WO2017126875A1 - Verre à faible émissivité et procédé de production associé - Google Patents

Verre à faible émissivité et procédé de production associé Download PDF

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Publication number
WO2017126875A1
WO2017126875A1 PCT/KR2017/000590 KR2017000590W WO2017126875A1 WO 2017126875 A1 WO2017126875 A1 WO 2017126875A1 KR 2017000590 W KR2017000590 W KR 2017000590W WO 2017126875 A1 WO2017126875 A1 WO 2017126875A1
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WO
WIPO (PCT)
Prior art keywords
dielectric layer
glass
low
layer
thickness
Prior art date
Application number
PCT/KR2017/000590
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English (en)
Korean (ko)
Inventor
오영훈
권승민
강현민
Original Assignee
주식회사 케이씨씨
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.)
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Application filed by 주식회사 케이씨씨 filed Critical 주식회사 케이씨씨
Publication of WO2017126875A1 publication Critical patent/WO2017126875A1/fr

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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
    • C03C17/34—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
    • 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
    • C03C17/3602—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 the metal being present as a layer
    • C03C17/3657—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 the metal being present as a layer the multilayer coating having optical properties
    • C03C17/366—Low-emissivity or solar control 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
    • 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
    • C03C17/3602—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 the metal being present as a layer
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • 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
    • C03C17/3602—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 the metal being present as a layer
    • C03C17/3657—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 the metal being present as a layer the multilayer coating having optical properties

