KR101642654B1 - Low emissivity substrate, and preparation method there of - Google Patents

Low emissivity substrate, and preparation method there of Download PDF

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KR101642654B1
KR101642654B1 KR1020150055088A KR20150055088A KR101642654B1 KR 101642654 B1 KR101642654 B1 KR 101642654B1 KR 1020150055088 A KR1020150055088 A KR 1020150055088A KR 20150055088 A KR20150055088 A KR 20150055088A KR 101642654 B1 KR101642654 B1 KR 101642654B1
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South Korea
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substrate
low
resin
layer
infrared
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KR1020150055088A
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Korean (ko)
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김대일
전재현
공태경
김소영
김승홍
김선경
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울산대학교 산학협력단
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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
    • C03C17/3411—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
    • 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
    • C03C17/3613—Coatings of type glass/inorganic compound/metal/inorganic compound/metal/other
    • 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
    • C03C17/3642—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 containing a metal layer

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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)
  • Laminated Bodies (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to a low-emission substrate that is surface-treated with an electron beam derived from a plasma and includes a crystalline infrared reflecting layer and a dielectric layer, and a method of manufacturing the same. The low-emission substrate according to the present invention is excellent in visible light transmittance and infrared reflectance by processing a surface of a low-emission substrate manufactured by a sputtering method with an electron beam derived from a plasma and including a crystalline infrared reflecting layer and a dielectric layer. In addition, the manufacturing method of the low-emission substrate has an economical advantage because it is easy to apply to existing low-emission substrate and easy to process large area.

Description

TECHNICAL FIELD [0001] The present invention relates to a low-emission substrate and a preparation method therefor,

The present invention relates to a low-emission substrate comprising a crystalline infrared reflecting layer and a dielectric layer treated by an electron beam derived from a plasma and a method of manufacturing the same.

Recently, the use of low emission substrates such as low emissivity glass has been increasing in order to block the infrared radiation incident on the sunlight from the building and to increase the transmittance of the visible light.

Such low-emission glass is generally manufactured by forming a metal layer or the like through sputtering of a metal target in a vacuum chamber. Specifically, the method first forms a dielectric layer on a glass substrate prior to sputtering of the metal. Next, the glass substrate is charged into the chamber, a vacuum and an inert gas atmosphere are created, and then a DC or AC voltage is applied between the two electrodes to generate a plasma of the gas. With such a plasma, gas ions collide with a cathode provided with a metal target, and atoms are released from the metal target, thereby depositing a metal layer on the dielectric layer. Finally, a further dielectric layer capable of protecting the metal layer is formed on the metal layer to produce a low-emission glass.

At this time, in order to improve the infrared reflectance or the visible light transmittance of the low-emission glass, the thickness of the light blocking layer (metal layer) may be appropriately adjusted through a method such as controlling the time of exposure to the sputtering process. However, in the conventional sputtering method, when the thickness of the metal layer is increased to increase the infrared reflectance, the transmittance of the visible light is lowered. On the other hand, if the thickness of the metal layer is decreased to increase the transmittance of the visible light, There is a desperate need to develop a technique capable of simultaneously improving the light transmittance and the infrared reflectance.

Korean Patent Publication No. 2011-0017580.

Accordingly, an object of the present invention is to provide a low-emission substrate having improved visible light transmittance and infrared reflectance.

Another object of the present invention is to provide a method of manufacturing the low-emission substrate.

In order to achieve the above object, the present invention provides, in one embodiment,

Transparent substrate,

A first dielectric layer provided on the transparent substrate,

An infrared reflecting layer provided on the first dielectric layer, and

And a second dielectric layer provided on the infrared reflecting layer,

In X-ray diffraction measurement,

Lt; RTI ID = 0.0 > 25 < / RTI > 0.5 and < RTI ID = 0.0 > 49 < / RTI >

In addition, the present invention, in one embodiment,

And irradiating an electron beam derived from the plasma to the surface of the low radiation substrate.

