KR20130132025A - Thermal resistance material comprising cesium-molybdenum and method of manufacturing thereof and method of manufacturing thermal resistance film using thereof - Google Patents

Abstract

The present invention relates to a thermal resistance material including cesium-molybdenum having a selective blocking function for heating wire, a manufacturing method thereof and a manufacturing method for thermal resistance film using same. The thermal resistance material including cesium-molybdenum having a selective blocking function for heating wire includes CsxMoyOz. The ratio between x and y is 1:2.5-1:4, the ratio between y and z is 1:2.8-1:3.2, and the ratio between x,y and z is 0.25:1:3-0.4:1:3. According to the present invention, a structure with the optimal mole ratio between cesium and molybdenum is applied to the thermal resistance material to increase visible light transmittance and remarkably improve heating wire blocking rate, thermal transmittance rate and UV blocking rate.

Description

Heat-resisting material having a selective blocking function of the hot wire region containing cesium-molybdenum, and a method of manufacturing the same and a method of manufacturing a heat-resisting film using the same USING THEREOF}

The present invention relates to a heat resistance material having a selective blocking function of a heat ray region including cesium-molybdenum, a method for manufacturing the same, and a method for manufacturing a heat resistance film using the same. More specifically, cesium and molybdenum are combined at an optimum molar ratio. By applying the structure to the heat-resistant material, selective blocking of the hot wire region containing cesium-molybdenum can improve the heat resistance characteristics such as selectively blocking the light of the wavelength corresponding to the hot wire while increasing the transmittance of visible light. It relates to a heat resistance material having a function, a method of manufacturing the same and a method of manufacturing a heat resistance film using the same.

The development of renewable energy or alternative energy technologies is emerging as an alternative technology due to greenhouse gas reduction and fossil energy depletion, and interest in creating added value through efficient management of energy is increasing rapidly.

Therefore, in summer, the heat rays flowing into the room are blocked to increase the efficiency of the room, while the visible light is kept the same as the existing glass to maintain a comfortable interior, and in winter, the function to manage the heat efficiently by minimizing the heat loss in the room. The demand for materials continues, and the demand for transparent thermal barrier materials is expected to soar.

The concept of heat-absorbing materials was proposed in the 1960s, but full-scale research began around 1998, the first products were launched in 2000, and by 2005 the first generation of products was formed.

These attempts to control the heating wire have been developed in various ways such as tilted glass, tilt film, sputter coated glass and sputter coated film, and some of them have already been commercialized, but performance or reliability are still widely available. There is a limit to. In particular, in the prior art, sputter-coated glass is an expensive process, has a weak disadvantage in oxidation and discoloration, the tilt film has a disadvantage of poor durability.

In Europe, which has been preparing alternatives to energy problems early in the 1990s and 2000s, sputter-coated glass, which is known to have the best thermal barrier properties, has a double layer, and an insulated window filled with an inert gas such as argon in the middle ( Low emission glass, low-E glass) was developed and used.

In addition, metal-coated low-emission glass has institutional devices such as Austria, Switzerland and the UK since Germany, and demand has increased, and the use ratio of Japan, China, etc. is gradually increasing in Asia. However, Korea still has the lowest application rate internationally due to lack of awareness of energy management technology.

However, the thin film metal coating technology can realize the performance characteristics such as high transmittance and heat ray shielding characteristics.However, there is a problem that the membrane is separated or discolored due to corrosion in high humidity areas. There is a problem that interferes with.

In addition, Southwall's V-KOOL product, which uses a technology of depositing a metal thin film on a film, has excellent characteristics such as infrared blocking rate of 96%, but the manufacturing process is very complicated, and thus the product price is very high. There is a disadvantage of being expensive.

In addition, in a product to which high heat-transfer performance is given, there is a problem that a multilayer low-emission glass which is continuously stressed due to a large difference in thermal expansion characteristics due to heat radiation absorption introduced from the outside causes an explosion phenomenon.

