WO2019022484A2 - Verre à faible émissivité - Google Patents

Verre à faible émissivité Download PDF

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Publication number
WO2019022484A2
WO2019022484A2 PCT/KR2018/008378 KR2018008378W WO2019022484A2 WO 2019022484 A2 WO2019022484 A2 WO 2019022484A2 KR 2018008378 W KR2018008378 W KR 2018008378W WO 2019022484 A2 WO2019022484 A2 WO 2019022484A2
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WO
WIPO (PCT)
Prior art keywords
dielectric layer
layer
metal layer
thickness
glass
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Ceased
Application number
PCT/KR2018/008378
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English (en)
Korean (ko)
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WO2019022484A3 (fr
Inventor
박준영
강현민
김진용
오영훈
윤성군
유보나
이현주
이제향
김민주
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KCC Corp
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KCC Corp
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Publication of WO2019022484A2 publication Critical patent/WO2019022484A2/fr
Publication of WO2019022484A3 publication Critical patent/WO2019022484A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • 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
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal

Definitions

  • the present invention relates to a low emissivity glass having improved crystallinity of a functional reflective metal layer.
  • Low-Emissivity (Low-E) Glass (commonly referred to as "Roy Glass”) is widely used in architectural and automotive applications. In order to protect privacy and prevent energy loss, insulation performance and shielding performance are basically required do. Low sputtered glass deposited by sputtering has better thermal insulation and shielding performance than low sputtered glass produced by hard coating method.
  • the low emissivity glass needs to undergo a bending or tempering type of bending or pre-stressing treatment (often heat treatment).
  • the window panes are usually heated to a temperature of about 600-700 ° C prior to substantial treatment to bend or apply pre-stresses, which is required to maintain good thermal and shielding performance even after such heat treatment.
  • An object of the present invention is to provide a low-emission glass having a high shielding property and a low crystallinity of a metal layer with little difference in physical properties before and after a heat treatment.
  • a liquid crystal display comprising a glass substrate, a first dielectric layer formed on the glass substrate, a metal layer formed on the first dielectric layer, a second dielectric layer formed on the metal layer, wherein the first dielectric layer comprises AlN x (where 0.5 ⁇ x ⁇ 2) Thereby providing low emissivity glass.
  • the present invention it is possible to manufacture a low-emission glass having a high degree of crystallinity and a high degree of shielding with little difference in physical properties before and after the heat treatment.
  • 1 (a) to 1 (c) are views showing a laminated structure of the single low emissivity glass of the present invention.
  • Figs. 2 (a) to 2 (c) are views showing specific examples of the laminated structure of the single low-emission glass of Fig. 1.
  • Fig. 2 (a) to 2 (c) are views showing specific examples of the laminated structure of the single low-emission glass of Fig. 1.
  • FIG 3 is a view showing a laminated structure of the multi-low emission glass of the present invention.
  • 4 (a) to 4 (d) are views showing specific examples of the laminated structure of the multiple low emission glass of FIG. 3.
  • 1 (a) to 1 (c) are views showing a laminated structure of the single low emissivity glass of the present invention.
  • the low emission glass of the present invention includes a glass substrate 10, a first dielectric layer 20 formed on the glass substrate, a metal layer 30 formed on the first dielectric layer 20, 30) a second dielectric layer 21 formed on, and comprises a top layer 50 formed on the second dielectric layer 21, the first dielectric layer 20, AlN x (here, 0.5 ⁇ x ⁇ 2) .
  • the glass substrate 10 serves as a base substrate of the low-emission glass.
  • a glass substrate 10 for example, ordinary glass such as soda lime glass, low iron glass, green disc glass or blue disc glass which is used for construction or automobile can be used.
  • glass having a thickness of 2 mm to 12 mm can be freely used.
  • transparent soda lime glass having a thickness of 5 mm or 6 mm can be used.
