KR101182194B1 - Method for manufacturing infrared ray absorption inorganic compound - Google Patents

Abstract

PURPOSE: A manufacturing method of an infrared ray-absorbing inorganic compound is provided to manufacture high infrared ray-shielding rate and invisible ray transmittance without discoloration due to solar light or ultraviolet rays. CONSTITUTION: A manufacturing method of an infrared ray-absorbing inorganic compound comprises a metal salt dissolution step(S1) forming an alcohol mixture solution by adding a first and a second metal salt to an alcohol solvent, an anti-agglomeration dissolving step(S2) forming an anti-agglomeration agent mixture by adding an anti-agglomeration agent into the alcohol mixture; a water mixing step(S3) forming a water mixture solution by adding water into the anti-agglomeration agent mixture; an inorganic compound synthesizing step manufacturing an inorganic compound by heating the water mixture solution by microwaves; a crystallization step(S5) forming a crystallized inorganic compound by heat-treating the inorganic compound.

Description

Method for manufacturing infrared ray absorption inorganic compound

The present invention relates to an infrared absorbing inorganic compound, a method for producing the same, and a product using the same. More specifically, a metal salt dissolving step of forming an alcohol mixed solution by adding a first metal salt and a second metal salt to an alcohol solvent, and the metal salt dissolving step. The water mixing step of forming a water mixed solution by adding water to the anticoagulant dissolving step of forming an anticoagulant mixed solution by adding an anticoagulant to the alcohol mixture solution formed in the above and the anticoagulant mixed solution formed in the anticoagulant dissolving step; Including an inorganic compound synthesis step of producing an inorganic compound by heating the water mixture solution formed in the water mixing step by microwave, and a crystallization step of forming a crystallized inorganic compound by heat-treating the inorganic compound prepared in the inorganic compound synthesis step, Discoloration due to sunlight or ultraviolet rays The present invention relates to an infrared absorbing inorganic compound having a high visible light transmittance and an infrared shielding rate, a method for preparing the same, and a product using the same.

In general, inorganic compounds used to block heat have excellent durability and high thermal barrier properties, but their application range is limited due to low visible light transmittance and chromism due to ultraviolet rays. Antimony tin oxide (ATO), indium tin oxide (ITO), tungsten bronze (Tungsten Bronze) and the like are used as the inorganic oxide.

ATO is cheaper than ITO and is often used in thermal barrier films. However, since the infrared blocking property is poor, a large amount of ATO must be used to improve the infrared shielding effect.

ITO shows higher visible light transmittance and infrared ray blocking properties than ATO. However, the indium price is well known as the world's most expensive raw material, and many IT industries are finding a substitute for ITO, and in the case of thermal barrier film production, using such an expensive raw material is very large. There is a burdensome problem.

Tungsten bronze is a tungsten trioxide having a basic structure, and is a wide band gap oxide. It is known that there is little absorption of light in the visible region and no free electrons exist in the structure. Accordingly, a small amount of oxygen is reduced, or a tungsten bronze compound in which a positive element such as Na is added to tungsten trioxide is made, and it is being studied little by little as a material that transmits visible light and shields infrared rays. However, it is not clear in what composition ratio, manufacturing method, etc. that the tungsten bronze compound has visible light transmission and infrared shielding properties, and there is a problem that discoloration occurs in the tungsten bronze compound.

Therefore, the necessity of the material which does not change color even if it is irradiated with sunlight or ultraviolet-ray, and has high visible light transmittance and an infrared shielding rate is increasing.

SUMMARY OF THE INVENTION The present invention has been made to solve the above problems,

SUMMARY OF THE INVENTION An object of the present invention is to provide an infrared absorbing inorganic compound having no discoloration property due to sunlight or ultraviolet rays, and having a high visible light transmittance and an infrared shielding rate, a method of manufacturing the same, and a product using the same.