In addition, the conventional heat shield glass also has a problem that the inside of the light is also darkened by blocking the visible light wavelength.

In other words, in the case of the conventional thermal barrier glass and film development technology, it is not possible to satisfy both heat resistance characteristics, economical efficiency and durability, so that a new concept can be solved and commercialized by applying a new concept rather than the conventional method. Development is required.

The present invention is to solve the above problems, an object of the present invention, by applying a structure in which the cesium and molybdenum combined in the optimum molar ratio to the heat resistance material, while improving the transmittance of visible light of the heat resistance film while improving the heat ray blocking rate The purpose of the present invention is to dramatically improve the overall heat transmission rate.

In addition, cesium carbonate and molybdenum ammonium are mixed at an optimum ratio, and through three-stage heat treatment and annealing, it is aimed to remarkably improve heat resistance characteristics such as thermal conductivity while minimizing a decrease in transmittance of visible light.

In addition, unlike the prior art, the durability is significantly improved and can be used for a long time more than 10 years, according to the improvement of the durability, as well as the vehicle window, the purpose of being able to apply directly to the window of the building.

In addition, by using the optimum metal ball, bead, dispersant and binder, it is possible to form a heat resistant layer quickly and uniformly on the base film, it is economical, and aims to maximize the durability and heat resistance.

In addition, it is an object to provide an environmentally friendly heat resistance film can not only significantly improve the heat resistance characteristics, economics and durability compared to the prior art, but also significantly improve energy efficiency to reduce energy consumption of vehicles and buildings.

A first embodiment of the heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum according to the present invention for achieving the above object, Cs _x Mo _y O _z , the x and the The ratio of y is 1: 2.5 to 1: 4, and the ratio of y to z is 1: 2.8 to 1: 3.2, and the ratio of x to y to z is 0.25: 1: 3 to 0.4: 1: 3.

In addition, a second embodiment of the heat resistance material having a selective blocking function of the hot wire region including cesium-molybdenum according to the present invention is characterized in that it comprises Cs _0.33 Mo ₁ O ₃ .

Next, the method for producing a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum of the present invention, an aqueous solution of cesium carbonate (Cs ₂ CO ₃ ) and ammonium molybdate (H ₈ MoN ₂ O ₄ ) Mixing step of preparing a mixed solution by mixing; Drying the mixed solution to prepare a mixed powder; And a heat treatment step of manufacturing a heat resistant material by heat-treating the mixed powder.

The heat treatment step, the heating step of heating the mixed powder to 400 ℃ to 500 ℃ at a temperature increase rate of 20 ℃ to 40 ℃ per minute; A first heat treatment step of heat treating the mixed powder at 400 ° C. to 500 ° C. for 40 to 80 minutes; A second heat treatment step of heat-treating the mixed powder at 450 ° C. to 800 ° C. for 5 to 20 minutes; And an annealing step of annealing the mixed powder at 450 ° C. to 900 ° C. for 10 to 80 minutes.

In addition, in the mixing step, the cesium carbonate (Cs ₂ CO ₃ ) aqueous solution is mixed with 0.25 to 0.4 mol per mol of the ammonium molybdate (H ₈ MoN ₂ O ₄ ) aqueous solution, the drying The step is characterized in that the mixture is dried for 5 to 10 hours at 100 ℃ to 300 ℃.

In the temperature raising step and the first heat treatment step, it is characterized in that 70 to 110cc per minute hydrogen, 5 to 20cc per minute nitrogen, in the second heat treatment step and the annealing step, to add 70 to 130cc per minute nitrogen It is characterized by.

Next, the method for producing a heat resistance film using a heat resistance material having a selective blocking function of the heat ray region containing cesium-molybdenum according to the present invention, the heat resistance material, dispersant of any one of claims 1 to 3. And a first dispersion step of adding a metal ball to an organic solvent to prepare a mixed sol and to disperse it. A second dispersion step of adding and dispersing beads to the mixed sol to prepare a heat resistance coating solution; And a heat resistance layer forming step of bar coating the heat resistance coating liquid on the base film.