  • the first dielectric layer 20 is formed on the glass substrate 10 and blocks oxygen or ions transferred to the metal layer 30 during heat treatment such as strengthening or bending. ), And may include AlN x (where 0.5 ⁇ x ⁇ 2), which is formed between the glass substrate 10 and the metal layer 30 as shown in FIGS.
  • the first dielectric layer 20 includes a main dielectric layer 20a, and at least one sub-dielectric layer 20b may be formed on an upper portion or a lower portion of the main dielectric layer 20a.
  • the main dielectric layer 20a may be an Si-based oxide, a nitride or a nitric oxide containing at least one element selected from AlN x (where 0.5 ⁇ x ⁇ 2) or Al, B, Ti, Nb, Sn and Mo . According to an embodiment of the present invention, the main dielectric layer 20a may use AlN x (where 0.5 ⁇ x ⁇ 2) or SiAlN x (where 1.3 ⁇ x ⁇ 1.5) If it is removed, the deposition rate may be lowered due to excess nitrogen (N 2 ).
  • the sub-dielectric layer (20b) is AlN x (here, 0.5 ⁇ x ⁇ 2) may include, where x is 0.5 ⁇ x ⁇ 2, and, x is is out of the value range of nitrogen (N 2) due to excess A decrease in the deposition rate may occur.
  • peaks of the sub-dielectric layer (AlN x layer) 20b and the metal layer 30 are shown according to one embodiment of the present invention, (30) has crystallinity.
  • This crystallinity induces the crystallization of the metal layer 30 to be well performed when the metal layer 30 is deposited on the sub-dielectric layer 20b, thereby reducing the sheet resistance of the coating film to improve the heat insulating performance, and the formed metal layer 30 can be stabilized Thereby preventing the occurrence of optical defects such as aggregation of the metal layer 30 during heat treatment or diffusion to the dielectric layers provided at the upper and lower portions of the metal layer 30.
  • the first dielectric layer 20 containing AlN x (where 0.5 ⁇ x ⁇ 2) before depositing the metal layer 30 when depositing the low emission glass of the present invention.
  • At least one of the main dielectric layer 20a and the sub-dielectric layer 20b may include AlN x (where 0.5 ⁇ x ⁇ 2).
  • the thickness of the main dielectric layer 20a may be 30 to 50 nm. If the thickness of the main dielectric layer 20a is less than 30 nm, durability may be deteriorated. If the thickness is more than 50 nm, the transmittance may be decreased.
  • the thickness of the sub-dielectric layer 20b is preferably smaller than the thickness of the main dielectric layer 20a, and may be, for example, 5 to 20 nm. If the thickness of the sub-dielectric layer 20b is less than 5 nm, durability may be deteriorated. If the sub-dielectric layer 20b is more than 20 nm, the transmittance may be decreased.
  • the metal layer 30 selectively reflects the sun radiation to provide high shielding performance and low emission.
  • a metal having excellent conductivity may be used, and at least one selected from the group consisting of Ag, Cu, Au, Al and Pt may be used.
  • the metal used as the metal layer 30 may be Ag.
  • the thickness of the metal layer 30 may be 5 to 25 nm. If the thickness of the metal layer 30 is less than 5 nm, the formation of the metal layer 30 is not normally performed and the low emission performance may not be sufficiently improved. If the thickness exceeds 25 nm, the transmittance decreases and the reflectance rises, .
  • the second dielectric layer 21 serves to block oxygen or ions that are transferred to the metal layer 30 during heat treatment such as strengthening or bending, (30) and the topmost layer (50).
  • the second dielectric layer 21 includes a main dielectric layer 21a and optionally one or more sub-dielectric layers 21b may be formed on the upper or lower portion of the main dielectric layer 21a.
  • the main dielectric layer 21a may be an Si-based oxide, a nitride or a nitric oxide containing at least one element selected from AlN x (where 0.5 ⁇ x ⁇ 2) or Al, B, Ti, Nb, Sn and Mo . According to an embodiment of the present invention, the main dielectric layer 21a may use AlN x (where 0.5 ⁇ x ⁇ 2) or SiAlN x (where 1.3 ⁇ x ⁇ 1.5) If it is removed, the deposition rate may be lowered due to excess nitrogen (N 2 ).
  • the sub-dielectric layer 21b may comprise an Si-based oxide, nitride or nitrides containing at least one element selected from AlN x (where 0.5 ⁇ x ⁇ 2) or Al, B, Ti, Nb, And when x is out of the above range, the deposition rate may be lowered due to excess nitrogen (N 2 ).