Definitions

  • the present invention relates to a low-emissive glass and a method for producing the same.
  • Low-emissivity glass deposits metal with high reflectance in the infrared region such as silver (Ag) on the transparent glass to maintain the transparency of the glass, and prevents the heat of the indoor heating from being discharged to the outside in the winter and enters the interior in the summer. It is a functional building material that reflects radiant heat. Low-emissivity glass used in non-residential buildings requires high insulation / shielding performance and beautiful appearance rather than high transmittance, but low-emissivity glass used in residential buildings requires high transmittance for visibility. In addition, since the amount of use is higher than that of low-emission glass used in non-residential buildings, a high level of durability that can be used in many processing agencies must be ensured.
  • Such low-emissive glass can be classified into two types according to the manufacturing method, soft low-E glass by the sputtering process and hard by Atmospheric Pressure Chemical Vapor Deposition. Hard Low-E glass.
  • the structure of the low-emissive glass manufactured by the sputtering method includes an infrared reflecting metal layer, and has a dielectric layer above and below the metal layer to protect the metal layer.
  • the infrared reflecting metal layer is oxidized or nitrided by oxygen or nitrogen injected into the chamber, resulting in high emissivity, thereby reducing the characteristics of the low-emissive glass. There was a problem of losing.
  • U. S. Patent No. 6,804, 048 discloses heat-treatable low-emissive glass having a structure of glass / first dielectric layer / infrared reflective metal layer / protective layer / second dielectric layer.
  • this low-emission glass had a disadvantage in that scratches were generated by foreign matters in the coating film during the heat treatment or bending process.
  • the present invention provides a low-emissivity glass having high transmittance, low emissivity, and improved durability.
  • the present invention provides a method for producing the low-emissive glass.
  • the low-emissive glass of the present invention includes a glass substrate and a first dielectric layer, a first auxiliary dielectric layer, a reflective metal layer, a second auxiliary dielectric layer, a second dielectric layer, and a top protective layer sequentially stacked from the glass substrate.
  • the low-emissive glass of the present invention comprises a first dielectric layer on a glass substrate; A first auxiliary dielectric layer; Reflective metal layer; A second auxiliary dielectric layer; A second dielectric layer; And a top protective layer may be sequentially coated, and the second auxiliary dielectric layer may be coated on the reflective metal layer under argon without oxygen.
  • the low-emissivity glass of the present invention not only has high transmittance and low emissivity, but also reduces scratch occurrence and is excellent in moisture resistance.
  • the reflective metal layer is prevented from being oxidized or nitrided by oxygen or nitrogen to increase the emissivity, it is not necessary to form a separate metal protective layer on the reflective metal layer.
  • the low-emissive glass of the present invention includes a glass substrate and a first dielectric layer, a first auxiliary dielectric layer, a reflective metal layer, a second auxiliary dielectric layer, a second dielectric layer, and a top protective layer sequentially stacked from the glass substrate.
  • glass substrate glass commonly used in the art may be used without limitation, and for example, conventional soda lime glass may be used.
  • the glass substrate may have a thickness of about 2 to 12 mm, or about 6 mm, but may not be limited thereto.
  • Emissivity of the low-emissivity glass of the present invention may preferably be about 0.04 to 0.08, visible light transmittance of 70% or more, but may not be limited thereto.
  • the first dielectric layer included in the low-emissivity glass of the present invention may have a thickness of about 20 to 50 nm, and is selected from the group consisting of Zn, Si, Zr, Ta, Sn, Nb, Al, Ti, and alloys thereof. Nitride or oxynitride of the metal may be included, but may not be limited thereto.
  • the first dielectric layer may have a function of protecting the reflective metal layer from ions or oxygen during heat treatment and controlling optical properties.
  • a material having a refractive index of about 1.8 or more and an absorption coefficient of about 0.1 or less may be used to prevent a decrease in transmittance, but may not be limited thereto.
  • the thickness of the first dielectric layer is less than 20 nm, durability may decrease, and when it exceeds 50 nm, transmittance may be reduced.
  • the first auxiliary dielectric layer included in the low-emissivity glass of the present invention may have a thickness of about 5 to 10 nm, and at least one selected from the group consisting of Sn, Nb, Al, Sb, Mo, Cr, Ti, and Ni. It may include a Zn-based oxide containing an element, but may not be limited thereto.
  • the first auxiliary dielectric layer may have a function of improving the crystallinity of the reflective metal layer and at the same time improving the low radiation property and durability.
  • a Zn-based oxide may be used as the first auxiliary dielectric layer, and a small amount of Al and / or Sn may be additionally included.
  • the first auxiliary dielectric layer may include ZnAlO, but may not be limited thereto.
  • the thickness of the first auxiliary dielectric layer is less than 5 nm, the crystallization of the reflective metal layer may be insufficient, and when it exceeds 10 nm, durability may be reduced.
  • the reflective metal layer included in the low-emissivity glass of the present invention may have a thickness of about 5 to 20 nm, and may include one or more metals selected from the group consisting of Ag, Cu, Au, Al, and Pt. This may not be limited.
  • the reflective metal layer may be a metal having excellent conductivity.
  • the second auxiliary dielectric layer included in the low-emissivity glass of the present invention may have a thickness of about 5 to 10 nm, and at least one selected from the group consisting of Sn, Nb, Al, Sb, Mo, Cr, Ti, and Ni. It may include a Zn-based oxide containing an element, but may not be limited thereto.
  • a Zn-based oxide may be used as the first auxiliary dielectric layer.
  • the second auxiliary dielectric layer may be deposited to be in direct contact with the reflective metal layer by using a Zn-based oxide, and at this time, the deposition atmosphere may be controlled so that oxidation does not occur in the reflective metal layer.
  • an argon atmosphere may be used, but is not limited thereto.
  • the second dielectric layer included in the low-emissivity glass of the present invention may have a thickness of about 20 to 50 nm, and is selected from the group consisting of Zn, Si, Zr, Ta, Sn, Nb, Al, Ti, and alloys thereof. Nitride or oxynitride of the metal may be included, but may not be limited thereto.
  • the second dielectric layer may have a function of controlling optical properties while protecting the reflective metal layer from ions or oxygen during heat treatment.