Further, in the first dispersion step, with respect to 100 parts by weight of the organic solvent, the heat resistance material is characterized in that 0.5 to 5 parts by weight, the dispersant is added to 0.5 to 5 parts by weight, in the first dispersion step , The dispersing agent comprises a compound containing a amine and a solvent, the solvent is characterized in that it comprises at least one of butylglycol, methoxypropylacetate or methoxypropanol (methoxypropanol) .

The solvent is characterized in that consisting of 35 to 55% by weight of the methoxypropyl acetate, 35 to 55% by weight of the butyl glycol, 15 to 35% by weight of the methoxypropanol, in the first dispersion step, the metal ball It is characterized by consisting of iron.

In the first dispersion step, the organic solvent may be at least one of ethanol, methanol, butanol, chloroform, dichloromethane, ethyl acetate, hexane, diethyl ether or acetonitrile. In the dispersing step, the dispersion time is characterized in that 90 to 150 minutes.

In the second dispersion step, the bead is characterized in that it comprises a zirconia, in the second dispersion step, the size of the bead is characterized in that 0.1mm to 0.8mm.

In addition, in the second dispersion step, the dispersion time is characterized in that 30 minutes to 90 minutes, in the heat resistance layer forming step, characterized in that the organic binder is added to the heat resistance coating liquid.

The organic binder is at least one of acrylic urethane, ethylene carbonate, methyl ethyl ketone or diacetone alcohol. In the heat resistance layer forming step, the organic binder is 100 to 100 parts by weight of the heat resistance coating liquid. It is characterized by adding 900 parts by weight.

According to the heat resistance material having a selective blocking function of the heat ray region including cesium-molybdenum of the present invention, and a method of manufacturing the same and a method of manufacturing a heat resistance film using the same, a structure in which cesium and molybdenum are combined at an optimal molar ratio By applying to the material, while increasing the transmittance of visible light of the heat resistance film, there is an advantage that can significantly improve the overall heat transmission rate by improving the heat ray blocking rate.

In addition, cesium carbonate and molybdenum ammonium are mixed at an optimum ratio, and through three-step heat treatment and annealing, there is an advantage in that heat resistance characteristics such as thermal conductivity can be significantly improved while minimizing a decrease in the transmittance of visible light.

In addition, unlike the prior art, the durability is significantly improved and can be used for a long time more than 10 years, according to the improved durability there is an advantage that can be applied directly to the window of the building as well as the vehicle window.

In addition, by using the optimum metal ball, bead, dispersant and binder, it is possible to form a heat resistant layer quickly and uniformly on the base film, it is economical, there is an advantage that can maximize the durability and heat resistance.

In addition, as well as significantly improving the heat resistance characteristics, economics and durability compared to the prior art, it is possible to significantly improve the energy efficiency to reduce the energy consumption of vehicles, buildings, there is an environmentally friendly advantage.

1 is a flow chart sequentially showing a method of manufacturing a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum of the present invention
Figure 2 is a graph showing the time-dependent temperature change of the heat treatment step (S12) in the method of manufacturing a heat resistant material having a selective blocking function of the hot wire region containing cesium-molybdenum of the present invention
Figure 3 is a flow chart sequentially showing a method of manufacturing a heat resistance film using a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum of the present invention
4 is a schematic diagram illustrating a first dispersion step (S20) of a method of manufacturing a heat resistant film using a heat resistant material having a selective blocking function of a heat ray region including cesium-molybdenum of the present invention.
FIG. 5 is a schematic diagram illustrating a first dispersion step (S20) of a method of manufacturing a heat resistance film using a heat resistance material having a selective blocking function of a heat ray region including cesium-molybdenum of the present invention.
Figure 6 is a graph showing the change in transmittance for each wavelength annealed at 500 ℃ a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum prepared by the present invention
Figure 7 is a graph showing the change in transmittance for each wavelength annealed at 500 ℃ a thermal resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum prepared by the present invention
Figure 8 is a graph showing the change in transmittance for each wavelength of annealing at 600 ° C heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum prepared by the present invention
9 is a graph showing the change in transmittance for each wavelength of annealing at 600 ° C heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum prepared by the present invention
10 is a graph showing the change in transmittance for each wavelength of annealing at 800 ℃ a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum prepared by the present invention
11 is a graph showing the change in transmittance for each wavelength annealed at 800 ℃ a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum prepared by the present invention