  • the thickness of the main dielectric layer 21a may be 35 to 70 nm. If the thickness of the main dielectric layer 21a is less than 35 nm, durability may be deteriorated. If the thickness is more than 70 nm, the transmittance may be decreased.
  • the thickness of the sub-dielectric layer 21b is preferably smaller than the thickness of the main dielectric layer 20a, and may be, for example, 5 to 20 nm. If the thickness of the sub-dielectric layer 21b is less than 5 nm, durability may be deteriorated. If the thickness is more than 20 nm, the transmittance may be decreased.
  • the uppermost layer 50 serves to protect the surface of the low-emission glass according to the present invention, and a material having high mechanical strength, low surface roughness, and high transmittance can be used.
  • the uppermost layer 50 may be, for example, an oxide or a nitride or a nitride of Si, Nb, Ti, Zr, Ta or an alloy thereof.
  • a Ti-containing oxide or oxides e.g., TiO z N y
  • the thickness of the top layer 50 may preferably be between 2 and 10 nm. If the thickness of the uppermost layer 50 is less than 2 nm, the durability may be deteriorated. If the thickness of the uppermost layer 50 is more than 10 nm, the transmittance may be decreased or blurring may occur.
  • the low emissivity glass of the present invention includes at least one absorbent layer 40 between the first dielectric layer 20 and the metal layer 30 or between the second dielectric layer 21 and the metal layer 30 ) May be further included.
  • the absorbing layer 40 is a layer in contact with the metal layer 30 and serves to improve the adhesion between the metal layer 30 and the first dielectric layer 20 or between the metal layer 30 and the second dielectric layer 21,
  • the metal layer 30 serves to prevent the movement of O 2 in the air and the diffusion of Na + in the glass during the heat treatment such as bending, and to help the fusion of the metal so that the metal layer 30 can stably behave even at a high heat treatment temperature. Finally, 30) to absorb the O 2 that permeates and help to maintain low radiation performance.
  • At least one selected from the group consisting of Ni, Cr and Ni-Cr alloys may be used as the absorbing layer 40.
  • the alloy composition may be, for example, 75 to 85 wt %, Cr of 15 to 25 wt%.
  • a Ni-Cr alloy may be used as the absorbing layer 40 according to one embodiment of the present invention.
  • the thickness of the absorbing layer 40 may be 0.1 to 10 nm. If the thickness of the absorbing layer 40 is less than 0.1 nm, durability may be deteriorated, and there may be a problem that the coating film becomes cloudy after the heat treatment and the bending process. If the thickness exceeds 10 nm, the transmittance is lowered, There is a problem that the blur of the coating film also increases.
  • FIG 3 is a diagram showing a laminated structure of a multiple (e.g., double or triple) low emissivity glass of the present invention.
  • the low emission glass of the present invention has a structure in which the dielectric layer 22, the metal layer 31 and the absorption layer 41 are sequentially formed between the metal layer 30 and the second dielectric layer 21 in the laminated structure of FIG.
  • Layered structure as shown in FIG. 1 may be a double-low-emission glass in which one of the above multi-layer structures is included in the single-layer structure as shown in FIG. 1, and a double- .
  • the dielectric layer 22 is as serving to block the oxygen or ion that is delivered to the metal layer 31 during heat treatment, such as strengthening and bending steps of the first dielectric layer 20 and second dielectric layer (21), AlN x (Where 0.5 ⁇ x ⁇ 2) A main dielectric layer 22a, AlN x (where 0.5 ⁇ x ⁇ 2) And an upper sub-dielectric layer 22b.
  • the main dielectric layer 22a may be an Si-based oxide, a nitride, or a nitride containing at least one element selected from AlN x (where 0.5 ⁇ x ⁇ 2) or Al, B, Ti, Nb, Sn and Mo . According to an embodiment of the present invention, the main dielectric layer 22a may use AlN x (where 0.5 ⁇ x ⁇ 2) or SiAlN x (where 1.3 ⁇ x ⁇ 1.5) If it is removed, the deposition rate may be lowered due to excess nitrogen (N 2 ).
  • the metal layer 31 selectively reflects the sun radiation to provide high shielding performance and low emission.
  • a metal having excellent conductivity may be used, and at least one selected from the group consisting of Ag, Cu, Au, Al, and Pt may be used.
  • the metal used as the metal layer 31 may be Ag.
