KR102108874B1 - Binder, coating composition for thermal blocking and method for manufacturing the same - Google Patents

Abstract

The present invention relates to a composition for a thermal barrier coating comprising a binder, a chalcogenide nanoparticle and an organic solvent, and a method for manufacturing the same, and the thermal barrier coating composition according to the present invention includes a binder having excellent adhesion to glass. In addition, it has the advantage of excellent thermal barrier effect and mechanical properties, including chalcogenide-based nanoparticles as an infrared blocker.

Description

Binder, thermal barrier coating composition containing the same, and a manufacturing method therefor {BINDER, COATING COMPOSITION FOR THERMAL BLOCKING AND METHOD FOR MANUFACTURING THE SAME}

The present invention relates to a composition for a thermal barrier coating having excellent thermal barrier effect and mechanical properties, including a binder having excellent adhesion to glass, and a chalcogenide nanoparticle as an infrared blocking agent, and a method for manufacturing the same.

As global warming progresses rapidly, the influx of ultraviolet rays is recognized as a serious problem due to the destruction of the ozone layer due to the rise in temperature in summer. As the area of glass windows increases significantly, the indoor temperature rises due to the radiant heat in summer and the indoor temperature imbalance depending on the location, and winter heating Problems such as efficiency drop are steadily occurring.

On the other hand, in addition to the frequent occurrence of secondary damage due to infringement of the view area, unsightly appearance, unprotected exposure to harmful ultraviolet rays, and scattering in the event of glass breakage, with a sunshade device (blind, vertical, curtain, etc.) in response to sunlight inflow The energy loss through the glass window exceeds 60%, and in order to reduce the freon gas and carbon dioxide, the importance of energy saving as well as various environmental regulations is emphasized around the world. .

In this regard, existing energy-saving glass is being constructed in buildings by manufacturing Low E-glass. This is a glass coated with a special metal film with high infrared reflectance inside ordinary glass, which reflects infrared rays to minimize the movement of heat inside and outside. This has the disadvantages of high cost and process difficulties such as the pyrrolitic method and the sputtering method.

In order to simplify the problems of the prior art, efforts have been made to simplify the process and reduce costs by enabling direct coating on general glass. However, the coating material that is applied as a thermal barrier for existing windows has a problem in that the adhesion to the glass is weak by using an organic binder, so that the coating film is easily peeled off and the mechanical properties are weak.

The present invention is to solve the problems of the prior art as described above, the object of the present invention includes a binder excellent in adhesion to glass, and includes a chalcogenide nanoparticle as an infrared ray blocking agent, a thermal barrier effect and mechanical properties. It is to provide this excellent thermal barrier coating composition.

Another object of the present invention is to provide a method for preparing a composition for thermal barrier coating as described above.

One aspect of the present invention for achieving the above object relates to a binder prepared by a sol-gel reaction of a compound represented by Structural Formula 1 and a compound represented by Structural Formula 2.

[Structural Formula 1]

In the structural formula 1,

R ¹ are each independently an alkyl group having 1 to 3 carbon atoms,

m is 4,

[Structural Formula 2]

In the structural formula 2,

이고,R ² are each independently an alkyl group having 1 to 3 carbon atoms, or

ego,

이고,R ³ are each independently an alkyl group of 1 to 3, or

ego,

r is an integer from 1 to 3,

, 또는

이고,X is

, or

ego,

s is an integer from 1 to 3,

p is an integer from 1 to 3,

q is an integer from 1 to 3,

p + q is 4.

Another aspect of the present invention is a binder as described above; Chalcogenide nanoparticles; And organic solvent; relates to a composition for a thermal barrier coating comprising a.

The composition for thermal barrier coating according to an embodiment of the present invention may include 1 to 20 parts by weight of a chalcogenide nanoparticle compound and 30 to 500 parts by weight of an organic solvent based on 100 parts by weight of a binder.

In addition, the compound represented by the structural formula 2 is methyltriethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, diethylylethoxysilane, gamma-aminopropyltri Methoxysilane (γ-Aminopropyltrimethoxysilane), gamma-glycidyloxypropyltrimethoxysilane, aminoethyl-gamma-aminopropyltrimethoxysilane and γ-glycidoxysilane It may include one or more selected from the group consisting of propyl trimethoxysilane (γ-Glycidoxypropyltrimethoxysilane).