The low-emission substrate according to the present invention is excellent in visible light transmittance and infrared reflectance because the surface of the low-emission substrate manufactured by the sputtering method is electron beam-processed by plasma-derived electron beam to include a crystalline infrared reflective layer and a dielectric layer. In addition, the manufacturing method of the low-emission substrate has an economical advantage because it is easy to apply to existing low-emission substrate and easy to process large area.

1 and 2 are sectional views showing the structure of a low-emission substrate of the present invention according to an embodiment.
FIG. 3 is a graph showing the light transmittance and the light reflectance of the low-emission substrate according to the electron beam irradiation energy in one embodiment.

While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail.

It should be understood, however, that the invention is not intended to be limited to the particular embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

In the present invention, the terms "comprising" or "having ", and the like, specify that the presence of a feature, a number, a step, an operation, an element, a component, But do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, or combinations thereof.

It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory and are intended to provide further explanation of the invention as claimed.

Hereinafter, the present invention will be described in detail with reference to the drawings, and the same or corresponding components are denoted by the same reference numerals regardless of the reference numerals, and a duplicate description thereof will be omitted.

In the present invention, "visible light" means light having a wavelength of 380 nm to 780 nm, and "infrared light " means light having wavelengths exceeding 780 nm.

The present invention provides a low-emission substrate improved in visible light transmittance and / or infrared reflectance by processing an electron beam derived from a plasma and including a crystalline infrared reflecting layer and a dielectric layer, and a method of manufacturing the same.

Generally, a low-emission glass is produced by a sputtering method of forming a metal layer or the like through sputtering of a metal target in a vacuum chamber. At this time, in order to improve the infrared reflectance and the visible light transmittance of the low-emission glass, the thickness of the light blocking layer (metal layer) can be appropriately controlled through a method such as controlling the exposure time to the sputtering process. However, in the conventional sputtering method, when the thickness of the metal layer is increased to increase the infrared reflectance, the transmittance of the visible light is lowered. On the other hand, if the thickness of the metal layer is decreased to increase the transmittance of the visible light, There is a desperate need to develop a technique capable of simultaneously improving the light transmittance and the infrared reflectance.

However, the low-emission substrate according to the present invention is excellent in visible light transmittance and infrared reflectance because the surface of the low-emission substrate manufactured by the sputtering method is electron beam-processed by plasma-derived electron beam to include a crystalline infrared reflecting layer and a dielectric layer. In addition, the manufacturing method of the low-emission substrate has an economical advantage because it is easy to apply to existing low-emission substrate and easy to process large area.

Hereinafter, the present invention will be described in detail.

The present invention, in one embodiment,

Transparent substrate,

A first dielectric layer provided on the transparent substrate,

An infrared reflecting layer provided on the first dielectric layer, and

And a second dielectric layer provided on the infrared reflecting layer,

In X-ray diffraction measurement,

Lt; RTI ID = 0.0 > 25 < / RTI > 0.5 and < RTI ID = 0.0 > 49 < / RTI >

The low-emission substrate according to the present invention includes a transparent substrate, a first dielectric layer, an infrared reflection layer, and a second dielectric layer, wherein the infrared reflection layer is disposed between the first and second dielectric layers on both sides and includes a crystalline layer of the infrared reflection layer and the dielectric layer The average transmittance for visible light and the average reflectance for infrared light are respectively 70% or more, specifically 75% or more, 76% or more, 77% or more, 78% or more or 80% or more. Since the infrared reflecting layer and the dielectric layer have a crystalline form, the crystalline peak can be confirmed by performing X-ray diffraction analysis on the low-radiated substrate. As one example, when silver (Ag) is included as the infrared reflecting layer and titanium oxide (TiO 2 ) is included as the second dielectric layer, the diffraction peak of 38 ± 0.5 ° represented by 2θ, There may be diffraction peaks of 25 ± 0.5 ° and 49 ± 0.5 ° indicating crystallinity (see Example 1).