In addition, the present invention is represented by the formula A _x B _y O _z wherein A is an alkali metal or alkaline earth metal and B is Mg, Mo, V, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni , Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti, Ge, Sn, Pb, W, any one selected from O is oxygen and x, y, z is 0.001≤x / y≤1 In order to provide an infrared absorbing inorganic compound having a range of 3 <z / y≤5, a manufacturing method thereof, and a product using the same.

In addition, an object of the present invention is to provide an infrared absorbing inorganic compound having a uniform particle size of 10 to 50nm, a method for producing the same, and a product using the same.

The present invention also provides an infrared absorbing inorganic compound, a method for producing the same, and a product using the same, which can shorten the manufacturing time by synthesizing a compound using microwaves, have uniform properties, and reduce the use of organic solvents. have.

In addition, an object of the present invention is to provide an infrared absorbing inorganic compound having high visible light transmittance and infrared ray shielding rate without heat discoloration by heat treatment at a constant temperature in an inert gas atmosphere, a manufacturing method thereof, and a product using the same.

In addition, an object of the present invention is to provide an infrared absorbing inorganic compound, a method for manufacturing the same, and a product using the same, which enables the control of light and heat introduced into the interior.

In order to achieve the above object, the present invention is implemented by the following embodiments.

According to an embodiment of the present invention, a method for preparing an infrared absorbing inorganic compound according to the present invention includes: a metal salt dissolving step of forming an alcohol mixed solution by adding a first metal salt and a second metal salt to an alcohol solvent; An anticoagulant dissolving step of forming an anticoagulant mixed solution by adding an anticoagulant to the alcohol mixture solution formed in the metal salt dissolving step; A water mixing step of forming water mixed solution by adding water to the anticoagulant mixed solution formed in the anticoagulant dissolving step; An inorganic compound synthesis step of preparing an inorganic compound by heating the water mixed solution formed in the water mixing step by microwave; And a crystallization step of forming a crystallized inorganic compound by heat-treating the inorganic compound prepared in the synthesis of the inorganic compound.

According to another embodiment of the present invention, in the method for preparing an infrared absorbing inorganic compound according to the present invention, the crystallized inorganic compound is represented by the formula A _x B _y O _z , wherein A is an alkali metal or an alkaline earth metal, B is Mg, Mo, V, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti, Ge, Sn, Any one selected from Pb and W, O is oxygen, x, y, z is characterized by having a range of 0.001≤x / y≤1, 3 <z / y≤5.

According to another embodiment of the present invention, in the method for preparing an infrared absorbing inorganic compound according to the present invention, in the step of synthesizing the inorganic compound, microwaves are irradiated for 100 to 300 seconds so that the heating temperature is 80 to 120 ° C. .

According to another embodiment of the present invention, in the crystallization step of the infrared absorption inorganic compound manufacturing method according to the present invention is characterized in that the heat treatment by irradiating microwaves for 0.5 to 2 hours so that the heating temperature is 400 to 800 ℃. .

According to still another embodiment of the present invention, in the method for preparing an infrared absorbing inorganic compound according to the present invention, the microwave irradiation is performed in an inert gas atmosphere.

According to another embodiment of the present invention, in the method for preparing an infrared absorbing inorganic compound according to the present invention, the first metal salt and the second metal salt are each used in an amount of 0.01 to 0.1 mol based on 1 L of the alcohol solvent. 1 to 20 parts by weight based on 100 parts by weight of the alcohol mixture solution, and 5 to 100 parts by weight based on 100 parts by weight of the anticoagulant mixture solution is used.

According to another embodiment of the present invention, the infrared absorption inorganic compound according to the present invention is represented by the formula A _x B _y O _z , wherein A is an alkali metal or alkaline earth metal, and B is Mg, Mo, V, Zr , Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti, Ge, Sn, Pb, W, O is oxygen, and x, y, and z have a range of 0.001 ≦ x / y ≦ 1 and 3 <z / y ≦ 5.