Hereinafter, a heat resistance material having a selective blocking function of a heat ray region including cesium-molybdenum according to the present invention, a method for manufacturing the same, and a method for manufacturing a heat resistance film using the same according to the accompanying drawings. It demonstrates in detail with reference. The present invention may be better understood by the following examples, which are for the purpose of illustrating the present invention and are not intended to limit the scope of protection defined by the appended claims.

First, the first embodiment of the heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum of the present invention, Cs _x Mo _y O _z , wherein the ratio of x and y is 1: 2.5 To 1: 4, and the ratio of y to z is 1: 2.8 to 1: 3.2, more preferably, the ratio of x to y is 1: 3.0 to 1: 3.5, and y It is effective that the ratio of and z is 1: 2.9 to 1: 3.1.

In the present invention, the heat resistance material composed of a structure in which cesium, molybdenum and oxygen atoms are bonded, the molar ratio between these elements has a great effect on the heat resistance characteristics, the inventors have made several experiments, the optimum as a heat resistance material Since the molar ratio has been found, when the molar ratio is out of the molar ratio range, there is a problem that the thermal resistance characteristic is significantly lowered.

The ratio of x to y and _z in the Cs _x Mo _y O _z is preferably 0.25: 1: 3 to 0.4: 1: 3, more preferably 0.30: 1: 3 to 0.35 1: 1 is effective. This is a more optimized value of the molar ratio between cesium, molybdenum and oxygen atoms.

In addition, it is preferable that the second embodiment of the heat resistant material having the selective blocking function of the hot wire region including cesium-molybdenum of the present invention comprises Cs _0.33 Mo ₁ O ₃ . This resulted in several experiments and found the molar ratio to maximize the heat resistance.

Next, the method of manufacturing a heat resistant material having a selective blocking function of the hot wire region containing cesium-molybdenum of the present invention, as shown in Figure 1, the mixing step (S10), drying step (S20) and heat treatment step ( S30), characterized in that made.

Mixing step (S10) is a step of preparing a mixed solution by mixing cesium carbonate (Cs ₂ CO ₃ ) aqueous solution and ammonium molybdate (H ₈ MoN ₂ O ₄ ) aqueous solution. This is a preparatory process for synthesizing the heat resistance material of the present invention in an optimum molar ratio.

Here, the cesium carbonate (Cs ₂ CO ₃ ) aqueous solution is a mixture of cesium carbonate and water, and the ammonium molybdate (H ₈ MoN ₂ O ₄ ) aqueous solution means that a mixture of ammonium molybdate and water.

In the mixing step (S10), with respect to 1 mol of the ammonium molybdate (H ₈ MoN ₂ O ₄ ) aqueous solution, the cesium carbonate (Cs ₂ CO ₃ ) aqueous solution is preferably mixed 0.25 to 0.4 mol, more preferably Preferably, mixing 0.30 to 0.35 moles is effective. When less than 0.25 mole or more than 0.4 mole, the molar ratio between elements of the synthesized heat resistance material is out of the optimum value, and there is a problem that the heat resistance characteristic is significantly lowered.

Drying step (S11) is to dry the mixed solution, to prepare a mixed powder. This is a process of drying the mixed solution so that the heat treatment, which is the next process, can be effectively performed.

