300～1600 ℃ with heavy oil, Sweet natural gas, electricity etc. and carry out.
Sheet glass with nesa coating can form nesa coating by the glass-board surface as above making, or forms basic metal barrier film at the glass-board surface as above making, then stops that at this basic metal face forms nesa coating and manufactures.In addition, also can be by the manufacturing process (i) of above-mentioned sheet glass～(V), the formation operation (iii-1) of additional above-mentioned basic metal barrier film, stops that at the basic metal of the prepared glass-board surface with basic metal barrier film face forms nesa coating and manufactures.In addition, also can be by the formation engineering (iii-1) at described basic metal barrier film afterwards, be attached to basic metal and stop that face forms the operation (iii-2) of nesa coating, manufactures the sheet glass with nesa coating.
(nesa coating)
As nesa coating, can exemplify with SnO 2for the film of principal constituent, film take ZnO as principal constituent, film take the Indium sesquioxide (ITO) of doped tin as principal constituent etc., while sneaking into electric layer from the composition of raw materials cost, production, nesa coating, the viewpoint of the few material of the impact of electric layer is considered, preferably with SnO 2for the film of principal constituent.Here, " principal constituent " refers to the mass percent of this composition in oxide compound benchmark, contains more than 90%.
As with SnO 2for the film of principal constituent, can exemplify by SnO 2the film forming, film, the film being formed by the stannic oxide of antimony dopant etc. being formed by the stannic oxide (FTO) of doped with fluorine.
As the formation method of nesa coating, can exemplify thermal decomposition method, CVD method, sputtering method, vapour deposition method, ion plating or spray method etc.
Preferably 200～1200nm of the thickness of nesa coating.
(basic metal barrier film)
As basic metal barrier film, can exemplify with SiO 2for the film of principal constituent, with SiO 2and SnO 2mixed oxide be principal constituent film and SiO 2and SnO 2multilayer film, with Al 2o 3, ZrO 2or the SiOC film that is principal constituent etc.Here, " principal constituent " refers to the mass percent of this composition in oxide compound benchmark, contains more than 90%.
As the formation method of basic metal barrier film, can exemplify thermal decomposition method, CVD method, sputtering method, vapour deposition method, ion plating or spray method etc.
From the aspect of alkali barrier properties, more than the thickness of basic metal barrier film is preferably 10nm, from cost aspect, preferably below 500nm.
(other films)
As other films that can be arranged between sheet glass and basic metal barrier film, can exemplify TiO 2film, SnO 2film etc.
As other films that can be arranged between basic metal barrier film and nesa coating, can exemplify SiO 2and SnO 2mixed oxide and multilayer film etc.
As other surperficial films of sheet glass of opposition side that can be arranged on nesa coating side, can exemplify antireflection film etc.
In addition, other films self can have basic metal barrier properties.
In the situation of the sheet glass with nesa coating of the present invention described above, K 2the content of O is counted more than 0.8% with the mass percent of oxide compound benchmark, and K 2the total content of O, SrO and BaO is counted more than 1.1% with the mass percent of oxide compound benchmark, so the volume specific resistance of sheet glass high (, specific conductivity reduces).Consequently, though long-term circulating current in the nesa coating of the sheet glass with nesa coating, contained Na in sheet glass +also be not easy by electric attraction to nesa coating Na +be not easy to diffuse to the surface of basic metal barrier film.So peeling off of nesa coating is inhibited.
In addition, be scaled Fe 2o 3the content of the full iron of meter counts 0～0.06% with the mass percent of oxide compound benchmark, so Tv is enough high.
< thin-film solar cells >
Sheet glass with nesa coating of the present invention is suitable as thin-film solar cells glass substrate.
Fig. 2 is the sectional view that represents an example of thin-film solar cells.Thin-film solar cells 20 is on a surface of sheet glass 12, across basic metal barrier film 14 be formed with Thinfilm solar cell component 22 and thin-film solar cells.Antireflection film (diagram slightly) etc. also can be set on another surface of sheet glass 12 (, the face of the opposition side of the forming surface of Thinfilm solar cell component 22).