In addition, the molar ratio of the compound represented by the structural formula 1: the compound represented by the structural formula 2 may be 1: 0.5 to 1:10.

In addition, the sol-gel reaction can be carried out under an acid catalyst.

In addition, the chalcogenide nanoparticles are Cu _2-x S _y (0 <x <2, 0 <y <2), Cu _2-x Se _y (0 <x <2, 0 <y <2), Cu _2-x Te _y (0 <x <2, 0 <y <2) may include one or more selected from the group consisting of.

In addition, the chalcogenide nanoparticles may be CuS.

In addition, the average diameter of the chalcogenide nanoparticles may be 1 to 200 nm.

Further, the chalcogenide-based nanoparticles may absorb infrared rays.

In addition, the composition for thermal barrier coating may further include a dispersant.

In addition, the composition for thermal barrier coating may further include a sunscreen.

In addition, the sunscreen may include one or more selected from the group consisting of hydroxyphenyl-benzotriazole and hydroxy-phenyl-triazine derivative.

Another aspect of the invention, glass; And a thermal barrier layer formed on the glass, and comprising a binder and chalcogenide nanoparticles. A sol-gel compound containing the compound represented by Structural Formula 1 and a compound represented by Structural Formula 2 is included. It relates to a heat shield glass produced by reacting.

[Structural Formula 1]

In the structural formula 1,

R ¹ are each independently an alkyl group having 1 to 3 carbon atoms,

m is 4,

[Structural Formula 2]

In the structural formula 2,

이고,R ² are each independently an alkyl group having 1 to 3 carbon atoms, or

ego,

이고,R ³ are each independently an alkyl group of 1 to 3, or

ego,

r is an integer from 1 to 3,

, 또는

이고,X is

, or

ego,

s is an integer from 1 to 3,

p is an integer from 1 to 3,

q is an integer from 1 to 3,

p + q is 4.

Another aspect of the invention, (a) preparing a binder; (b) preparing a dispersion liquid containing a chalcogenide-based nanoparticle compound; And (c) mixing the binder and the dispersion; relates to a method for producing a thermal barrier coating composition comprising a.

In the method of preparing a composition for thermal barrier coating according to an embodiment of the present invention, the step (a) is a step of mixing the compound represented by Structural Formula 1 and the compound represented by Structural Formula 2 into an organic solvent and the mixed solution. It may be to include a step of sol-gel reaction.

[Structural Formula 1]

In the structural formula 1,

R ¹ are each independently an alkyl group having 1 to 3 carbon atoms,

m is 4,

[Structural Formula 2]

In the structural formula 2,

이고,R ² are each independently an alkyl group having 1 to 3 carbon atoms, or

ego,

이고,R ³ are each independently an alkyl group of 1 to 3, or

ego,

r is an integer from 1 to 3,

, 또는

이고,X is

, or

ego,

s is an integer from 1 to 3,

p is an integer from 1 to 3,

q is an integer from 1 to 3,

p + q is 4.

 In addition, step (b) may include ball milling by introducing chalcogenide-based nanoparticles into an organic solvent.

The composition for thermal barrier coating according to the present invention can be directly coated on transparent glass, and can be applied to thermal barrier glass by absorbing near infrared rays, and also has a high transmittance of 60% or more even in the transmittance of visible light.

In particular, it has an effect of improving performance such as adhesion, mechanical properties, transparency, and moisture resistance as compared with a coating material to which an existing organic binder is applied.

1A is a photograph of a glass specimen prepared according to Example 2-2, and FIG. 1B is a photograph of a glass specimen prepared according to Comparative Example 2-1.
2A is a photograph of a thermal barrier glass specimen prepared according to Example 4-1, and FIG. 2B is a photograph of a thermal barrier glass specimen prepared according to Comparative Example 4-2.
3 is a graph showing the results of measuring the transmission spectrum of a thermal barrier glass specimen prepared according to Example 4-1.

The present invention can be applied to a variety of transformations and can have various embodiments, and specific embodiments will be illustrated and described in detail in the detailed description. However, this is not intended to limit the present invention to specific embodiments, and should be understood to include all conversions, equivalents, and substitutes included in the spirit and scope of the present invention. In the description of the present invention, when it is determined that detailed descriptions of related well-known technologies may obscure the subject matter of the present invention, detailed descriptions thereof will be omitted.