  • the thickness of the metal layer 31 may be 5 to 25 nm. If the thickness of the metal layer 31 is less than 5 nm, the formation of the metal layer 31 is not normally performed and the low radiation performance may not be sufficiently improved. If the thickness exceeds 25 nm, the transmittance decreases and the reflectance increases, .
  • the absorbing layer 41 is a layer in contact with the metal layer 31 and functions to improve the adhesion between the metal layer 31 and the dielectric layer 22 or between the metal layer 31 and the second dielectric layer 21,
  • the metal layer 31 serves to interfere with the movement of O 2 in the air and the diffusion of Na + in the glass during the heat treatment of the metal layer 31.
  • the metal layer 31 serves to help fusion of the metal so that the metal layer 31 can stably behave even at a high heat treatment temperature, Absorbing O 2 penetrating into the surface of the substrate, thereby maintaining low radiation performance.
  • At least one selected from the group consisting of Ni, Cr and Ni-Cr alloys may be used as the absorbent layer 41.
  • the composition of the alloy may be, for example, 75 to 85 wt %, Cr of 15 to 25 wt%.
  • a Ni-Cr alloy may be used as the absorption layer 41 according to an embodiment of the present invention.
  • the thickness of the absorbing layer 41 may be 0.1 to 10 nm. If the thickness of the absorbing layer 41 is less than 0.1 nm, durability may be deteriorated, and there may be a problem that the coating film becomes cloudy after the heat treatment and the bending process. If the thickness exceeds 10 nm, the transmittance is lowered, There is a problem that the blur of the coating film also increases.
  • the multi-low emission glass of the present invention at least one of the multi- at least one absorption layer 41 may be further provided between the upper sub-dielectric layer 22b and the metal layer 31 as shown in FIGS.
  • a first dielectric layer (AlNx, 0.5 ⁇ x ⁇ 2) was coated on a 5 mm clear glass substrate to a thickness of 32 nm under nitrogen / argon (nitrogen ratio: 25 vol%) atmosphere using a Magnetron sputter coater, Subsequently, the metal layer (Ag) was coated to a thickness of 10 nm in an argon atmosphere of 100%, and then an absorbing layer (Ni-Cr alloy) was coated to a thickness of 2 nm under an argon atmosphere. Next, a second dielectric layer (SiAlNx, 1.3 ⁇ x ⁇ 1.5) was coated with a thickness of 38 nm under an atmosphere of nitrogen / argon (nitrogen ratio: 25 vol%).
  • a main dielectric layer SiAlN x , 1.3 ⁇ x ⁇ 1.5
  • a main dielectric layer SiAlN x , 1.3 ⁇ x ⁇ 1.5
  • nitrogen ratio: 25 vol% the sub-dielectric layer
  • the sub-dielectric layer AlN x , 0.5 ⁇ x ⁇ 2
  • the metal layer was coated to a thickness of 10 nm in an argon atmosphere of 100%
  • an absorbing layer Ni-Cr alloy
  • the second dielectric layer (SiAlN x , 1.3 ⁇ x ⁇ 1.5) was then coated with a thickness of 38 nm under nitrogen / argon (nitrogen ratio: 25 vol%) atmosphere.
  • Example 1 the first dielectric layer (AlN x, 0.5 ⁇ x ⁇ 2) , instead, the first dielectric layer (SiAlN x, 1.3 ⁇ x ⁇ 1.5), the nitrogen / argon: thickness under (nitrogen ratio of 25% by volume) atmosphere 32 Lt; / RTI > in Example 1, the low-emission glass was produced.
  • Example 2 Low-emission glass.
  • compositions and thicknesses of Examples 1 and 2 and Comparative Examples 1 and 2 are shown in Tables 1 and 2 below.
  • Example Film type (film thickness: nm) One Glass / AlN x (32 nm) / Ag (10 nm) / NiCr (2 nm) / SiAlN x (35 nm) / TiO z N y (5 nm) 2 Glass / SiAlN x (32nm) / AlN x (6nm) / NiCr (2nm) / Ag (10nm) / NiCr (2nm) / SiAlN x (38nm) / TiO z N y (5nm)
  • the transmittance and reflectance of the low-emission glass-coated surface obtained in Examples 1 and 2 and Comparative Examples 1 and 2 were measured, and the surface resistance was measured using a non-contact sheet resistance measuring apparatus.
  • the D65 standard light source 10 was measured according to the KS L 2514 standard in the wavelength range of 380 to 780 nm.
  • test specimen having the size of 100 mm ⁇ 100 mm corresponding to the left, middle, and right parts of the product shall be used as the specimen.
  • the sub-dielectric layer (AlN x (0.5 ⁇ x ⁇ 2)) is included in the lower part of the metal layer, the degree of crystallization of the metal layer (Ag) can be increased and the sheet resistance can be reduced. And the optical defects such as diffusion into the dielectric layer can be prevented and stabilized.