According to another embodiment of the present invention, the infrared absorption inorganic compound according to the present invention is characterized in that the microwave is used as a heat source is produced.

According to another embodiment of the present invention, in the infrared absorption inorganic compound according to the present invention, the microwave is characterized in that the irradiation temperature for 100 to 300 seconds so that the heating temperature is 80 to 120 ℃.

According to another embodiment of the present invention, the infrared absorption inorganic compound according to the present invention is prepared by crystallizing the inorganic compound by heat treatment, wherein the heat treatment is performed by irradiating microwave at 0.5 to 2 hours at 400 to 800 ℃ temperature It is done.

According to another embodiment of the present invention, in the infrared absorption inorganic compound according to the present invention, the heat treatment is performed in an inert atmosphere.

According to another embodiment of the present invention, it is characterized by a product comprising the infrared shielding inorganic compound of any one of claims 7 to 11 according to the present invention.

According to another embodiment of the present invention, a product containing an infrared absorbing inorganic compound according to the present invention is a film comprising a base layer and an infrared shielding layer formed on one surface of the base layer, the infrared shielding layer is the infrared It is characterized by including a shielding inorganic compound.

 According to another embodiment of the present invention, in the product containing an infrared absorbing inorganic compound according to the present invention, the infrared shielding layer forms a dispersion solution by mixing a dispersant and an organic solvent in the powder of the infrared shielding inorganic compound, A binder and an organic solvent are mixed with the dispersion solution to form a coating solution, and the coating solution is formed by coating one surface of the base layer.

According to another embodiment of the present invention, in the product containing the infrared absorbing inorganic compound according to the present invention, the dispersion solution is 1.5 to 5 parts by weight of the dispersant based on the infrared shielding inorganic compound, 100 parts by weight of the inorganic compound, organic It is characterized by including a solvent 210 to 400 parts by weight.

According to another embodiment of the present invention, in the product containing the infrared absorption inorganic compound according to the present invention, the coating solution is 80 to 125 parts by weight of the binder with respect to the dispersion solution, 100 parts by weight of the dispersion solution, the organic solvent Characterized in that it comprises 20 to 50 parts by weight.

The present invention can obtain the following effects by the above embodiment.

The present invention does not exhibit discoloration by sunlight or ultraviolet rays, and has an effect of providing an infrared absorbing inorganic compound having high visible light transmittance and high infrared shielding rate.

In addition, the present invention is represented by the formula A _x B _y O _z wherein A is an alkali metal or alkaline earth metal and B is Mg, Mo, V, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni , Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti, Ge, Sn, Pb, W, any one selected from O is oxygen and x, y, z is 0.001≤x / y≤1 In addition, there is an effect that can provide an infrared absorption inorganic compound having a range of 3 <z / y ≤ 5.

In addition, the present invention has the effect of providing a uniform infrared absorption inorganic compound having a particle size of 10 ~ 50nm.

In addition, the present invention has the effect of shortening the production time by synthesizing the compound using microwave, has a uniform characteristic and can reduce the use of organic solvents.

In addition, the present invention is effective in providing an infrared absorbing inorganic compound having high visible light transmittance and high infrared shielding rate without heat discoloration by heat treatment at a constant temperature in an inert gas atmosphere.

In addition, the present invention has the effect of providing an infrared absorption inorganic compound to enable the control of light and heat introduced into the interior.

1 is a flow chart of a method for producing an infrared absorbing inorganic compound according to an embodiment of the present invention.
Figure 2 is a SEM photograph of the inorganic compound prepared according to Example 1.
3 is an XRD graph of an inorganic compound prepared according to Example 1;
4 is an XRD graph of an inorganic compound prepared according to Example 6.
Figure 5 is a graph diluting the inorganic compound prepared in Example 1 and showing the UV / Vis / IR spectrum measurement results.
Figure 6 is a graph diluting the inorganic compound prepared in Example 6 and showing the UV / Vis / IR spectrum measurement results.
Figure 7 is a graph diluting the inorganic compound prepared in Comparative Example and showing the UV / Vis / IR spectrum measurement results.