Further, terms including ordinal numbers such as first and second to be used below may be used to describe various components, but the components are not limited by the terms. The terms are used only for the purpose of distinguishing one component from other components. For example, the first component may be referred to as a second component without departing from the scope of the present invention, and similarly, the second component may be referred to as a first component.

Also, when it is stated that a component is "on another component", "formed on another component" or "laid on another component", it is directly applied to the front or one side of the surface of the other component. It may be attached or formed or laminated, but it should be understood that other components may be further present in the middle.

Singular expressions include plural expressions unless the context clearly indicates otherwise. In this application, terms such as “include” or “have” are intended to indicate that a feature, number, step, operation, component, part, or combination thereof described in the specification exists, one or more other features. It should be understood that the existence or addition possibilities of fields or numbers, steps, operations, components, parts or combinations thereof are not excluded in advance.

Hereinafter, the present invention will be described in detail. However, this is presented as an example, and the present invention is not limited thereby, and the present invention is only defined by the scope of claims to be described later.

One aspect of the present invention relates to a binder prepared by a sol-gel reaction of a compound represented by Structural Formula 1 and a compound represented by Structural Formula 2.

[Structural Formula 1]

In the structural formula 1,

R ¹ are each independently an alkyl group having 1 to 3 carbon atoms,

m is 4,

[Structural Formula 2]

In the structural formula 2,

이고,R ² are each independently an alkyl group having 1 to 3 carbon atoms, or

ego,

이고,R ³ are each independently an alkyl group of 1 to 3, or

ego,

r is an integer from 1 to 3,

, 또는

이고,X is

, or

ego,

s is an integer from 1 to 3,

p is an integer from 1 to 3,

q is an integer from 1 to 3,

p + q is 4.

Another aspect of the present invention is a binder as described above; Chalcogenide nanoparticles; And organic solvent; relates to a composition for a thermal barrier coating comprising a.

The composition for thermal barrier coating according to an embodiment of the present invention may include 1 to 20 parts by weight of a chalcogenide nanoparticle compound and 30 to 500 parts by weight of an organic solvent based on 100 parts by weight of a binder.

In addition, the compound represented by the structural formula 2 is methyltriethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, diethylylethoxysilane, gamma-aminopropyltri Methoxysilane (γ-Aminopropyltrimethoxysilane), gamma-glycidyloxypropyltrimethoxysilane, aminoethyl-gamma-aminopropyltrimethoxysilane and γ-glycidoxysilane It may include one or more selected from the group consisting of propyl trimethoxysilane (γ-Glycidoxypropyltrimethoxysilane).

In the present invention, the molar ratio of the compound represented by the structural formula 1: the compound represented by the structural formula 2 is preferably 1: 0.5 to 1:10. When the molar ratio of the compound represented by Structural Formula 1: Compound 2 represented by Structural Formula 2 is less than 1: 0.5, the functional group is relatively short, and the hardening shrinkage occurs strongly during condensation due to the hydrolysis reaction of many compounds, resulting in a harder coating film but a thickness of 1 μm or more. When the coating layer is broken, it is not desirable, and when it exceeds 1:10, the coating layer can be thickened, but instead of having a long functional group or a small number, it has the properties of an organic binder, resulting in low mechanical properties, which is undesirable.

In the present invention, when the base catalyst is applied during the sol-gel reaction, it is preferable to perform the sol-gel reaction under an acid catalyst, because silica particles are generated by hydrolysis and condensation reaction.

In general, a sol-gel reaction means a method of manufacturing glass or ceramic at a relatively low temperature using hydrolysis and condensation reaction of metal alkoxide, M (OR) n.

Here, the sol refers to a state in which solid particles are dispersed in a colloidal form in a liquid phase, and in particular, the size of the solid particles is very small (a few nm to hundreds of nm), so that brown motion can be performed with little influence of gravity. , Gel refers to a state in which the components of the sol form a network or a polymer chain connected to each other by specific chemical and physical bonds, thereby losing fluidity. In the gel state, this includes cases where the solid phase forms a network and the liquid phase adheres to the network.