Here, it is preferable to dry the said mixture liquid at 100 degreeC-300 degreeC for 5 to 10 hours, More preferably, it is effective to dry at 150 degreeC-200 degreeC for 7 to 9 hours. If it is less than 100 ° C, it is difficult to dry sufficiently, the efficiency of the next heat treatment process is significantly lowered, and if it exceeds 300 ° C, there is a problem that the constituents may be damaged.

Next, the heat treatment step (S12) is a step of producing a heat resistance material by heat treatment of the mixed powder. This is a process for manufacturing a heat resistance material through a heat treatment synthesis process.

As shown in FIG. 2, the heat treatment step S12 includes a temperature raising step S121, a first heat treatment step S122, a second heat treatment step S123, and an annealing step S124.

First, the temperature raising step (S121) corresponds to step (1) of Figure 2, the step of heating the mixed powder to 400 ℃ to 500 ℃ at a temperature rising rate of 20 ℃ to 40 ℃ per minute. This is a process of heating up at an optimum rate for effective heat treatment of the mixed powder.

Here, it is preferable that the temperature increase rate is 20 to 40 degreeC per minute, More preferably, it is effective that it is 25 to 30 degreeC per minute, Most preferably, it is 27.5 degreeC. If it is less than 20 ° C or exceeds 40 ° C, not only economic efficiency is poor, but also a problem that the heat resistance material is not uniformly synthesized.

The first heat treatment step (S122) is a step of heat-treating the mixed powder for 40 to 80 minutes at 400 ℃ to 500 ℃. This is the first heat treatment process that causes synthesis by heating the mixed powder while maintaining a constant temperature.

It is preferable that heat processing temperature is 400 degreeC-500 degreeC, More preferably, it is effective that it is 430 degreeC-470 degreeC. If the temperature is less than 400 ° C., the synthesis termination reaction occurs, and if the temperature exceeds 500 ° C., there is a problem in that it is difficult to form uniform thermal resistance material particles due to rapid synthesis.

In the temperature raising step (S121) and the first heat treatment step (S122), it is preferable to add 70 to 110cc hydrogen per minute, 5 to 20cc nitrogen per minute, more preferably, 85 to 95cc hydrogen per minute, nitrogen It is effective to add 8 to 12cc per minute. This is to improve pressure control and reactivity in order to increase the efficiency of the temperature increase and the synthesis reaction. If it is out of the input range, it may rather interfere with the synthesis reaction, lowering the yield.

The second heat treatment step (S123) is a step of heat-treating the mixed powder at 450 ° C. to 800 ° C. for 5 to 20 minutes. This is the second heat treatment process in which a full synthetic reaction takes place.

Here, it is preferable that the heat processing temperature is 450 degreeC-800 degreeC, More preferably, it is effective that it is 500 degreeC-600 degreeC, It is preferable that the heat processing time is 5 to 20 minutes, More preferably, it is 8 to 12 minutes Is effective. If it is out of the above range, there is a problem that the heat resistance material of the present invention is difficult to synthesize.

Finally, the annealing step (S124) is a step of annealing the mixed powder at 450 ℃ to 900 ℃ for 10 to 80 minutes. This is a process for maximizing the selective blocking characteristics of the heat ray region of the heat-resistant material synthesized by heat treatment by performing annealing under optimum conditions.

Here, it is preferable that annealing temperature is 450 degreeC-900 degreeC, More preferably, it is effective that it is 480 degreeC-600 degreeC, and most preferably 500 degreeC. If the temperature is less than 450 ° C., the heat resistance of the heat resistant material is remarkably inferior, and if it exceeds 900 ° C., there is a problem that the transparency of the heat resistant material is sharply lowered.

In the second heat treatment step (S123) and the annealing step (S124), it is preferable to add 70 to 130cc per minute nitrogen, more preferably, 90 to 110cc per minute nitrogen is effective. This is to improve the pressure control and reactivity to increase the efficiency of heat treatment and annealing. If it is out of the input amount range, rather, the synthesis and annealing reaction may be hindered, thereby lowering the yield and lowering the performance of the heat resistant material.