Figures 1 and 2 are cross-sectional views showing the structure of a low emissivity substrate according to the present invention. The low-emission substrate according to the present invention may have a structure in which a transparent substrate 10, a first dielectric layer 20, an infrared reflective layer 30, and a second dielectric layer 40 are sequentially stacked as shown in FIG. In addition, as shown in FIG. 2, the second dielectric layer 40 may further include a metal layer 50 and a third dielectric layer 60 on the second dielectric layer 40 shown in FIG. Hereinafter, with reference to Figs. 1 and 2, the respective components of the low radiation substrate will be described in detail.

First, the transparent substrate 10 serves as a base substrate and serves as a basic framework of the low-emission substrate. The transparent substrate 10 is not particularly limited as long as it has a high light transmittance. As an example, the transparent substrate 10 may be formed of a transparent glass substrate, or a transparent glass substrate may be used, or a transparent glass substrate may be used. Alternatively, a transparent glass substrate may be used, or a transparent glass substrate may be used. A transparent resin substrate containing at least one of acrylic resin, polyvinyl chloride resin, polyvinylidene chloride resin, polystyrene resin, polyvinyl alcohol resin, polyarylate resin and polyphenylene sulfide resin can be used have.

The average thickness of the transparent substrate 10 is not particularly limited as long as it does not decrease the light transmittance. Specifically, the average thickness is 0.3 mm or less; 0.28 mm or less; 0.25 mm or less; 0.24 mm or less; Or 0.23 mm or less.

Next, the first to third dielectric layers 20, 40, and 60 reduce the surface reflection, thereby increasing the density of incident light, thereby increasing the light transmittance of the low-emission substrate and eliminating interference or scattering due to reflected light do. Further, it has a function of preventing the discoloration due to oxidation of the infrared ray reflective layer 30 or damage caused by an external impact, thereby improving the deterioration of the infrared reflectance.

For this purpose, the first to third dielectric layers 20, 40 and 60 have a high refractive index and a low light absorption rate for suppressing surface reflection and improving transmittance, and have excellent surface hardness in order to protect the infrared ray reflective layer 30. The dielectric layers 20, 40, and 60 that satisfy these conditions can be formed of a material selected from the group consisting of TiO 2 , Al 2 O 3 , ZrO 2 , Ta 2 O 5 , Nb 2 O 5 ), lanthanum oxide (La 2 O 3 ), yttrium oxide (Y 2 O 3 ), zinc oxide (ZnO), zinc sulfide (ZnS) and indium oxide (In 2 O 3 ) And may include one or more species. Specifically, the dielectric layer may include at least one of titanium oxide (TiO 2 ), aluminum oxide (Al 2 O 3 ), zinc oxide (ZnO), and indium oxide (In 2 O 3 ) It may include (TiO 2).

In addition, although the shape of the dielectric layer is not particularly limited, it may preferably have a crystalline form capable of improving light transmittance.

Next, the infrared ray reflective layer 30 reflects infrared rays having a wavelength of about 380 nm to 780 nm, and the infrared ray reflective layer 30 is not particularly limited as long as the refractive index is low and the reflectance to infrared rays is high Can be used. As one example, it may include at least one metal selected from the group consisting of gold (Au), silver (Ag), aluminum (Al), and copper (Cu) .

In addition, the average thickness of the infrared ray reflective layer 30 can be appropriately adjusted within a range that does not reduce the infrared reflectance and the visible light transmittance. Specifically, the average thickness of the infrared ray reflective layer 30 may be 10 to 50 nm, more specifically 10 to 40 nm; 10 to 30 nm; 20 to 40 nm; Or 10 to 20 nm.

Next, the metal layer 50 is formed on the second dielectric layer and serves to reflect infrared rays incident on the surface of the low-emission substrate. The low emission substrate according to the present invention can further improve the effect of reflecting infrared rays by providing the metal layer 50 that reflects infrared rays together with the infrared ray reflection layer 30. [ At this time, the metal layer 50 may include gold (Au) and / or silver (Ag) having a low refractive index and a high infrared reflectance, and may have a crystalline form like the infrared reflecting layer 30.