Hereinafter, an infrared absorbing inorganic compound according to the present invention, a method for preparing the same, and a product using the same will be described in detail with reference to the accompanying drawings. Unless defined otherwise, all terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs and, if conflict with the meaning of the terms used herein, It follows the definition used in the specification.

1 is a flow chart of a method for producing an infrared absorbing inorganic compound according to an embodiment of the present invention.

Referring to Figure 1, the method for producing an infrared absorbing inorganic compound according to an embodiment of the present invention is a metal salt dissolving step (S1) to form an alcohol mixed solution by adding a first metal salt and a second metal salt to the alcohol solvent, and Water is added to the anticoagulant dissolving step (S2) and the anticoagulant mixed solution formed in the anticoagulant dissolving step (S2) to form an anticoagulant mixed solution by adding an anticoagulant to the alcohol mixed solution formed in the metal salt dissolving step (S1). Water mixing step (S3) of adding and forming a water mixture solution, inorganic compound synthesis step (S4) of preparing an inorganic compound by heating the water mixture solution formed in the water mixing step (S3) with microwaves, and the inorganic It characterized in that it comprises a crystallization step (S5) of heat-treating the inorganic compound prepared in the compound synthesis step (S4) to form a crystallized inorganic compound.

The inorganic compound obtained through the manufacturing process is represented by the formula A _x B _y O _z , wherein A is an alkali metal or alkaline earth metal and B is Mg, Mo, V, Zr, Cr, Mn, Fe, Ru, Co, Any one selected from Rh, Ir, Ni, Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti, Ge, Sn, Pb, W, O is oxygen, x, y, z is 0.001 It is characterized by having a range of ≤ x / y ≤ 1, 3 <z / y ≤ 5.

The metal salt dissolving step (S1) is a step of forming an alcohol mixture solution by dissolving the first metal salt and the second metal salt in an alcohol solvent by adding a first metal salt and a second metal salt to an alcohol solvent and spraying ultrasonic waves.

The alcohol solvent is an organic solvent containing a hydroxyl group (OH), ethylene glycol (Ethylene glycol (EG)), diethyl glycol (Diethylene glycol (DEG)), triethylene glycol (TEG) and tetraethylene glycol One or a mixture of two or more selected from (Tetraethylene glycol (TTEG)) may be used.

The first metal salt provides A to the inorganic compound prepared by the preparation method, and salts of alkali metals and alkaline earth metals may be used in the form of sulfates, carbonates, nitrates, and the like.

The second metal salt provides B to the inorganic compound prepared by the method, and in the form of sulfate, carbonate, nitrate, etc., Mg, Mo, V, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir Salts including any one of Ni, Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti, Ge, Sn, Pb, and W may be used. As the second metal salt, salts of tungsten, molybdenum and vanadium, which easily change inherent photochemical properties in the infrared region, are preferably used.

The first metal salt and the second metal salt are preferably used in an amount of 0.01 to 0.1 mol based on 1 L of the alcohol solvent. Small amounts of the result are produced when less than 0.01 mol of the first and second metal salts are used, and the first and second metal salts do not react when more than 0.1 mol of the first and second metal salts are used. There is a problem that can occur.

The anticoagulant dissolving step (S2) is a step of forming an anticoagulant mixed solution by adding an anticoagulant to the alcohol mixed solution formed in the metal salt dissolving step (S1) and spraying ultrasonic waves to dissolve the anticoagulant in the alcohol mixed solution. In the process of preparing the inorganic compound, when an alcohol solvent is present alone, aggregation occurs to reduce surface energy together with nucleation and particle generation, so that an aggregation agent is used to prevent aggregation.

The aggregation inhibitor is one or two selected from polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyacrylic acid (PAA), and sodium acetate. Mixtures of the above may be used.