Sheet glass with nesa coating of the present invention arranges the thin-film solar cells of nesa coating on sheet glass applicable to whole thin film silicon class solar cell, CdTe based thin film solar cells etc.
Thinfilm solar cell component 22 has transparent electrode layer 24, photoelectric conversion layer 26 (, electric layer), backplate layer 28 successively from sheet glass 12 sides.
Transparent electrode layer 24 is the layers that formed by above-mentioned nesa coating 16.
Photoelectric conversion layer 26 is the layers that formed by thin film semiconductor.As thin film semiconductor, can exemplify non-crystalline silicon based semiconductor, microcrystal silicon based semiconductor, compound semiconductor (such as chalcopyrite based semiconductor, CdTe based semiconductor etc.), organic semi-conductor etc.
As the material of backplate layer 28, can exemplify material (for example silver, aluminium etc.) without light transmission, have material (for example ITO, the SnO of light transmission 2, ZnO etc.).
< double glazing >
Sheet glass with nesa coating of the present invention has Low-E (Low Emissivity: low radiation) performance, therefore also can be used as Low-E sheet glass.
Fig. 3 is the sectional view that represents an example of the double glazing that uses Low-E sheet glass.The spacer 34 of the frame shape that double glazing 30 has two sheet glass 12, configure between the circumference of sheet glass 12 with the condition that forms spaces 32 12 of sheet glass and be arranged at spacer and sheet glass 12 between containment member (diagram slightly), as a side of sheet glass 12, use in the space of double glazing 32 sides, from sheet glass 12 sides set gradually basic metal barrier film 14, nesa coating 16 and the sheet glass with nesa coating.Low-reflection film (diagram slightly) etc. also can be set on the surface of the sheet glass 12 of 32Ce opposition side, space.
Embodiment
Exemplify embodiment below the present invention is specifically described, but the present invention is not limited to these examples.
[example 1～31]
Example 2～31st, embodiment, example 1 is comparative example.
Nesa coating formation is measured and is calculated by following method by each performance of sheet glass and the sheet glass with nesa coating.
(Redox)
The Fe of the sheet glass of gained 2o 3fe is measured and calculate, is scaled to amount by fluorescent X-ray 2o 3the content (%=mass percent) of the full iron of meter.
The amount that calculates the divalent iron in required sheet glass of Redox is from being converted and calculated by the transmissivity of utilizing transmissivity to measure the wavelength 1000nm obtaining.Here, after 8% deducts, convert the impact causing because of the reflection at wavelength 1000nm place to uptake factor, to utilize the calibration curve that wet analysis method is made in advance as basis, the amount of divalent iron to be carried out quantitatively.
(Tv)
The sheet glass of gained is ground to 4mm thickness, measures the transmission of visible light (Tv) (adopting A light source) of JIS R3106 regulation.
(Te)
The sheet glass of gained is ground to 4mm thickness, measures the solar radiation transmissivity (Te) of JIS R3106 regulation.
(volume specific resistance)
The volume specific resistance of sheet glass can be measured by the method based on ASTM C657-78.As sheet glass, use there is the size of about 50mm × 50mm, to carrying out optical grinding and the thickness made is about the sheet glass of 4mm in two sides.Form Al metal membrane using as electrode on the two sides of this sheet glass by vapour deposition method, the volume specific resistance while measuring 100 ℃, 150 ℃, 200 ℃.In addition, the volume resistance value of arbitrfary point, by using the slope A and section square B that calculate from the relation of the inverse (1/T) of volume specific resistance (log (ρ [Ω cm])) at each temperature and absolute temperature, calculates according to following prediction type.
log(ρ[Ω·cm])=A/T+B
(DHB test)
Be partial to the endurance test (being denoted as below DHB test) of (Dump Heat Bias (DHB)) class by moisture-proof, can estimate the easness of peeling off of nesa coating.