The average thickness of the metal layer 50 may be 10 to 50 nm, more specifically 10 to 40 nm; 10 to 30 nm; 20 to 40 nm; Or 10 to 20 nm.

In the low-emission substrate according to the present invention, the sum of the average thicknesses of the respective layers laminated on the transparent substrate 10 may be 100 nm or less, and the average thickness of the infrared reflective layer 30 and the average thickness of the metal layer 50 The sum of the average thickness may be between 10 and 50 nm.

In general, the phase change of light is the same as a function of the refractive index and the thickness of the thin film. Therefore, in order to suppress the surface reflection of incident light, the low-emission substrate according to the present invention has a total thickness of layers laminated on the transparent substrate 10, The sum of the average thicknesses of the respective layers laminated on the transparent substrate 10 can be controlled to 100 nm or less according to the refractive index of the dielectric layers 20, 40, In addition, when the low-emission substrate includes the metal layer 50, the sum of the average thickness of the infrared ray reflective layer 30 and the average thickness of the metal layer 50 is set to 10 to 50 nm, specifically, 10 to 40 nm; 10 to 30 nm; 20 to 40 nm; Or 10 to 20 nm, it is possible to prevent the infrared ray reflecting layer 30 and the metal layer 50 from being formed in a sufficient thickness and preventing the infrared ray from being properly reflected or the transmittance of the infrared ray due to the excessive thickness to decrease.

Since the low-emission substrate according to the present invention includes the infrared reflective layer 30 and the dielectric layers 20, 40, and 60 having a crystalline form, the visible light transmittance and the infrared reflectance are excellent at 80% or more.

The present invention measures the light transmittance and the light reflectance of a low-emission substrate including a crystalline type infrared reflecting layer and a dielectric layer, and a low-emission substrate including an amorphous infrared reflecting layer. As a result, it was found that the low-emission substrate of the present invention had an average transmittance of about 80.7% for visible light and an average reflectance of about 80.4% for infrared light. On the other hand, low emission substrates containing an amorphous infrared reflective layer were found to be about 80.2% and 77.5%, respectively. From these results, it can be seen that the crystalline form of the infrared reflection layer improves both the visible light transmittance and the infrared reflectance compared to the amorphous infrared reflection layer, and particularly the infrared reflectance improves by about 3% (see Experimental Example 2).

In addition, the present invention, in one embodiment,

Irradiating the surface of the low-emission substrate with an electron beam derived from the plasma.

The method of manufacturing a low-radiation substrate according to the present invention can include the steps of manufacturing a low-radiation substrate and irradiating the low-radiation substrate produced on the surface of the low-radiation substrate with electrons derived from the plasma.

The step of irradiating the electron beam is a step of modifying the amorphous type infrared reflecting layer provided in the substrate with a crystalline infrared reflecting layer by irradiating the electron beam, thereby improving the visible light transmittance and the infrared reflectance of the low emitting substrate at the same time.

At this time, the plasma may be formed at RF power of 1 to 20 W / cm 2 of 12 to 15 MHz radio frequency (RF). More specifically a 1 to 15 W / cm 2 power of 12 to 14 MHz Radio Frequency (RF); 1 to 10 W / cm 2 power; 2 to 8 W / cm 2 power; 8 to 12 W / cm 2 power; 10 to 20 W / cm 2 power; Or 3 to 7 W / cm < 2 > power. In the present invention, by controlling the electric power in the above-described range in the plasma atmosphere formation, the plasma of the low density at low power is formed and the infrared ray reflective layer 30 is not denatured into crystalline, or the infrared ray reflective layer 30 and the second dielectric layer It is possible to prevent the problem of melting and mixing of the resin 40.