The sol-gel reaction is a technique that can be adjusted to realize specific physical properties at all stages from sol to gelation, and can be referred to as a method of manufacturing a material through formation of sol, gelation, and removal of solvent. In the gel state, the formed network or polymer chain has the same refractive index as the surrounding sol, and thus is observed as a transparent state.If the concentration of the particles is much higher than the surrounding sol, the refractive index and density increase, which makes it possible to observe the naked eye. The case is defined as precipitation.

Since the sol-gel reaction can start the state of a reactant in a liquid phase, reaction control is easy, chemical uniformity can be maintained, and various types of final products can be produced. The most commonly used metal alkoxides are alkoxysilanes, which are relatively easy to control reactions compared to other metal alkoxides.

In general, since alkoxysilanes are not soluble in water, an organic solvent is used as a cosolvent, and in solution, an oligomeric precursor sol is subjected to hydrolysis and condensation reaction of a metal alkoxide as shown in the following reaction formula. After formation, a sol-gel reaction that becomes a gel of a three-dimensional network structure is caused by an additional condensation reaction.

Hydrolysis:

≡Si-OR + H ₂ O → ≡Si-OH + ROH

Condensation reaction:

≡Si-OH + ≡Si-OH → ≡Si-O-Si≡ + H ₂ O

≡Si-OH + ≡Si-OR → ≡Si-O-Si≡ + ROH

The particles grow in the solution to form the initial sol phase, and then transfer to the gel phase through growth and connection. Gel properties are greatly affected by the initial growth pattern of the particles. Therefore, it can be said that controlling the growth method of these particles is the core technology of the sol-gel process.

When the particles in the solution are connected while forming a metal-oxygen bond by hydrolysis and condensation reaction to form a three-dimensional network structure, the viscosity of the solution rises rapidly and loses fluidity as it passes through the gel point. . This process is called gelation. The phenomenon in which the monomers dissolved in the connected parts of the gel on the gel thus formed grows and thickens is called necking and this process is called aging. Until this process, there is a solvent introduced at the beginning of the reaction. In order to prepare the product as a useful product, a process of removing these solvents is necessary.

When comparing the classic ceramic manufacturing process with the sol-gel process, the sol-gel process uses a molecular compound as a starting material, so it is not only easy to control the size of the intermediate product, but also the shape of the final product. Powder, particle, fiber, thin film, monolith, composite, etc. can be manufactured in various ways.

The fields of application of these new materials include various optical coating fields, protective coating fields, functional films, structural materials, and component materials. Among them, the areas of greatest interest are coating fields that can provide various functions.

In the present invention, the chalcogenide nanoparticles are Cu _2-x S _y (0 <x <2, 0 <y <2), Cu _2-x Se _y (0 <x <2, 0 <y < 2), Cu _2-x Te _y (0 <x <2, 0 <y <2) may include one or more selected from the group consisting of. At this time, the chalcogenide nanoparticles may be preferably CuS.

In the present invention, the average diameter of the chalcogenide-based nanoparticles may be preferably 1 to 200 nm. At this time, the chalcogenide nanoparticles may be uniformly distributed in the binder.

Since the chalcogenide nanoparticles according to the present invention absorb infrared rays and have thermal barrier properties, the coating composition of the present invention including this can be applied to energy-saving glass.

In the present invention, as the organic solvent, alcohols such as methanol, ethanol, isopropanol, butanol, octanol, methyl ethyl ketone, methyl isobutyl ketone, ketones such as cyclohexanone, acetone, diacetone alcohol, ethylene glycol mono Polyhydric alcohols such as methyl ether and diethylene glycol monobutyl ether, ethers, methyl acetate, ethyl acetate, propylene glycol monomethyl ether acetate, esters such as propylene glycol monoethyl ether acetate, aromatics such as benzene, toluene, and xylene One or more substances selected from hydrocarbons, dimethylformamide, dimethylacetamide and N-methylpyrrolidone may be appropriately mixed according to the solubility, viscosity and coating conditions of the composition.

The composition for thermal barrier coating according to the present invention may further include a dispersant for improving the acidity of the chalcogenide-based nanoparticles.

In addition, the composition for thermal barrier coating according to the present invention may further include a sunscreen. At this time, as the sunscreen, one or more selected from the group consisting of hydroxyphenyl-benzotriazole and hydroxy-phenyl-triazine derivative may be used.