DHB test is to evaluate the test that the electricity of the test film to being coated with film is attacked and heat is attacked simultaneously.As shown in following (1)～(4), heat time enough until be stabilized in design temperature by the sheet glass to nesa coating (sample), carry out applying electric field with the sheet glass of nesa coating simultaneously.
(1) sample is configured between two electrodes.Make not form a side contacts Graphite Electrodes (anode) of nesa coating, the copper electrode (negative electrode) that nesa coating side contacts is covered by aluminium.Be heated to after design temperature, with voltage 500V sustaining voltage application time 15 minutes.
(2) be cooled to after room temperature, the nesa coating side of sample be exposed in the atmosphere of relative humidity 100% to 1 hour, make nesa coating side generation aggegation.Aggegation humidity, water temperature are made as 55 ℃, and gasification temperature is made as 50 ℃ ± 2 ℃.
(3) whether confirmation there is peeling off of nesa coating on the surface of the nesa coating side of sample.Peel off about having or not, as long as the released part that has a place with the naked eye to confirm in sample is defined as and has occurred to peel off.
(4) prepare multiple other samples that make under identical conditions, carry out one by one three tests for each design temperature.The temperature that the nesa coating of sample is peeled off is denoted as T max(℃).T maxhigher, be judged as nesa coating and be not easy for a long time to peel off (, weather resistance is high).
Basic metal barrier film (SiO 2) and nesa coating (SnO 2) the mechanism of peeling off generation of interface be, contained Na in sheet glass +, to described interface movement, there is following reaction as the voltage of negative pole at this interface as anodal, nesa coating side owing to being applied to sheet glass side, peel off this closely sealed interface by Sn-O key.
1.Na ++e -→Na
2.H 2O+Na→NaOH+1/2H 2
3.2H 2+SnO 2→Sn+2H 2O
The making of the sheet glass of example 1～31 is carried out in such a way.
According to the composition shown in table 1-1～1-5, mix silica sand, other various glass chief component raw materials and finings (SO 3), prepare frit.Frit is put into crucible, in electric furnace, in 1500 ℃ of heating 3 hours, make melten glass.Melten glass is poured on carbon plate, carries out cooling.Grind two sides, obtain the sheet glass that thickness is 4mm.For sheet glass, use spectrophotometer (Hitachi Ltd. (vertical System Zuo Suo of day society) system, U-4100) to measure the transmissivity of every 1nm, calculate Tv, Te, volume specific resistance.The results are shown in table 1-1～1-5.
On the surface of sheet glass that is heated to 580 ℃, form the TiO of thickness 8nm by CVD method 2film, thickness 25nm by SiO 2form basic metal barrier film and thickness 550nm by SnO 2the nesa coating forming.For the sheet glass with nesa coating, carry out DHB test.T maxbe shown in Table 1.Here the anticipation T when temperature that is 8.8 o'clock by the volume specific resistance at 150 ℃ (log (ρ [Ω cm])), is defined as thickness of glass and is 4mm max, represent the temperature of estimating with above-mentioned prediction type.
In addition, in table 1-1～1-5, A[K] and slope A and section square B (zero dimension) of B while representing volume calculated resistance value.
[table 1-1]
Composition (quality %) Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
SiO 2 71.3 71.4 71.4 71.4 71.2 70.29
Al 2O 3 1.5 1.86 1.86 1.8 1.6 1.5
CaO 8.5 7.81 7.81 7.81 7.4 11
MgO 4.2 4.69 4.69 4.69 5 6
Na 2O 13.1 12.29 11.79 11.29 9.5 9
K 2O 1 1.51 2.01 2.51 4 0
SrO ? ? ? ? ? 2
BaO ? ? ? ? ? 0
K 2O+SrO+BaO 1 1.51 2.01 2.51 4 2
Fe 2O 3 0.036 0.022 0.022 0.022 0.011 0.010
SO 3 0.23 0.4 0.4 0.4 0.29 0.2
TiO 2 0.04 0.021 0.021 0.021 1 0
CeO 2 0.1 ? ? ? ? ?