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

Abstract

La présente invention concerne un verre à faible émissivité comprenant : un substrat de verre ; une première couche diélectrique formée sur le substrat de verre ; une couche métallique formée sur la première couche diélectrique ; une seconde couche diélectrique formée sur la couche métallique ; et une couche supérieure formée sur la seconde couche diélectrique, la première couche diélectrique comprenant de l'AlNx (0,5<x<2). Par conséquent, la présente invention concerne un verre à faible émissivité comprenant une couche métallique ayant une cristallinité améliorée.
PCT/KR2018/008378 2017-07-25 2018-07-25 Verre à faible émissivité Ceased WO2019022484A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR20170093848 2017-07-25
KR10-2017-0093848 2017-07-25

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WO2019022484A2 true WO2019022484A2 (fr) 2019-01-31
WO2019022484A3 WO2019022484A3 (fr) 2019-03-21

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101047177B1 (ko) * 2004-12-31 2011-07-07 주식회사 케이씨씨 내구성이 향상된 저방사 유리
KR101302259B1 (ko) * 2008-11-21 2013-09-02 (주)엘지하우시스 내구성이 우수한 저방사 유리
KR101015072B1 (ko) * 2009-02-27 2011-02-16 주식회사 케이씨씨 열처리후 흐림 현상이 감소된 열처리 가능한 저방사 유리 및 그 제조방법
KR101381531B1 (ko) * 2011-08-18 2014-04-07 (주)엘지하우시스 열처리가 가능한 저방사 유리 및 이의 제조방법
KR20130051521A (ko) * 2011-11-09 2013-05-21 주식회사 케이씨씨 열처리 가능한 저방사 유리 및 그 제조방법

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