JP2009167330A - Paint for forming infrared ray shielding film and infrared ray shielding material - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a paint for forming an infrared ray shielding film hardly causing application film defects such as cissing and irregularity on application to a transparent base material surface of a resin film and the like, and to provide an infrared ray shielding material. <P>SOLUTION: This paint is prepared by dispersing or dissolving fine particles of composite tungsten oxide, which is represented by a general formula M<SB>Y</SB>WO<SB>Z</SB>(wherein M is at least one kind of element selected from H, He, alkali metals, alkaline-earth metals, rare earth elements, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be, Hf, Os, Bi, and I, W is tungsten, O is oxygen, 0.001≤Y≤1.0, and 2.2≤Z≤3.0) and has a hexagonal system crystal structure, a surfactant and a binder resin in a solvent. The infrared ray shielding material is composed of a transparent base material and the infrared ray shielding film formed on the base material surface by using the above paint. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a coating material for forming an infrared shielding film in which composite tungsten oxide fine particles that are transparent in the visible light region and absorb in the near infrared region are dispersed in a solvent. The present invention relates to an improvement in a coating material for forming an infrared shielding film in which coating film defects such as repellency, leakage and unevenness hardly occur when applied, and an infrared shielding body produced using this coating material.

As this type of coating material for forming an infrared shielding film, a coating material (infrared shielding material) in which composite tungsten oxide fine particles represented by the general formula _MY WO _Z and having a hexagonal crystal structure are dispersed in a solvent such as an organic solvent. (Dispersion liquid of material fine particles) was proposed by the present applicant (see Patent Document 1), and was formed by applying the paint (dispersion liquid of infrared shielding material fine particles) on the surface of a transparent substrate such as a resin film. An infrared shielding film (infrared shielding material fine particle dispersion) has already been proposed in Patent Document 1.

  By the way, the infrared shielding film (infrared shielding material fine particle dispersion) in which the composite tungsten oxide fine particles are dispersed in the film is, as described above, an infrared shielding film forming coating (on the surface of a transparent substrate such as a resin film). Infrared shielding material fine particle dispersion) is applied.

  As a method for applying the infrared shielding film-forming coating material on the transparent substrate surface, gravure roll coating method, reverse roll coating method, dip coating method, blade coating method, air knife coating method, wire block coating method, reblocks Known methods such as a coating method, a reblock roll coating method, an extrusion coating method, a rod coating method, a wire bar coating method, a slide coating method, and a curtain coating method are used.

  However, when the above-described coating material for forming an infrared shielding film is applied onto the surface of the transparent substrate using these known coating methods, the surface of the transparent substrate may be repelled or missing depending on the composition of the coating material or the surface state of the transparent substrate. There has been a problem that coating film defects and coating unevenness (transverse unevenness) continuously generated in the width direction with respect to the coating direction may be remarkably exhibited, and the performance required for the infrared shielding film is not satisfied.

  One of the methods for improving the coating property is a surface treatment for the substrate surface (coating surface). As this surface treatment method, ultraviolet treatment, corona discharge treatment, glow discharge treatment, flame treatment, high frequency treatment, plasma treatment are performed. Laser treatment, mechanical treatment, mixed acid treatment, ozone oxidation treatment and the like are known, and in particular, corona discharge treatment and glow discharge treatment are widely used industrially. And about a corona discharge process, there exists the method described in patent documents 2-7, for example, and there exists a method described in patent documents 8-14 about glow discharge processing, for example.

However, these surface treatment methods require heating and cooling of the base material in the course of the surface treatment, so that the base material itself is easily plastically deformed, and the flatness of the base material surface is impaired. A molecular weight body (such as an additive or a monomer component of a resin film as a base material) may be deposited on the surface of the base material, thereby deteriorating transparency and blocking resistance. Furthermore, since it is difficult to deal with various base materials and coating compositions only by surface treatment of these base materials, the coating unevenness cannot be completely eliminated.
International Publication WO 2005/37932 (Claim 1, Paragraph 0069) Japanese Patent Publication No. 48-5043 Japanese Examined Patent Publication No. 47-51905 JP 47-28067 A JP 49-83767 A JP-A-51-41770 JP 51-131576 A Japanese Patent Publication No. 35-7578 Japanese Patent Publication No. 36-10336 JP-A-45-22004 JP-A 45-22005 JP-A-45-24040 JP-A-46-43480 JP-A-53-129262

  The present invention has been made paying attention to such problems, and the problem is that when coated on a transparent substrate such as a resin film, coating film defects such as repellency, leakage, unevenness, etc. are caused. An object of the present invention is to provide a coating material for forming an infrared shielding film which is difficult, and to provide an infrared shielding body manufactured using the coating material.

  Therefore, the inventors of the present invention diligently studied to solve the above problems, and by adding a surfactant into the infrared shielding film-forming coating material in which the composite tungsten oxide fine particles are dispersed, It has been found that coating film defects such as unevenness are prevented. Furthermore, an infrared shielding body composed of an infrared shielding film formed using an infrared shielding film-forming coating material in which the surfactant is dispersed and a transparent substrate has a precise in-plane uniformity, It has also been found that it is transparent in the visible light region and has excellent shielding properties in the near infrared region. The present invention has been completed by such technical discovery.