Amount to 100.0 100.0 100.0 99.9 100.0 100.0
Redox[%] ? 14.5 13.7 13.5 ? ?
Tv[%] ? 91.7 91.7 916 ? ?
Te[%] ? 90.6 90.6 90.6 ? ?
Log (ρ [Ω cm]) is in 100 ℃ 10.424 10.56 10.79 11.01 11.54 11.38
Log (ρ [Ω cm]) is in 150 ℃ 8.914 9.12 9.35 9.5 9.97 9.90
Log (ρ [Ω cm]) is in 200 ℃ 7.725 7.95 8.12 8.3 8.70 8.66
A[x1000K] 4.72 4.56 4.65 4.68 4.96 4.74
B -2.29 -1.72 -17.3 -1.63 -1.81 -1.38
T max[℃] 152 160 169 175 190 192
[table 1-2]
Composition (quality %) Example 7 Example 8 Example 9 Example 10 Example 11 Example 12
SiO 2 70.29 71.29 65.29 63.29 62.29 65.29
Al 2O 3 2.5 0.5 0.5 2.5 2.5 0.5
CaO 11 3 11 11 3 11
MgO 2 2 2 6 6 6
Na 2O 9 11 17 9 17 9
K 2O 4 4 4 0 4 4
SrO 0 4 0 4 4 4
BaO 1 4 0 4 1 0
K 2O+SrO+BaO 5 12 4 8 9 8
Fe 2O 3 0.010 0.010 0.010 0.010 0.010 0.010
SO 3 0.2 0.2 0.2 0.2 0.2 0.2
TiO 2 0 0 0 0 0 0
CeO 2 ? ? ? ? ? ?
Amount to 100.0 100.0 100.0 100.0 100.0 100.0
Redox[%] ? ? ? ? ? ?
Tv[%] ? ? ? ? ? ?
Te[%] ? ? ? ? ? ?
Log (ρ [Ω cm]) is in 100 ℃ 12.23 11.80 10.87 12.41 10.66 13.37
Log (ρ [Ω cm]) is in 150 ℃ 10.60 10.17 9.35 10.80 9.15 11.65
Log (ρ [Ω cm]) is in 200 ℃ 9.28 8.86 8.06 9.49 7.94 10.24
A[x1000K] 5.16 5.13 4.91 5.09 4.75 5.47
B -1.66 -2.03 -2.34 -1.31 -2.14 -1.37
T max[℃] 220 201 168 231 161 265
[table 1-3]
Composition (quality %) Example 13 Example 14 Example 15 Example 16 Example 17 Example 18
SiO 2 70.95 70.84 70.71 70.28 70.28 70.28
Al 2O 3 1.9 1.9 1.9 1.88 1.88 1.88
CaO 9.77 8.91 9.74 8.4 8.2 8.3
MgO 3.42 4.24 3.41 4.54 4.83 4.73
Na 2O 12.31 11.98 11.64 11.26 10.9 10.9
K 2O 1.44 1.92 2.39 2.53 2.8 2.8
SrO 0 0 0 0 0 0
BaO 0 0 0 0.9 0.9 0.9
K 2O+SrO+BaO 1.44 1.92 2.39 3.43 3.7 3.7
Fe 2O 3 0.010 0.010 0.010 0.010 0.010 0.010
SO 3 0.2 0.2 0.2 0.2 0.2 0.2
TiO 2 0 0 0 0 0 0
CeO 2 ? ? ? ? ? ?
Amount to 100.0 100.0 100.0 100.0 100.0 100.0
Redox[%] ? ? ? ? ? ?
Tv[%] ? ? ? ? ? ?