The anti-agglomerating agent is preferably used 1 to 20 parts by weight based on 100 parts by weight of alcohol mixed solution. If the anti-agglomerating agent is used in less than 1 part by weight can not control the growth of the inorganic compound particles, when used in excess of 20 parts by weight there is a problem that it is difficult to remove later.

The water mixing step (S3) is a step of forming a water mixture solution by adding water to the anticoagulant mixture solution formed in the anticoagulant mixing step (S2), the complex compound formed in the anticoagulant mixing step is added by water It is forced to hydrate and change to a hydrate state.

The water is preferably used 5 to 100 parts by weight based on 100 parts by weight of the anticoagulant mixture solution. When less than 5 parts by weight of water is used, complete oxidation is not achieved, resulting in a mixture of forms of metals other than oxides, and when used in excess of 100 parts by weight, the yield of metal oxides may be reduced. There is a problem that can be.

The inorganic compound synthesis step (S4) is a step of preparing an inorganic compound by heating the water mixture solution formed in the water mixing step (S3) with a microwave, in the water mixture solution by the dehydration reaction by the thermal energy of the microwave inorganic The compound is synthesized. Preferably, the temperature of the microwave is adjusted to a heating temperature of 80 to 120 ° C., followed by heating for 100 to 300 seconds to prepare an inorganic compound. If the microwave irradiation time is less than 100 seconds, the unreacted substance may remain because the nucleus is not grown. If the microwave irradiation time is 300 seconds or more, nanoparticles of a desired size cannot be obtained due to an excessive heat source. More preferably, the inorganic compound is prepared by heating for 120 to 180 seconds. The microwave heating is faster than the conventional heating method using a conventional apparatus, the selective heating is carried out by the wave rather than the heat transfer by conduction heat and convection, uniform heating of the entire solution is possible to produce a conventional inorganic compound Compared to the method, it is possible to shorten the production time and synthesize an inorganic compound having uniform properties. In addition, since the amount of the organic solvent can be reduced, the inorganic compound can be environmentally friendly. When irradiated with microwaves in a liquid material with a relatively weak binding force of molecules, the dipoles of the liquid molecules change in polarity according to the frequency of microwaves and rotate or translate rapidly to generate frictional heat between molecules. It is called dielectric heating method. Therefore, in mixtures with high or low dielectric constants, microwaves can selectively penetrate into liquid materials with high dielectric constants and heat them up quickly to the inside of the mixtures. It is possible to reduce the amount of solvent used and to prepare inorganic compounds having uniform properties.

The crystallization step (S5) is a step of crystallizing the inorganic compound prepared in the inorganic compound synthesis step (S4), it is preferable to heat-treated at 400 to 800 ℃ temperature 0.5 to 2 hours by irradiating microwaves in an inert gas atmosphere. Do. The inorganic compound of formula A _x B _y O _z obtained in the synthesis of the inorganic compound (S4) has a characteristic of transmitting visible light but shielding infrared rays by changing the structure and crystallinity of the crystal through the crystallization step (S5). .

Another embodiment of the present invention is represented by the formula A _x B _y O _z prepared by the method for producing an inorganic compound according to an embodiment of the present invention, wherein A is an alkali metal or alkaline earth metal and B is Mg, Mo Selected from V, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti, Ge, Sn, Pb, W Either one, O is oxygen, x, y, z is for the inorganic compound having a range of 0.001≤x / y≤1, 3 <z / y≤5. The particle size of the inorganic compound is characterized in that 10 ~ 50nm. In addition, the inorganic compound has a high transmittance of visible light and an infrared shielding rate, so that light passes but blocks heat, and has a property of not being discolored by sunlight or ultraviolet rays.