Also, the step of irradiating the electron beam may be performed in an inert gas atmosphere injected at an injection amount of 1 to 20 sccm, wherein the operating pressure may be 1.0 × 10 -4 Torr to 1.0 × 10 -6 Torr. The inert gas may be argon (Ar), helium (He), neon (Ne), krypton (Kr), or the like.

Further, the average acceleration energy of the electron beam may be 50 to 5000 eV. Specifically, the average acceleration energy of the electron beam is 50 to 4500 eV; 100 to 4000 eV; 100 to 3500 eV; 100 to 2000 eV; 250 to 3500 eV; 130 to 3200 eV; 100 to 1500 eV; 250 to 1500 eV, or 250 to 1100 eV. The present invention is capable of easily modifying the infrared reflecting layer and the dielectric layer from amorphous to crystalline in the average acceleration energy range and preventing melting of the dielectric layer and the infrared reflecting layer or the dielectric layer and the metal layer at a high average acceleration energy, It is possible to prevent the problem that the transmittance is lowered.

Meanwhile, the low-emission substrate according to the present invention can be manufactured by a method commonly used in the art. Specifically, the infrared radiation reflective layer 30, the metal layer 50, and the first to third dielectric layers 20, 40, and 60 of the low-emission substrate may be formed by a PECVD (Plasma Enhanced Chemical Vapor Deposition) method, a sputtering method, a MOCVD deposited on the transparent substrate 10 by using a vapor deposition method, an e-beam evaporation method, an imprint method, a wet coating method, or the like, preferably by a RF / DC sputtering method .

Hereinafter, the present invention will be described in more detail with reference to Examples and Experimental Examples.

However, the following Examples and Experimental Examples are merely illustrative of the present invention, and the present invention is not limited to the following Examples and Experimental Examples.

Example  1 and 2.

A transparent glass substrate (corning 1747) was introduced as a transparent substrate into a dry evaporator and fixed, and the inside of the reactor was converted to a vacuum of about 1 x 10 -7 Torr. When the pressure condition of the evaporator is satisfied, argon (10 sccm) is injected into the evaporator so as to maintain it at 1 × 10 -3 Torr, and the sputtering gun installed in the evaporator is supplied with 50 W power of 13.56 MHz radio frequency To form a plasma. Thereafter, titanium oxide (TiO 2 ), silver (Ag) and titanium oxide (TiO 2 ) were deposited on the transparent glass substrate by RF / DC sputtering so as to have an average thickness of 24 nm, 15 nm and 24 nm, respectively. At this time, titanium oxide (TiO 2 ) was deposited at a deposition rate of 5 nm / minute, and silver (Ag) was deposited at a deposition rate of 10 nm / minute.

When the deposition was completed, the inside of the reactor was changed to a vacuum of about 1 × 10 -7 Torr, and argon (10 sccm) was further introduced to adjust the pressure to 1 × 10 -5 Torr. Thereafter, a plasma was formed by applying a power of 5 W / cm 2 of 13.56 MHz radio frequency (RF) to the copper wire wound around the electron beam source. When a plasma was formed in the evaporator, the low-emission substrate was subjected to surface treatment for about 20 minutes under accelerated energy conditions shown in Table 1 using electrons derived from the formed plasma.

Accelerated energy Example 1 150 eV Example 2 300 eV Example 3 1000 eV

Example  4.

Instead of depositing titanium oxide (TiO 2 ), silver (Ag) and titanium oxide (TiO 2 ) on the transparent glass substrate to have an average thickness of 24 nm, 15 nm and 24 nm, respectively, TiO 2 ) and silver (Ag) were alternately laminated so as to have an average thickness of 24 nm and 15 nm, respectively, in the same manner as in Example 1 except that the number of laminated layers was 5, Thereby obtaining a low-emission substrate.

Comparative Example  One.