Next, the method of manufacturing a heat resistance film using a heat resistance material having a selective blocking function of the heat ray region including cesium-molybdenum of the present invention, as shown in Figure 3, the first dispersion step (S20), the second It comprises a dispersion step (S21) and the heat resistance layer forming step (S22).

First, as shown in FIGS. 4 and 5, in the first dispersion step S20, the heat resistance material, the dispersant and the metal ball of any one of claims 1 to 3 are added to the organic solvent and mixed. The sol is prepared and dispersed. This is a preparatory process for coating the film of the heat resistant material particles prepared in the present invention.

Here, when a heat resistant material, a dispersant, and a metal ball are added to the organic solvent and stirred, they are in the form of a sol while the heat resistant material particles are evenly dispersed in the organic solvent by the metal ball and the dispersant.

In the first dispersion step (S20), with respect to 100 parts by weight of the organic solvent, 0.5 to 5 parts by weight of the heat resistant material, 0.5 to 5 parts by weight of the dispersing agent is added, more preferably, The heat resistance material is 0.5 to 2.5 parts by weight, it is effective to add 0.5 to 3.0 parts by weight of the dispersant. If it is out of the above range, not only the transparency of the heat resistant material is significantly lowered, but also the heat resistant particles are not effectively dispersed in the heat resistant film, and there is a problem that the heat resistance efficiency is also lowered.

In the case of the metal ball, it is preferable to include 10 to 20 parts by weight based on 100 parts by weight of the organic solvent.

In addition, the dispersant may be made of a compound containing a amine and a solvent, and may be any compound containing an amine, but the solvent is butylglycol, methoxypropylacetate or methoxypropanol It is preferable to include at least one of). This is the most effective dispersion of the heat resistant material particles of the present invention, it was confirmed by several experiments.

The solvent is preferably butylglycol (butylglycol), methoxypropylacetate (Methoxypropylacetate) and methoxypropanol (methoxypropanol), and more preferably, 35 to 55% by weight of the methoxypropyl acetate, the butyl It is most effective to consist of 35 to 55% by weight of glycol, 15 to 35% by weight of the methoxypropanol. If the content ranges, the dispersion efficiency can be maximized.

In addition, in the first dispersion step (S20), the metal ball may be made of any metal, but made of iron is most suitable for the present invention.

The organic solvent is preferably at least one of ethanol, methanol, butanol, chloroform, dichloromethane, ethyl acetate, hexane, diethyl ether or acetonitrile, and more preferably, ethanol.

The dispersion time of the first dispersion step (S20) is preferably 90 to 150 minutes, more preferably 110 to 130 minutes. When it is less than 90 minutes, it is difficult to fully form a mixed sol, and when it exceeds 150 minutes, there exists a problem of inferior economy.

Next, the second dispersion step (S21) is to add a beads to the mixed sol, to disperse, to prepare a heat resistance coating liquid. This is a process for producing a uniform heat resistance coating liquid by easily dispersing the mixed sol prepared by dispersion, heat resistance coating.

In other words, the mixed sol is a step of adding beads and stirring again.

Here, the beads are preferably made of zirconia. The beads can more uniformly disperse the heat resistant material particles dispersed in the mixed sol.

The size of the beads is preferably 0.1mm to 0.8mm, more preferably 0.3mm to 0.5mm. If it is less than 0.1 mm, the dispersion effect is insignificant, and if it exceeds 0.8 mm, the dispersion uniformity is lowered.

The dispersion time of the second dispersion step (S21) is preferably 30 to 90 minutes, more preferably 50 to 70 minutes. When it is less than 90 minutes, it is difficult to fully disperse, and when it exceeds 90 minutes, there exists a problem of inferior economy.

Finally, the heat resistance layer forming step (S22) is a step of bar coating the heat resistance coating liquid on the base film. This is a step of forming a heat resistance layer on the base film to produce a heat resistance film.