Another embodiment of the present invention is directed to a product comprising the inorganic compound. Since the inorganic compound has high visible light transmittance and infrared ray shielding rate, when used in a smart window or a film for smart window, visible light may pass through sunlight in the glass window, but the infrared ray may be shielded to suppress an increase in room temperature. In addition, the inorganic compound may be applied to various fields such as an optical device, an optical switch, a display, a gas sensor, and the like. As an example of the product, a film including the inorganic compound will be described.

The film including the inorganic compound includes a base layer and an infrared shielding layer formed on one surface of the base layer.

The substrate layer is coated with an infrared shielding layer on one surface thereof to support the infrared shielding layer, and as the substrate layer, polyethylene terephthalate, polycarbonate, nylon, polypropylene film, or the like may be used.

The infrared shielding layer is formed on one surface of the base layer to shield the infrared rays to prevent radiant heat from being introduced or emitted, the infrared shielding layer is represented by the formula A _x B _y O _z , wherein A is an alkali metal Or alkaline earth metal and B is Mg, Mo, V, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti , Ge, Sn, Pb, W is any one selected from O is oxygen, x, y, z has a range of 0.001≤x / y≤1, 3 <z / y≤5, particle size of 10 to 50nm It includes an inorganic compound having a.

The infrared shielding layer forms a dispersion solution by mixing the inorganic compound powder, a dispersant, and an organic solvent, and forms a coating solution by mixing a binder and an organic material in the dispersion solution, the coating solution on one side of the base layer Formed by coating.

The dispersion solution is formed to disperse the inorganic compound because it does not exhibit optical properties when the powder of the inorganic compound is agglomerated with each other. The dispersion solution is based on 100 parts by weight of the inorganic compound and the inorganic compound. It is preferable to contain 1.5-5 weight part of dispersing agents, and 210-400 weight part of organic solvents. When the organic solvent is less than 210 parts by weight does not exhibit sufficient optical properties at low thickness when forming the final coating film, when more than 400 parts by weight does not have sufficient storage stability due to high solids, the dispersion solution itself changes due to the time-dependent gelation There is this. When the dispersant is less than 1.5 parts by weight, sufficient dispersing sol may not be obtained, and when the dispersant is 5 parts by weight or more, the dispersant may remain on the surface during secondary processing, resulting in surface defects. The dispersion solution is prepared by a ball mill method. The ball mill method includes a powder and a solvent (organic solvent) to be dispersed in a predetermined container, a dispersant is added thereto, and then zirconium beads are added and turned to turn the powder. The friction or shear stress is applied to disperse or separate the agglomerated powder from the primary particles little by little.

The coating solution is formed to easily coat the dispersion solution on the base layer, and includes 80 to 125 parts by weight of binder and 20 to 50 parts by weight of an organic solvent based on the dispersion solution and 100 parts by weight of the dispersion solution. It is preferable. Less than 80 parts by weight of the binder is used, coating film adhesion and surface scratch resistance is inferior, and when more than 125 parts by weight is used, the ratio of the dispersion solution is lowered, the optical properties are degraded. The binder facilitates bonding with the base layer, and also serves to adjust the thickness of the coating layer. The binder is composed of oligomers and monomers and photoinitiators which cause photopolymerization by UV irradiation as photopolymers. The organic solvent is methyl ethyl ketone, toluene, ethyl acetate, isopropyl alcohol, ethyl cellosolve, isobutyl alcohol, dimethylformide, ethanol, butyl cellosolve, xylene, 1-octanol, diethylene, glycol, nitro One or two or more mixtures selected from banzen may be used.

The infrared shielding layer has a thickness of 3 to 4㎛ preferred for coating the coating solution on one surface of the base layer and irradiated with ultraviolet rays. When the thickness is less than 3㎛ does not express optical properties, there is a disadvantage that the surface scratch resistance is deteriorated, when the thickness is more than 4㎛ because there is a disadvantage that the adhesion with the substrate. The method of coating the coating solution on the base layer may be, for example, microgravure coating, knife coating, roll-to-roll coating, or the like.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, these are intended to describe the present invention in more detail, but the scope of the invention is not limited thereto.