A transparent glass substrate (corning 1747) was introduced as a transparent substrate into a dry evaporator and fixed, and the inside of the reactor was converted to a vacuum of about 1 x 10 -7 Torr. When the pressure condition of the evaporator is satisfied, argon (10 sccm) is injected into the evaporator so as to maintain it at 1 × 10 -3 Torr, and the sputtering gun installed in the evaporator is supplied with 50 W power of 13.56 MHz radio frequency To form a plasma. Thereafter, titanium oxide (TiO 2 ), silver (Ag) and titanium oxide (TiO 2 ) were deposited on the transparent glass substrate by RF / DC sputtering so as to have an average thickness of 24 nm, 15 nm and 24 nm, An emissive substrate was prepared. At this time, titanium oxide (TiO 2 ) was deposited at a deposition rate of 5 nm / minute, and silver (Ag) was deposited at a deposition rate of 10 nm / minute.

Comparative Example  2.

A low-emission substrate was prepared in the same manner as in Example 1, except that the electron beam was surface-treated at an acceleration energy of 5100 eV instead of being subjected to an acceleration energy of 150 eV.

Experimental Example  One.

The following experiment was conducted to evaluate the shape of the infrared reflecting layer of the low-emission substrate according to the present invention.

X-ray diffraction analysis was performed on the low-emission substrates obtained in Examples 1 to 3 and Comparative Examples 1 and 2. Here, the X-ray diffraction was measured using an ultra-X (CuKa radiation, 40 kV, 120 mA) of Rigaku Corporation (Japan), a wavelength of 1.5406 Å at 2 θ was injected at a rate of 0.02 ° / sec 20- X-ray diffraction pattern was obtained in the range of 80 °.

Measurements, embodiments that radiation substrate obtained in 1 to 3 in 2θ representing the crystallinity of the titanium oxide constituting the diffraction peak with the dielectric layer of 38 ° is represented by 2θ representing the crystallinity of the (Ag) (TiO 2) It was confirmed that there were 25 ° and 49 ° diffraction peaks to be displayed. Also, the intensity of the diffraction peaks was stronger as the average acceleration energy at the surface treatment was larger. On the other hand, in the case of the low-emission base material obtained in Comparative Example 1, the intensity of 38 °, which is represented by 2θ indicating the crystallinity of (Ag), was confirmed to be insignificant, but the peak indicating the crystallinity of titanium oxide (TiO 2 ) was not observed. In addition, in the low-emission substrate of Comparative Example 2, which was surface-treated with a high average acceleration energy, the second dielectric layer and the infrared reflection layer were melted, and the crystalline diffraction peaks of titanium oxide as the second dielectric layer and silver as the infrared reflection layer were not confirmed. This means that when the low-emission substrate is surface-treated with an electron beam derived from a plasma, the amorphous-type infrared reflective layer is transformed into a crystalline infrared reflective layer without deformation of the dielectric layer on the surface. From these results, it can be seen that the low-emission substrate according to the present invention includes a crystalline infrared reflecting layer.

Experimental Example  2.

The following experiments were conducted to evaluate the transmittance of the low-emission substrate according to the present invention to visible light and the degree of reflection to infrared rays.

The low transmittance substrate obtained in Example 2 and Comparative Example 1 was measured for light transmittance and light reflectance in a wavelength range of 200 to 2500 nm using an ultraviolet-visible light-infrared spectroscope. The results are shown in Fig.

As shown in FIG. 3, the low-emission substrate according to the present invention shows improved visible light transmittance and infrared reflectance.

Specifically, referring to FIG. 3, the low-emission substrate of Example 2 showed an average transmittance of 80.7% for visible light and an average reflectance of 80.4% for infrared rays. On the other hand, the low-emission substrate of Comparative Example 1 showed an average transmittance of 80.2% for visible light and an average reflectance of 77.5% for infrared light. This means that the low-emission substrate including the crystalline infrared reflecting layer and the dielectric layer is improved in both transmittance to visible light and reflectance to infrared light compared to a low-emission substrate having a low crystallinity and including an infrared reflective layer and an amorphous dielectric layer . It is also seen that, in electron beam surface treatment, the larger the acceleration energy of the electron beam is, the more the visible light transmittance and the infrared reflectance are improved.