Here, before the bar coating, it is preferable to add the organic binder to the heat resistance coating liquid. This is not only to effectively coat the base film, but also to improve adhesion durability.

The organic binder is preferably at least one of acrylic urethane, ethylene carbonate, methyl ethyl ketone or diacetone alcohol.

In addition, the organic binder is preferably added to 100 to 900 parts by weight, more preferably 300 to 600 parts by weight, most preferably 500 parts by weight based on 100 parts by weight of the heat resistance coating liquid. If it is less than 100 parts by weight, the durability of the heat resistant film is significantly lowered. If it exceeds 900 parts by weight, there is a problem that the heat resistance characteristics of the heat resistant film are lowered.

In addition, the heat resistance layer forming step (S22), after applying the heat resistance coating liquid to the base film, it is preferably baked for 30 seconds to 2 minutes at 60 ℃ to 90 ℃, it is preferable to perform ultraviolet curing.

Ultraviolet curing is preferably performed for 10 to 30 seconds at an intensity of 600 W / cm to 1000 W / cm.

Here, the base film may be any material in the form of a film, but it is preferable to use a PET film.

Hereinafter, the results of experiments of changes in transmittance for each wavelength according to the temperature of the annealing of the heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum prepared by the present invention.

Here, Cs _0.33 Mo ₁ O ₃ was used as the heat resistance material, and the content thereof was 100 parts by weight of the organic solvent, and the heat resistance material was (a) 0.5 part by weight, (b) 1.0 part by weight, (c) 1.5 The experiment was conducted by adding 2.5 parts by weight of (d).

6 and 7 are heat resistance materials annealed at 500 ° C., and the transmittance was generally excellent. FIGS. 8 and 9 are heat resistance materials annealed at 600 ° C., and FIGS. 10 and 11 are at 800 ° C. FIG. As the heat resistance material annealed, it was found that the transmittance decreased as the annealing temperature increased.

However, the thermal resistance material within the scope of the present invention has been proved to be very excellent in permeability as compared with the conventional thermal resistance material as a whole.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. It is clear that the present invention can be suitably modified and applied in the same manner. Therefore, the above description does not limit the scope of the present invention, which is defined by the limitations of the following claims.

Claims (22)