&Lt; Example 1 >

1) After mixing tungsten chloride and cesium chloride in the alcohol solvent ethylene glycol (EG) in a weight ratio of 0.4 to 0.4, dissolve the tungsten chloride and cesium chloride using an ultrasonic device.

2) 5 parts by weight of aggregating agent PVP is added to 100 parts by weight of the alcohol mixture solution and mixed in an alcohol mixture solution in which tungsten chloride and cesium chloride are dissolved.

3) 50 parts by weight of water is mixed with 100 parts by weight of the solution in which the anticoagulant is mixed and mixed with the solution in which the anticoagulant is mixed.

4) Heat the solution to which water is added to a microwave device (3Kw class laboratory, Korea High Frequency Application Equipment) at an output of 800W and a frequency of 4 kHz for 150 seconds to obtain a hydrated inorganic oxide.

5) The inorganic oxide obtained by removing impurities from the hydrated inorganic oxide and drying is heat-treated in a nitrogen atmosphere at 400 ° C. for 30 minutes using the microwave apparatus to prepare a crystallized inorganic oxide.

<Example 2>

An inorganic compound was prepared in the same manner as in Example 1, except that tungsten chloride and cesium chloride were mixed in an alcohol solvent in a weight ratio of 1 to 0.5.

<Example 3>

An inorganic compound was prepared in the same manner as in Example 1, except that tungsten chloride and cesium chloride were mixed in an alcohol solvent in a weight ratio of 1 to 1.

<Example 4>

An inorganic compound was prepared in the same manner as in Example 1, except that tungsten chloride and cesium chloride were mixed in an alcohol solvent in a weight ratio of 1: 2.

<Example 5>

An inorganic compound was prepared in the same manner as in Example 1, except that tungsten chloride and cesium chloride were mixed in an alcohol solvent in a weight ratio of 1: 3.

<Example 6>

An inorganic compound was prepared in the same manner as in Example 1, except that tungsten chloride and cesium chloride were mixed in an alcohol solvent in a weight ratio of 1 to 5.

&Lt; Comparative Example 1 &

An inorganic compound was prepared in the same manner as in Example 1 except that the inorganic oxide was crystallized by heat treatment in a nitrogen atmosphere at 200 ° C. for 20 minutes.

<Test Example 1> Identification of the prepared inorganic compound

-Test purpose: Checking the composition, particle size and crystallinity of the inorganic compound according to the present invention

-Test method: The composition of the prepared inorganic compound was determined by RBS analysis, the particle size of the prepared inorganic compound was obtained by SEM image, and the crystallinity of the prepared inorganic compound was determined by XRD analysis.

-Check the results: Table 1 below shows the composition ratio of the inorganic compounds prepared according to Examples 1 to 6 and Comparative Examples, Figure 2 is a SEM photograph of the inorganic compound prepared according to Example 1, Figure 3 XRD graph of the inorganic compound prepared according to Example 1, Figure 4 is an XRD graph of the inorganic compound prepared according to Example 6.

Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative example Cs _{0 .348} W ₁ O _{3 .745} Cs _{0 .36} W ₁ O ₄ Cs _{0 .371} W ₁ O ₄ Cs _{0 .386} W ₁ O _{4 .55} Cs _{0 .405} W ₁ O _{4 .44} Cs _{0 .480} W ₁ O _{4 .45} Cs _{0 .36} W ₁ O _{5 .6}

Referring to FIG. 2, the inorganic compound prepared according to Example 1 has a particle size of 20 to 30 nm and has a uniform round shape. Referring to FIG. 3, the inorganic compound prepared according to Example 1 may be a hexagonal particle. 4, it can be seen that the inorganic compound prepared according to Example 6 is mixed with hexagonal crystals and pyrochloro crystals.