Another aspect of the present invention, (a) preparing a binder, (b) preparing a dispersion comprising a chalcogenide-based nanoparticle compound, and (c) mixing the binder and dispersion. It relates to a method for producing a composition for a thermal barrier coating comprising.

In the production method according to the present invention, the step (a) comprises a step of mixing the compound represented by structural formula 1 and the compound represented by structural formula 2 in an organic solvent and reacting the mixed solution with a sol-gel reaction. Can be.

[Structural Formula 1]

In the structural formula 1,

R ¹ are each independently an alkyl group having 1 to 3 carbon atoms,

m is 4,

[Structural Formula 2]

In the structural formula 2,

이고,R ² are each independently an alkyl group having 1 to 3 carbon atoms, or

ego,

이고,R ³ are each independently an alkyl group of 1 to 3, or

ego,

r is an integer from 1 to 3,

, 또는

이고,X is

, or

ego,

s is an integer from 1 to 3,

p is an integer from 1 to 3,

q is an integer from 1 to 3,

p + q is 4.

At this time, the sol-gel reaction may be preferably performed under an acid catalyst.

In the method of preparing the composition for thermal barrier coating according to the present invention, the step (b) may include ball milling by introducing chalcogenide nanoparticles into an organic solvent. At this time, it is preferable to additionally add a dispersant to improve the dispersibility of the chalcogenide-based nanoparticles.

Hereinafter, the present invention will be described in more detail with reference to examples. However, this is for illustrative purposes, and the scope of the present invention is not limited thereby.

[Example]

Example 1: Binder synthesis

Example 1-1: Synthesis of Binder 1

In a round flask, 50% by weight of TEOS: VTMOS (Vinyltrimethoxysilane) was added at a molar ratio of 1: 1 and 50% by weight of an ethanol solvent, and the mixture was stirred at room temperature for about 1 hour. .

Subsequently, acid catalyst acetic acid was added and the sol-gel reaction was performed at a temperature of 60-70 for 5 hours. After completion of the reaction, filtering with # 300 mesh yielded a binder.

Example 1-2: Synthesis of Binder 2

Binder 2 was synthesized in the same manner as in Example 1-1, except that the molar ratio of TEOS: VTMOS was 1: 5 instead of 1: 1.

Example 1-3: Synthesis of Binder 3

Binder 3 was synthesized in the same manner as in Example 1-1, except that the molar ratio of TEOS: VTMOS was 1:10 instead of 1: 1.

Comparative Example 1-1: Synthesis of Binder 4

Binder 4 was synthesized in the same manner as in Example 1-1, except that only TEOS was used instead of mixing TEOS and VTMOS.

Comparative Example 1-1: Synthesis of organic binder

20% by weight of acrylate monomer Dipentaerythritol Hexaacrylate (DPHA), 5% by weight of Trimethylopropane Triactylate (TMPTA), 5% by weight of Tripropylene Glycol Diacrylate (TPGDA), 10% by weight of HDDA (1,6-Hexanediol Diacrylate), Igarcure 184 (photoinitiator Igarcure 184 ( Basf) 5% by weight, 30% by weight of methyl ethyl keton (MEK), 10% by weight of Propylene Glycol Monomethyl Ether (PGME), 15% by weight of butyl acetate (BA) It was placed in a beaker and mixed using a stirrer.

Then, the mixture was filtered with # 300 mesh to obtain an organic binder.

Example 2: Preparation of a glass specimen coated with a binder

Example 2-1: Preparation of glass specimen coated with binder 1

The binder 1 synthesized as in Example 1-1 was coated with # 10 bar (Mayer Bar) on a glass substrate using a bar coater, and then cured in a convention oven of 150 for 30 minutes to obtain a coating layer.

Example 2-2: Preparation of glass specimen coated with binder 2

A glass specimen coated with binder 2 was prepared in the same manner as in Example 2-1, except that binder 2 was used instead of binder 1.

Example 2-3: Preparation of glass specimen coated with binder 3

A glass specimen coated with binder 3 was prepared in the same manner as in Example 2-1, except that binder 3 was used instead of binder 1.

Comparative Example 2-1: Preparation of glass specimen coated with binder 4

A glass specimen coated with binder 3 was prepared in the same manner as in Example 2-1, except that binder 4 was used instead of binder 1.