  • a material having a refractive index of about 1.8 or more and an absorption coefficient of about 0.1 or less may be used to prevent a decrease in transmittance, but may not be limited thereto.
  • the thickness of the second dielectric layer is less than 20 nm, durability may decrease, and when it exceeds 50 nm, transmittance may be reduced.
  • the uppermost protective layer included in the low-emissivity glass of the present invention may have a thickness of about 2 to 15 nm, an oxide of a metal selected from the group consisting of Si, Nb, Ti, Zr, Ta, and alloys thereof, It may include, but is not limited to, nitrides or oxynitrides.
  • the uppermost protective layer may function to protect the dielectric layer and the reflective metal layer.
  • a material having high mechanical strength, low surface roughness, and high transmittance may be used.
  • the reflective metal layer can be easily damaged by scratches generated by the rubbing, and when the uppermost protective layer having a small surface roughness is applied, it is possible to prevent damage due to scratches.
  • the visible light transmittance of the low-emissivity glass of the present invention may be about 80% to 90%, for example, the visible light transmittance may be about 82% to 90%, about 85 to 90%, or about 85 to 86%, but It may not be limited.
  • the glass substrate the first dielectric layer; A first auxiliary dielectric layer; Reflective metal layer; A second auxiliary dielectric layer; A second dielectric layer; And it can be prepared by sequentially coating the top protective layer.
  • the reflective metal layer may be prevented from being oxidized or nitrided by oxygen or nitrogen to increase emissivity. It is not necessary to form a separate metal protective layer on the reflective metal layer.
  • Coating of the respective functional layers can be performed using a magnetron sputtering method.
  • the low-emissive glass of the present invention can be produced by the following procedure according to the vacuum sputtering method.
  • the glass substrate is placed in a vacuum chamber and evacuated until the degree of vacuum becomes 5 ⁇ 10 ⁇ 7 to 9 ⁇ 10 ⁇ 5 torr to form a vacuum.
  • argon (Ar) oxygen (O 2 ), nitrogen (N 2 ) gas, etc. are introduced into the vacuum chamber, a discharge occurs when a direct current or an alternating voltage is applied between the two electrodes.
  • gas ions collide with a negative electrode provided with a metal target to be deposited on it, atoms are released from the metal target and stacked on the substrate.
  • An appropriate gas is introduced according to the type of coating film to be laminated, and the thickness of the coating film to be formed is appropriately controlled by appropriately adjusting the deposition rate of each coating film and the time exposed to the sputtering process. At this time, the temperature of the substrate is not particularly limited.
  • low-emissivity glass in which a multilayer coating film having the following composition and thickness were formed on a 6-mm-thick soda-lime transparent glass substrate, respectively.
  • the first dielectric layer, SiAlN x (x 1.3-1.5), was deposited on a glass substrate under an atmosphere of nitrogen / argon (nitrogen ratio: 45-60% by volume), and the first auxiliary dielectric layer, ZnAlO, was oxygen / argon (oxygen). Ratio: 60-70% by volume) was deposited on the first dielectric layer under an atmosphere.
  • An Ag reflective metal layer was deposited on the first auxiliary dielectric layer under an argon atmosphere.
  • a second auxiliary dielectric layer, ZnAlO layer was deposited on the reflective metal layer using a ZnAlO ceramic target under an argon atmosphere containing no oxygen.
  • the first auxiliary dielectric layer, ZnAlO layer was coated at 10 nm under an argon / oxygen atmosphere.
  • an Ag layer which is a reflective metal layer, was coated at about 15 nm under an argon atmosphere.
  • a second auxiliary dielectric layer, ZnAlO layer was coated at 10 nm under an argon atmosphere.
  • the film structure of the low-emissive glass of the example is as follows: SiAlN x / ZnAlO / Ag / ZnAlO / SiAlN x / TiO x N y .
  • the first auxiliary dielectric layer, ZnAlO layer was coated at 10 nm under an argon / oxygen atmosphere.
  • an Ag layer which is a reflective metal layer, was coated at about 15 nm under an argon atmosphere.
  • a second auxiliary dielectric layer, ZnAlO layer was coated at 10 nm under an argon atmosphere.
  • the film structure of the low-emissive glass of Comparative Example 1 is as follows: SiAlN x / ZnAlO / Ag / ZnAlO / SiAlN x .
  • the TiO x ceramic target was deposited to a thickness of 5 nm under a nitrogen / argon (nitrogen ratio: 45 to 60% by volume) atmosphere to finally prepare a low-emissive glass.
  • the film structure of the low-emissivity glass of Comparative Example 2 was prepared as follows: SiAlN x / Ag / ZnAlO / SiAlN x / TiO x N y .
  • the first auxiliary dielectric layer, ZnAlO was coated at 10 nm under an argon / oxygen atmosphere
  • the Ag layer which is a reflective metal layer, was coated at about 15 nm under an argon atmosphere.
  • the second auxiliary dielectric layer, ZnAlO layer was then coated at 10 nm under argon / oxygen atmosphere.
  • a low-emissive glass was finally prepared by depositing at a thickness of 5 nm under a nitrogen / argon (nitrogen ratio: 45-60 vol%) atmosphere using a TiO x ceramic target.
  • the film structure of the low-emissive glass of Comparative Example 2 was prepared as follows: SiAlN x / ZnAlO / Ag / ZnAlO / SiAlN x / TiO x N y .
  • each of the low-emissive glass samples prepared according to the Examples and Comparative Examples 1 to 3 is shown in Table 1 below. Specifically, each of the low-emissivity glass samples was measured transmittance in accordance with the D65 standard light source 10 degrees KS L 2514 in the wavelength range of 380 ⁇ 780 nm, and the sheet resistance was measured through a surface resistance meter (non-contact sheet resistance meter). Emissivity was measured according to KS L 2525 standard using an infrared spectrometer (FTIR). Emissivity is a value measured by Ag, a reflective metal layer, which is one of the properties that can be used as a low-emission glass.
  • FTIR infrared spectrometer
  • the brush test cuts the sample into 100 x 300 mm size by ASTM D 2486 method, sprays distilled water on the coated surface, reciprocates 200 times with a brush for Roy glass, and checks the scratch number of the coated film. It proceeded by the method.
  • the moisture resistance test cuts the sample into 300 x 300 mm size and checks the number of pinholes on the coated surface after storing it in a constant temperature and humidity chamber maintained at a temperature of 30 ° C. and a humidity of 80% for three days. Proceed by the method.
  • Comparative Example 1 which does not include the uppermost protective layer, was found to be inferior in durability because many scratches and pinholes were observed.
  • Comparative Example 2 not including the first auxiliary dielectric layer was confirmed that the emissivity is lowered.
  • the second auxiliary dielectric layer on the reflective metal layer is argon / oxygen It was confirmed that the low-emissivity glass of Comparative Example 3 prepared by coating in an atmosphere significantly reduced transmittance and emissivity.