Te[%] ? ? ? ? ? ?
Log (ρ [Ω cm]) is in 100 ℃ 10.82 10.95 11.19 11.26 11.38 11.39
Log (ρ [Ω cm]) is in 150 ℃ 9.34 9.45 9.67 9.72 9.82 9.86
Log (ρ [Ω cm]) is in 200 ℃ 8.17 8.27 8.47 8.49 8.57 8.62
A[x1000K] 4.58 4.62 4.77 4.83 4.86 4.82
B -1.55 -1.52 -1.65 -1.76 -1.76 -1.61
T max[℃] 170 175 183 184 188 190
[table 1-4]
Composition (quality %) Example 19 Example 20 Example 21 Example 22 Example 23 Example 24
SiO 2 70.28 70.28 70.87 70.99 71.1 71.1
Al 2O 3 1.88 1.88 1.9 1.9 1.91 1.91
CaO 8.3 8.3 8.11 8.3 7.37 7.54
MgO 4.73 4.73 4.79 4.8 4.97 4.8
Na 2O 11.5 11.7 12.3 12.3 12.34 12.34
K 2O 2.2 2 1.5 1.5 1.5 1.5
SrO 0 0 0 0 0 0
BaO 0.9 0.9 0.3 0 0.6 0.6
K 2O+SrO+BaO 3.1 2.9 1.8 1.5 2.1 2.1
Fe 2O 3 0.010 0.010 0.008 0.010 0.010 0.010
SO 3 0.2 0.2 0.2 0.2 0.2 0.2
TiO 2 0 0 0.021 0 0 0
CeO 2 ? ? ? ? ? ?
Amount to 100.0 100.0 100.0 100.0 100.0 100.0
Redox[%] ? ? ? ? ? ?
Tv[%] ? ? 91.2 ? ? ?
Te[%] ? ? 90.3 ? ? ?
Log (ρ [Ω cm]) is in 100 ℃ 11.13 11.04 10.69 10.68 10.65 10.66
Log (ρ [Ω cm]) is in 150 ℃ 9.61 9.54 9.21 9.22 9.14 9.15
Log (ρ [Ω cm]) is in 200 ℃ 8.39 8.35 8.04 8.08 7.95 7.96
A[x1000K] 4.73 4.67 4.54 4.49 4.72 4.72
B -1.66 -1.57 -1.57 -1.45 -2.06 -2.06
T max[℃] 179 177 164 165 161 161
[table 1-5]
Composition (quality %) Example 25 Example 26 Example 27 Example 28 Example 29 Example 30 Example 31
SiO 2 70.65 70.89 70.99 70.89 71.09 70.89 71.19
Al 2O 3 1.9 1.7 1.6 1.7 1.6 1.4 1.6
CaO 8 8.11 8.21 8.21 8.21 8.3 8.11
MgO 4.8 4.79 4.79 4.79 4.79 5 4.79
Na 2O 12.34 12.2 12.1 12.1 12 12.2 12.3
K 2O 1.5 1.5 1.5 1.5 1.5 1.4 1.5
SrO 0 0 0 0 0 0 0
BaO 0.6 0.6 0.6 0.6 0.6 0.6 0.3
K 2O+SrO+BaO 2.1 2.1 2.1 2.1 2.1 2 1.8
Fe 2O 3 0.010 0.010 0.010 0.010 0.010 0.010 0.010
SO 3 0.2 0.2 0.2 0.2 0.2 0.2 0.2
TiO 2 0 0 0 0 0 0 0
CeO 2 ? ? ? ? ? ? ?
Amount to 100.0 100.0 100.0 100.0 100.0 100.0 100.0
Redox[%] ? ? ? ? ? ? ?
Tv[%] ? ? ? ? ? ? ?
Te[%] ? ? ? ? ? ? ?