From these results, it can be seen that the low-emission substrate according to the present invention is surface-treated with an electron beam derived from a plasma to increase the crystallinity of the infrared reflective layer without deformation of the dielectric layer and crystallize the component of the dielectric layer, whereby the transmittance to visible light and the reflectance to infrared It can be seen that it is improved.

10: transparent substrate 40: second dielectric layer
20: first reflection reflective layer 50: metal layer
30: Infrared reflection layer 60: Third dielectric layer

Claims (15)

Transparent substrate,
A first dielectric layer provided on the transparent substrate,
An infrared reflecting layer provided on the first dielectric layer,
A second dielectric layer provided on the infrared reflecting layer,
A metal layer provided on the second dielectric, and
And a third dielectric layer provided on the metal layer,
The first to third dielectric layers contain titanium oxide (TiO 2 )
The infrared reflecting layer and the metal layer contain silver (Ag)
In the X-ray diffraction measurement, a low-emission substrate in which diffraction peaks are present at 25 ± 0.5 ° and 49 ± 0.5 °, expressed in 2θ.
delete The method according to claim 1,
The infrared reflecting layer has an average thickness of 10 to 50 nm,
And an average thickness sum of the metal layer and the metal layer is 10 to 50 nm when the metal layer is provided on the second dielectric layer.
The method according to claim 1,
The low emissivity substrate is a low emissivity substrate having an average reflectivity to infrared of 70% or higher.
The method according to claim 1,
The low emissivity substrate is a low emissivity substrate having an average transmittance to visible light of at least 70%.
delete delete delete The method according to claim 1,
The transparent substrate may be a transparent glass substrate or a transparent substrate made of a resin such as a polyester resin, an acetate resin, a polyether sulfone resin, a polycarbonate resin, a polyamide resin, a polyimide resin, a polyacrylic resin, a polyvinyl chloride resin, A transparent resin substrate comprising at least one of a vinylidene resin, a polystyrene resin, a polyvinyl alcohol resin, a polyarylate resin, and a polyphenylene sulfide resin.
Sequentially depositing a first dielectric layer, an infrared reflective layer, a second dielectric layer, a metal layer, and a third dielectric layer on a transparent substrate to produce a low-emission substrate; And
Irradiating an electron beam derived from the plasma to the prepared low-emission substrate surface,
The first to third dielectric layers contain titanium oxide (TiO 2 )
The infrared reflecting layer and the metal layer contain silver (Ag)
Wherein the diffraction peak is present at 25 ± 0.5 ° and 49 ± 0.5 ° represented by 2θ in the X-ray diffraction measurement of the low-emission substrate on which the electron beam is irradiated to the surface.
11. The method of claim 10,
Wherein the plasma is formed at an RF applied power of 1 to 20 W / cm < 2 >.
11. The method of claim 10,
Wherein the average acceleration energy of the electron beam is 50 to 5000 eV.
11. The method of claim 10,
Wherein the step of irradiating the electron beam is performed at a pressure of 1.0 x 10 -4 Torr to 1.0 x 10 -6 Torr.
11. The method of claim 10,
Wherein the step of irradiating the electron beam is performed in an inert gas atmosphere.
15. The method of claim 14,
Wherein the inert gas has an injection amount of 1 to 20 sccm.
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KR20200030343A (en) * 2018-09-12 2020-03-20 (주)엘지하우시스 Functional building material including low-emissivity coat for windows and insulated glazing
KR20200062836A (en) * 2018-11-27 2020-06-04 (주)엘지하우시스 Functional building material including low-emissivity coat for windows and insulated glazing

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KR20200030343A (en) * 2018-09-12 2020-03-20 (주)엘지하우시스 Functional building material including low-emissivity coat for windows and insulated glazing
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