Comparative Example 2-1: Preparation of glass specimen coated with an organic binder

The obtained organic-based binder synthesized as Comparative Example 1 was coated with a # 10 bar (Mayer Bar) on a glass substrate using a Bar coater, dried in a Convention oven of 80 for 2 minutes, and then 400 mJ / cm2 using a mercury lamp. The surface was cured with the amount of light to obtain a coating layer.

Example 3: Preparation of a composition for thermal barrier coating

Preparation Example 3-1: Preparation of chalcogenide-based CuS dispersion

A total of 100 g of copper sulfide nanoparticle powder was put into a ball milling device, and methyl ethyl ketone was added as an organic solvent to make 30% by weight of solid content to the ball milling device, and Disperbyk 161 (Disperbyk 161) (manufactured by BK Korea) ) Was added so that 5% by weight compared to the powder, and ball milling was performed for 192 hours using 0.1 mm zirconia beads (balls).

The rotational speed of the ball milling device was set to about 300 rpm. Through this method, a dispersion of copper sulfide nanoparticles was prepared, and as a result of measuring the particle size through a nanoparticle analyzer (Zetasizer Nano ZS90), it was confirmed that the primary particle size ranged from 10 to 100 nm.

Example 3-1: Preparation of composition for thermal barrier coating

The binder prepared in Example 1-2 and the CuS dispersion prepared in Preparation Example 3-1 were mixed so that the weight ratio of the binder and the dispersion was 10: 1, put into a beaker, and then used a stirrer at a rate of 300 rpm. The composition for thermal barrier coating with infrared ray blocking function was prepared by sufficiently stirring for a minute.

Comparative Production Example 3-1: Preparation of ATO (Antimony tin oxide) dispersion

An ATO dispersion was prepared in the same manner as in Preparation Example 3-1, except that ATO powder was used instead of copper sulfide nanoparticle powder.

Comparative Example 3-1: Preparation of composition for thermal barrier coating

It was carried out in the same manner as in Example 2, except that the ATO dispersion of Comparative Preparation Example 3-1 was used instead of using the CuS dispersion of Preparation Example 3-1.

Comparative Example 3-2: Preparation of thermal barrier coating composition

It was carried out in the same manner as in Example 3-1, except that the organic binder of Comparative Example 1-1 was used instead of the binder of Example 1-2.

Example 4: Preparation of thermal barrier glass

Example 4-1: Preparation of thermal barrier glass

The composition for thermal barrier coating prepared according to Example 3-1 was coated with # 10 bar (Mayer Bar) on a glass substrate using a bar coater, and then cured for 30 minutes in a convention oven of 150 to prepare a thermal barrier glass. .

Comparative Example 4-1: Preparation of thermal barrier glass

It was carried out in the same manner as in Example 3-1, except that the composition for thermal barrier coating of Comparative Example 3-1 was used instead of the composition for thermal barrier coating of Example 3-1.

Comparative Example 4-2: Preparation of thermal barrier glass

It was carried out in the same manner as in Example 3, except that the composition for thermal barrier coating of Comparative Example 3-2 was used instead of the composition for thermal barrier coating of Example 3-1.

Test Example 1: Evaluation of the physical properties of the binder

The transmittance, Haze, adhesion, pencil hardness and QUV durability of the glass specimens prepared according to Examples 2-1 to 2-3, Comparative Examples 1-1 and Comparative Examples 1-1 were measured and shown in [Table 1] below. Did.

[How to measure]

-Transmittance: Through the UV-Vis-NIR spectrophotometer, the transmittance of the UV, visible, and near infrared regions of the coated specimen can be measured. The visible light transmittance represents a wavelength range in the range of 380-780 nm, and an average value of the transmittance was obtained.

-Haze: The haze value was confirmed using a Haze Meter (model name NHD-200, manufacturer Nippon Denshoku Kogyo Co.).

-Adhesion: 100 squares of 1mm X 1mm size are formed using a cross-cutter on the cured coating on glass. Then, after attaching a standard (3M) tape on 100 squares and attempting to peel the film, check if there are 100 sauare and count the number of remaining cells.

-Pencil hardness: Mitsubishi pencil (UNI) for pencil evaluation using a pencil hardness tester 7.5N, 10mm at a rate of 0.5mm / sec 5 times, and then the number of wounds was checked.