Log (ρ [Ω cm]) is in 100 ℃ 10.73 10.77 10.81 10.80 10.82 10.81 10.72
Log (ρ [Ω cm]) is in 150 ℃ 9.22 9.26 9.30 9.29 9.31 9.30 9.21
Log (ρ [Ω cm]) is in 200 ℃ 8.03 8.07 8.11 8.10 8.12 8.12 8.02
A[x1000K] 4.72 4.72 4.72 4.72 4.72 4.72 4.72
B -1.99 -1.94 -1.91 -1.91 -1.89 -1.90 -1.99
T max[℃] 164 166 168 167 168 168 164
K 2in the situation of the example 1 (being equivalent to the embodiment 5 of patent documentation 1) that the total content of O+SrO+BaO is few, test the temperature T of peeling off that nesa coating occurs by DHB maxlow.On the other hand, K 2the total content of O, SrO and BaO is counted with the mass percent of oxide compound benchmark in the situation of more than 1.1% example 2～31, tests the temperature T of peeling off that nesa coating occurs by DHB maxup to more than 160 ℃, knownly can continue for a long time to suppress nesa coating peeling off from basic metal barrier film.
The possibility of utilizing in industry
Sheet glass with nesa coating of the present invention is useful as glass substrate, low radiation sheet glass (Low-E sheet glass) etc. for thin-film solar cells.
Here quote the full content of specification sheets, claims, accompanying drawing and summary of No. 2011-212265, the Japanese patent application of filing an application on September 28th, 2011 as the announcement of specification sheets of the present invention.
The explanation of symbol
10 sheet glass with nesa coating
12 sheet glass (nesa coating formation sheet glass)
14 basic metal barrier films
16 nesa coatings
20 thin-film solar cells
22 Thinfilm solar cell components
24 transparent electrode layers
26 photoelectric conversion layers
28 backplate layers
30 double glazings
32 spaces
34 spacers

Claims (9)

1. the sheet glass with nesa coating, it is the sheet glass with nesa coating with sheet glass and nesa coating, it is characterized in that,
Described sheet glass represents with the mass percent of following oxide-base standard, comprises:
Figure FDA0000482584300000011
2. the sheet glass with nesa coating as claimed in claim 1, is characterized in that,
Described sheet glass represents with the mass percent of following oxide-base standard, comprises:
Figure FDA0000482584300000012
3. the sheet glass with nesa coating as claimed in claim 1 or 2, is characterized in that, the volume specific resistance (log (ρ [Ω cm])) when 150 ℃ of described sheet glass is 8.8～12.0.
4. the sheet glass with nesa coating as described in any one in claim 1～3, is characterized in that, the top temperature (T that the film in DHB test is not peeled off max) be more than 150 ℃.
5. the sheet glass with nesa coating as described in any one in claim 1～4, is characterized in that, has the basic metal barrier film being arranged between described sheet glass and described nesa coating.
6. a nesa coating formation sheet glass, is characterized in that, represents with the mass percent of following oxide-base standard, comprises:
Figure FDA0000482584300000021
7. nesa coating formation sheet glass as claimed in claim 6, is characterized in that, represents with the mass percent of following oxide-base standard, comprises:
Figure FDA0000482584300000022
8. nesa coating formation sheet glass as claimed in claim 6, is characterized in that, represents with the mass percent of following oxide-base standard, comprises:
Figure FDA0000482584300000023
Figure FDA0000482584300000031
9. the sheet glass with nesa coating, it is the sheet glass with nesa coating with sheet glass and nesa coating, it is characterized in that,
Described sheet glass represents with the mass percent of following oxide-base standard, comprises:
Figure FDA0000482584300000032
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TWI743029B (en) * 2014-12-09 2021-10-21 比利時商Ａｇｃ歐洲玻璃公司 Chemically temperable glass sheet and uses thereof
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TWI743029B (en) * 2014-12-09 2021-10-21 比利時商Ａｇｃ歐洲玻璃公司 Chemically temperable glass sheet and uses thereof
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