<Test Example 2> identification of visible and infrared ray blocking properties of the inorganic compound according to the present invention

-Test purpose: Comparison of visible and infrared blocking properties of the inorganic compound according to the present invention

-Test method: After dispersing the inorganic compounds prepared according to Examples 1 to 6 and Comparative Examples to 15% in ethyl cellosorb, which is a measuring organic solvent, respectively, the dispersion solution was diluted to 0.33% in ethyl cellosorb. Transmittance of visible light (550 nm) and infrared light (780 nm, 950 nm)

-Confirmation of results: The test results are shown in Table 2 below. FIG. 5 is a graph showing the results of diluting the inorganic compound prepared in Example 1 and measuring the UV / Vis / IR spectra. FIG. 6 is the diluting the inorganic compound prepared in Example 6 and measuring the UV / Vis / IR spectra. It is a graph which shows a result, FIG. 7 is a graph which dilutes the inorganic compound manufactured by the comparative example, and shows the UV / Vis / IR spectrum measurement result.

Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative example 550nm transmittance (%) 78 75 76 75 74 69 40 780nm transmittance (%) 34 37 30 37 23 6 60 950 nm transmittance (%) 8 5 7 8 8 3 75

Referring to Tables 1 to 2 and FIGS. 5 to 7, the inorganic compounds prepared according to Examples 1 to 6, that is, even when the ratio of oxygen to tungsten exceeds 3, the transmittance of visible light and infrared ray blocking rate (opposite concept of transmittance) It can be seen that this is high. It can be seen that the inorganic compound prepared by the comparative example has a low visible light transmittance and an infrared shielding rate when the ratio of oxygen to tungsten exceeds 5. Therefore, the film containing the inorganic compound prepared in Examples 1 to 6 has a feature that can pass the light but block the heat.

While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, Should be interpreted as falling within the scope of.

Claims (16)

A metal salt dissolving step of forming an alcohol mixed solution by adding a first metal salt and a second metal salt to an alcohol solvent;
An anticoagulant dissolving step of forming an anticoagulant mixed solution by adding an anticoagulant to the alcohol mixture solution formed in the metal salt dissolving step;
A water mixing step of forming water mixed solution by adding water to the anticoagulant mixed solution formed in the anticoagulant dissolving step;
An inorganic compound synthesis step of preparing an inorganic compound by heating the water mixed solution formed in the water mixing step by microwave;
And a crystallization step of forming a crystallized inorganic compound by heat-treating the inorganic compound prepared in the synthesis step of the inorganic compound. The method of claim 1, wherein the crystallized inorganic compound
Represented by the formula A _x B _y O _z , A is an alkali metal or alkaline earth metal, B is Mg, Mo, V, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ti, Ge, Sn, Pb, W is any one selected from, O is oxygen, x, y, z is 0.001≤x / y≤1, A method for producing an infrared absorbing inorganic compound, characterized in that it has a range of 3 <z / y ≤ 5. The method of claim 2,
In the inorganic compound synthesis step, the microwave is irradiated for 100 to 300 seconds so that the heating temperature is 80 to 120 ℃ method of producing an infrared absorbing inorganic compound. The method of claim 2,
In the crystallization step, a method for producing an infrared absorbing inorganic compound, characterized in that the heat treatment by irradiating microwaves for 0.5 to 2 hours so that the heating temperature is 400 to 800 ℃. The method of claim 4, wherein
The microwave irradiation is carried out in an inert gas atmosphere, the method for producing an infrared absorbing inorganic compound. The method of claim 2,
0.01 to 0.1 mol of the first metal salt and the second metal salt are used with respect to 1 L of the alcohol solvent, respectively.
The anti-agglomerating agent is used 1 to 20 parts by weight based on 100 parts by weight of alcohol mixed solution,
The water is a method for producing an infrared absorbing inorganic compound, characterized in that 5 to 100 parts by weight based on 100 parts by weight of the anticoagulant mixture solution. delete delete delete delete delete delete delete delete delete delete

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