-QUV Durability: As an accelerated weathering test evaluation, a change in color and characteristics was confirmed by repeating the coating sample using an ultraviolet lamp.

Example 2-1 Example 2-2 Example 2-3 Comparative Example 2-1 Comparative Example 2-1 Transmittance (%) 84.43 92.94 91.23 86.58 91.94 Haze (%) 2.63 0.35 0.58 53.82 0.42 Adhesion 100/100 100/100 95/100 80/100 5/100 Pencil hardness 9H 9H 8H 7H 6H QUV durability Good Good NG Good NG

As can be seen from [Table 1], it can be seen that the binder according to the present invention has improved mechanical properties such as adhesion and pencil hardness compared to a conventional organic binder.

Meanwhile, FIG. 1A is a photograph of a glass specimen prepared according to Example 2-2, and FIG. 1B is a photograph of a glass specimen prepared according to Comparative Example 2-1. Referring to Figures 1a and 1b, it can be seen that the binder according to the present invention does not crack when coated with a thickness of about 5 μm or more on the coated glass substrate through an appropriate condensation reaction and has good appearance.

Test Example 2: Measurement of the transmittance of the heat absorption dispersion

The transmittance up to 380-1400 nm for the heat absorbing dispersion prepared according to Preparation Example 3-1 and Comparative Preparation Example 3-1 was measured and shown in Table 2 below.

[How to measure]

-Visible light transmittance: UV-Vis-NIR spectrophotometer can be used to measure the transmittance of ultraviolet, visible, and near-infrared regions of coated specimens. The visible light transmittance represents a wavelength range in the range of 380-780 nm, and an average value of the transmittance was obtained.

-Near-infrared blocking rate: UV-Vis-NIR spectrophotometer can measure the transmittance of UV, visible and near-infrared regions of coated specimens. The near-infrared transmittance indicates a wavelength range in the range of 780-1400nm, and the near-infrared cutoff rate was determined as "100 (%)-average of transmittance".

Preparation Example 3-1 Comparative Production Example 3-1 Visible light transmittance (%) 59.54 60.17 Near infrared ray blocking rate (%) 80.92 76.58

As can be seen from [Table 2], it was confirmed that the heat absorption dispersion liquid containing the chalcogenide nanoparticles according to the present invention is superior to the transmittance of the visible light region compared to the conventional heat absorption dispersion liquid, and the blocking rate of the near infrared region is excellent. Can be.

Test Example 3: Evaluation of physical properties of thermal barrier glass

The transmittance, haze, adhesion, pencil hardness and QUV durability of the thermal barrier glass coating layers prepared according to Example 4-1, Comparative Example 4-1 and Comparative Example 4-2 were measured and are shown in Table 3 below.

Example 4-1 Comparative Example 4-1 Comparative Example 4-2 Visible light transmittance (%) 63 65 64 Near infrared ray blocking rate (%) 70 67 72 Haze (%) 0.42 0.35 0.53 Adhesion 100/100 100/100 10/100 QUV durability Good Good NG

As can be seen from [Table 3], in the case of the thermal barrier glass coated with the composition for thermal barrier coating according to the present invention, the adhesion between the substrate and the coating layer is superior to the thermal barrier glass coated with the conventional organic binder composition. It can be confirmed that the QUV durability is excellent.

In addition, FIG. 2A is a photograph of a thermal barrier glass specimen prepared according to Example 4-1, and FIG. 2B is a photograph of a thermal barrier glass specimen prepared according to Comparative Example 4-2. In the case of Comparative Example 4-2, all of the coating layers were separated when the adhesion was evaluated, but in Example 4-1, the adhesion was good.

In addition, Figure 3 is a graph showing the result of measuring the transmission spectrum of ultraviolet, visible, and infrared regions of the thermal barrier glass specimen according to Example 4-1. As can be seen in Figure 3, the composition for thermal barrier coating according to the present invention shows that the transmittance in the visible region is excellent and the transmittance in the infrared region is low, so that heat in the infrared region is absorbed.

Although preferred embodiments of the present invention have been described above, those skilled in the art can add, change, delete, or delete components without departing from the spirit of the present invention as set forth in the claims. The present invention may be variously modified and changed by addition, etc., and it will be said that it is also included within the scope of the present invention. For example, each component described as a single type may be implemented in a distributed manner, and similarly, components described as distributed may be implemented in a combined form. The scope of the present invention is indicated by the following claims rather than the above detailed description, and it should be interpreted that all changes or modified forms derived from the meaning and scope of the claims and equivalent concepts thereof are included in the scope of the present invention. do.