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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)
  • Surface Treatment Of Glass (AREA)

Abstract

La présente invention concerne un verre à faible émissivité et son procédé de fabrication, le verre à faible émissivité comprenant un substrat en verre, et une première couche diélectrique, une première couche diélectrique auxiliaire, une couche métallique réfléchissante, une seconde couche diélectrique auxiliaire, une seconde couche diélectrique, et une couche de protection supérieure, qui sont empilées séquentiellement sur le substrat de verre.
PCT/KR2017/000590 2016-01-18 2017-01-18 Verre à faible émissivité et procédé de production associé WO2017126875A1 (fr)

Applications Claiming Priority (2)

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KR10-2016-0005852 2016-01-18
KR20160005852 2016-01-18

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WO2017126875A1 true WO2017126875A1 (fr) 2017-07-27

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11279651B2 (en) 2018-07-16 2022-03-22 Guardian Glass, LLC Low-E matchable coated articles having absorber film and corresponding methods
CN114853360A (zh) * 2022-05-31 2022-08-05 长兴旗滨节能玻璃有限公司 一种减反射低辐射玻璃及中空玻璃

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108975726B (zh) * 2018-09-30 2024-02-23 吴江南玻华东工程玻璃有限公司 超低反可钢化low-e玻璃
KR102259346B1 (ko) * 2019-09-19 2021-06-02 주식회사 케이씨씨글라스 저방사 유리
KR102269783B1 (ko) * 2019-12-19 2021-06-28 주식회사 케이씨씨글라스 저방사 유리

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KR20090099364A (ko) * 2008-03-17 2009-09-22 주식회사 케이씨씨 내구성이 우수한 열처리 가능한 저방사 유리 및 그제조방법
KR101015072B1 (ko) * 2009-02-27 2011-02-16 주식회사 케이씨씨 열처리후 흐림 현상이 감소된 열처리 가능한 저방사 유리 및 그 제조방법
KR20110062566A (ko) * 2009-12-03 2011-06-10 현대자동차주식회사 굽힘 및 열처리가 가능한 저방사유리 및 그 제조방법
KR20130051521A (ko) * 2011-11-09 2013-05-21 주식회사 케이씨씨 열처리 가능한 저방사 유리 및 그 제조방법
KR101302273B1 (ko) * 2008-08-14 2013-09-02 (주)엘지하우시스 저방사 유리 및 이의 제조방법

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JP2008297177A (ja) * 2007-06-01 2008-12-11 Nippon Sheet Glass Co Ltd サーモクロミックガラスおよびサーモクロミック複層ガラス
KR20110033769A (ko) * 2009-09-25 2011-03-31 (주)엘지하우시스 저방사 유리 및 이의 제조방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20090099364A (ko) * 2008-03-17 2009-09-22 주식회사 케이씨씨 내구성이 우수한 열처리 가능한 저방사 유리 및 그제조방법
KR101302273B1 (ko) * 2008-08-14 2013-09-02 (주)엘지하우시스 저방사 유리 및 이의 제조방법
KR101015072B1 (ko) * 2009-02-27 2011-02-16 주식회사 케이씨씨 열처리후 흐림 현상이 감소된 열처리 가능한 저방사 유리 및 그 제조방법
KR20110062566A (ko) * 2009-12-03 2011-06-10 현대자동차주식회사 굽힘 및 열처리가 가능한 저방사유리 및 그 제조방법
KR20130051521A (ko) * 2011-11-09 2013-05-21 주식회사 케이씨씨 열처리 가능한 저방사 유리 및 그 제조방법

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11279651B2 (en) 2018-07-16 2022-03-22 Guardian Glass, LLC Low-E matchable coated articles having absorber film and corresponding methods
CN114853360A (zh) * 2022-05-31 2022-08-05 长兴旗滨节能玻璃有限公司 一种减反射低辐射玻璃及中空玻璃

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