Cs _x Mo _y O _z ,
The ratio of x to y is 1: 2.5 to 1: 4, and the ratio of y to z is 1: 2.8 to 1: 3.2. The selective blocking function of the hot wire region including cesium-molybdenum Heat resistance material
The method of claim 1,
The ratio of x, y, and z is 0.25: 1: 3 to 0.4: 1: 3, a thermal resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that
Cs _0.33 Mo ₁ O ₃ Heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum characterized in that it comprises
A mixing step of preparing a mixed solution by mixing a cesium carbonate (Cs ₂ CO ₃ ) aqueous solution and an ammonium molybdate (H ₈ MoN ₂ O ₄ ) aqueous solution;
Drying the mixed solution to prepare a mixed powder; And
A heat treatment step of manufacturing a heat resistant material by heat-treating the mixed powder; a method of manufacturing a heat resistant material having a selective blocking function of a hot wire region including cesium-molybdenum, characterized in that it comprises a.
5. The method of claim 4,
The heat treatment step may include:
A heating step of heating the mixed powder to 400 ° C. to 500 ° C. at a temperature rising rate of 20 ° C. to 40 ° C. per minute;
A first heat treatment step of heat treating the mixed powder at 400 ° C. to 500 ° C. for 40 to 80 minutes;
A second heat treatment step of heat-treating the mixed powder at 450 ° C. to 800 ° C. for 5 to 20 minutes; And
Annealing step of annealing the mixed powder at 450 ℃ to 900 ℃ for 10 to 80 minutes; Method of manufacturing a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that comprises a
The method according to claim 4 or 5,
In the mixing step, with respect to 1 mol of the ammonium molybdate (H ₈ MoN ₂ O ₄ ) aqueous solution, the cesium carbonate (Cs ₂ CO ₃ ) aqueous solution comprises cesium-molybdenum, characterized in that to mix 0.25 to 0.4 mol Manufacturing method of heat resistant material having selective blocking function of hot wire region
The method according to claim 4 or 5,
The drying step, the method of producing a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that for 5 to 10 hours to dry the mixed solution at 100 ℃ to 300 ℃.
6. The method of claim 5,
In the heating step and the first heat treatment step, a method of manufacturing a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that 70 to 110cc per minute hydrogen, 5 to 20cc per minute nitrogen.
6. The method of claim 5,
In the second heat treatment step and the annealing step, a method of manufacturing a heat resistant material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that 70 to 130cc per minute nitrogen is added.
The first dispersion step of adding a heat resistance material, a dispersant and a metal ball of any one of claims 1 to 3 to the organic solvent to prepare a mixed sol, and to disperse;
A second dispersion step of adding and dispersing beads to the mixed sol to prepare a heat resistance coating solution; And
A method of manufacturing a heat resistance film using a heat resistance material having a selective blocking function of the heat ray region comprising cesium-molybdenum, characterized in that it comprises a; a heat resistance layer forming step of bar coating the heat resistance coating liquid on the base film
The method of claim 10,
In the first dispersion step, with respect to 100 parts by weight of the organic solvent, 0.5 to 5 parts by weight of the heat resistant material, 0.5 to 5 parts by weight of the dispersing agent of the hot wire region containing cesium-molybdenum Manufacturing method of heat resistant film using heat resistant material with selective blocking function
The method according to claim 10 or 11,
In the first dispersion step, the dispersing agent comprises a compound and a solvent containing an amine, the solvent is at least one of butyl glycol (butylglycol), methoxypropylacetate (methoxypropanol) or methoxypropanol (methoxypropanol) Method for producing a thermal resistance film using a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum comprising
13. The method of claim 12,
The solvent has a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that consisting of 35 to 55% by weight of the methoxypropyl acetate, 35 to 55% by weight of the butyl glycol, 15 to 35% by weight of the methoxypropanol Method for manufacturing a thermal resistance film using a thermal resistance material having a
The method according to claim 10 or 11,
In the first dispersion step, the metal ball is a method of manufacturing a heat resistance film using a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that made of iron
The method according to claim 10 or 11,
In the first dispersion step, the organic solvent comprises cesium-molybdenum, characterized in that at least one of ethanol, methanol, butanol, chloroform, dichloromethane, ethyl acetate, hexane, diethyl ether or acetonitrile. Manufacturing method of heat resistant film using heat resistant material having selective blocking function of hot wire region
The method according to claim 10 or 11,
In the first dispersion step, the dispersion time is a method of manufacturing a heat resistance film using a heat resistant material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that 90 to 150 minutes.
The method according to claim 10 or 11,
In the second dispersion step, the bead comprises a zirconia method of producing a heat resistance film using a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that
The method according to claim 10 or 11,
In the second dispersion step, the size of the beads is 0.1mm to 0.8mm method of manufacturing a heat resistance film using a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that
The method according to claim 10 or 11,
In the second dispersion step, the dispersion time is 30 minutes to 90 minutes, the method of manufacturing a heat resistance film using a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that
The method according to claim 10 or 11,
In the step of forming the heat resistance layer, a method of manufacturing a heat resistance film using a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that the organic binder is added to the heat resistance coating liquid.
The method of claim 20,
The organic binder is a method of producing a thermal resistance film using a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that at least one of acrylic urethane, ethylene carbonate, methyl ethyl ketone or diacetone alcohol.
The method of claim 20,
In the heat resistance layer forming step, with respect to 100 parts by weight of the heat resistance coating liquid, the organic binder is a heat resistance material having a selective blocking function of the hot wire region containing cesium-molybdenum, characterized in that the addition of 100 to 900 parts by weight. Method of manufacturing a thermal resistance film using

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