Claims (17)

bookbinder;
Chalcogenide nanoparticles; And
It includes; a first organic solvent;
The binder is prepared by a sol-gel reaction of a compound represented by Structural Formula 1 and a compound represented by Structural Formula 2,
The composition for thermal barrier coating wherein the first organic solvent comprises methyl ethyl ketone:
[Structural Formula 1]

In the structural formula 1,
R ¹ are each independently an alkyl group having 1 to 3 carbon atoms,
m is 4,
[Structural Formula 2]

In the structural formula 2,
R ² is

ego,
R ³ are each independently an alkyl group of 1 to 3,
p is 1,
q is 3. delete According to claim 1,
The composition for thermal barrier coating, characterized in that 1 to 20 parts by weight of the chalcogenide nanoparticles and 30 to 500 parts by weight of the organic solvent with respect to 100 parts by weight of the binder. According to claim 1,
A composition for thermal barrier coating, characterized in that the compound represented by Structural Formula 2 includes Vinyltrimethoxysilane. According to claim 1,
A composition for thermal barrier coating, characterized in that the molar ratio of the compound represented by the structural formula 1: the compound represented by the structural formula 2 is 1: 0.5 to 1:10. According to claim 1,
The composition for thermal barrier coating, characterized in that the sol-gel reaction is carried out under an acid catalyst. According to claim 1,
The chalcogenide nanoparticles are Cu _2-x S _y (0 <x <2, 0 <y <2), Cu _2-x Se _y (0 <x <2, 0 <y <2), Cu _{2 -x} Te _y (0 <x <2, 0 <y <2) composition for thermal barrier coating, characterized in that it comprises at least one selected from the group consisting of. The method of claim 7,
A composition for thermal barrier coating, characterized in that the chalcogenide nanoparticles are CuS. The method of claim 8,
The composition for thermal barrier coating, characterized in that the average diameter of the chalcogenide nanoparticles is 1 ~ 200nm. According to claim 1,
The composition for thermal barrier coating, characterized in that the chalcogenide nanoparticles absorb infrared rays. According to claim 1,
The composition for thermal barrier coating, characterized in that the composition for thermal barrier coating further comprises a dispersant. According to claim 1,
The composition for thermal barrier coating, characterized in that the composition for thermal barrier coating further comprises a sunscreen. The method of claim 12,
The sunscreen is a thermal barrier, characterized in that it comprises at least one selected from the group consisting of hydroxyphenyl-benzotriazole and hydroxy-phenyl-triazine derivatives. Coating composition. Glass; And
Formed on the glass, a thermal barrier layer comprising a binder and chalcogenide nanoparticles; includes,
The binder is prepared by a sol-gel reaction of a compound represented by Structural Formula 1 and a compound represented by Structural Formula 2,
The thermal barrier layer is a thermal barrier glass prepared by curing the composition for thermal barrier coating of claim 1:
[Structural Formula 1]

In the structural formula 1,
R ¹ are each independently an alkyl group having 1 to 3 carbon atoms,
m is 4,
[Structural Formula 2]

In the structural formula 2,
R ² is

ego,
R ³ are each independently an alkyl group of 1 to 3,
p is 1,
q is 3. (a) preparing a binder;
(b) preparing a dispersion liquid containing chalcogenide nanoparticles; And
(c) mixing the binder and the dispersion; includes,
The step (a) of the compound represented by the formula (1) and the compound represented by the formula (2) in a second organic solvent and the compound represented by the formula (1) and the compound represented by the formula (2) sol-gel reaction Including,
The step (b) is a method for producing a thermal barrier coating composition comprising the step of ball milling by introducing the chalcogenide-based nanoparticles into a first organic solvent containing methyl ethyl ketone:
[Structural Formula 1]

In the structural formula 1,
R ¹ are each independently an alkyl group having 1 to 3 carbon atoms,
m is 4,
[Structural Formula 2]

In the structural formula 2,
R ² is

ego,
R ³ are each independently an alkyl group of 1 to 3,
p is 1,
q is 3. delete delete

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