That is, the invention according to claim 1
Assuming a paint for forming an infrared shielding film,
General formula M _Y WO _Z (where M is H, He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo , Ta, Re, Be, Hf, Os, Bi, I, one or more elements, W is tungsten, O is oxygen, and 0.001 ≦ Y ≦ 1.0, 2.2 ≦ A composite tungsten oxide fine particle represented by Z ≦ 3.0) and having a hexagonal crystal structure, a surfactant and a binder resin are dispersed or dissolved in a solvent.

Next, the invention according to claim 2
On the premise of the infrared shielding film forming paint according to the invention of claim 1,
The content of the surfactant is 0.001 to 10 parts by weight when the entire coating is 100 parts by weight,
The invention according to claim 3
Based on the infrared shielding film forming paint according to the invention of claim 1 or 2,
The composite tungsten oxide fine particles are composite tungsten oxide fine particles having a particle diameter of 1 nm to 800 nm.

The invention according to claim 4
On the premise of the infrared shielding film forming paint according to the invention of claim 1,
The surfactant is at least one selected from a cationic, anionic, amphoteric or nonionic surfactant,
The invention according to claim 5
Based on the infrared shielding film forming paint according to the invention of claim 4,
The nonionic surfactant is a silicone surfactant composed of a silicone compound having a hydrophobic group of dimethylpolysiloxane and a hydrophilic group of polyalkylene oxide,
The invention according to claim 6
On the premise of the infrared shielding film forming paint according to the invention of claim 5,
The silicone-based surfactant is one or more selected from the following chemical formulas (1) to (6).

［但し、化学式（１）〜（６）中において、Ｒはアルキル基または水素を示し、Ｒ’はアルキレン基を示し、また、ａ、ｂはそれぞれ１〜５００の整数、ｍ、ｎはそれぞれ１〜２００の整数である。］
更に、請求項７に係る発明は、
赤外線遮蔽体を前提とし、
請求項１〜６のいずれかに記載の赤外線遮蔽膜形成用塗料を透明基材の面上に塗布しかつ形成された塗布膜を板状、フィルム状または薄膜状に成形して成る赤外線遮蔽膜と、上記透明基材とで構成されることを特徴とする。

[In the chemical formulas (1) to (6), R represents an alkyl group or hydrogen, R ′ represents an alkylene group, a and b are each an integer of 1 to 500, and m and n are 1 respectively. It is an integer of ~ 200. ]
Furthermore, the invention according to claim 7 provides
Assuming an infrared shield,
An infrared shielding film formed by coating the coating material for forming an infrared shielding film according to any one of claims 1 to 6 on a surface of a transparent substrate, and forming the formed coating film into a plate shape, a film shape, or a thin film shape. And the transparent substrate.

  The infrared shielding film-forming paint according to the present invention is characterized in that composite tungsten oxide fine particles, a surfactant and a binder resin are dispersed or dissolved in a solvent.

  When the infrared shielding film-forming paint according to the present invention is applied to a transparent substrate such as a resin film, coating film defects such as repellency, leakage, and unevenness are unlikely to occur. The infrared shielding body composed of the formed infrared shielding film and a transparent substrate has a precise in-plane uniformity, and is transparent in the visible light region and has excellent shielding properties in the near infrared region. Has an effect.

  Hereinafter, embodiments of the present invention will be described in detail.

First, the coating material for forming an infrared shielding film according to the present invention has a general formula M _Y WO _Z (where M is H, He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe). Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S , Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be, Hf, Os, Bi, I, one or more elements, W is tungsten, O is oxygen, and 0.001 ≦ Y ≦ 1.0, 2.2 ≦ Z ≦ 3.0) and a composite tungsten oxide fine particle having a hexagonal crystal structure, a surfactant and a binder resin are dispersed in a solvent. Alternatively, it is dissolved.

1. The composite tungsten microparticles general, because there is no valid free electrons in WO _3, WO ₃ absorption in the near infrared region, the reflection characteristic is small, not effective as an infrared-shielding material. On the other hand, so-called tungsten bronze in which positive elements such as Na are added to tungsten trioxide is known to be a conductive material and a material having free electrons, suggesting a response of free electrons to light in the infrared region. ing. The present applicant has found that there is a particularly effective range as an infrared shielding material in a specific portion of the composition range of tungsten and oxygen, and is transparent in the visible light region and has absorption in the near infrared region. Composite tungsten oxide fine particles are obtained (see Patent Document 1). In this specification, the term “transparent” is used in the sense that the light is less scattered and has high transparency.

  Here, the particle diameter (sometimes abbreviated as particle diameter) of the composite tungsten oxide fine particles can be selected depending on the purpose of use, but when used for applications that maintain transparency, it is 800 nm or less. It preferably has a particle size. This is because particles having a particle diameter of 800 nm or less do not completely block light due to scattering, can maintain visibility in the visible light region, and at the same time can efficiently maintain transparency. In particular, when importance is attached to transparency in the visible light region, it is necessary to further consider scattering by particles. When importance is attached to the reduction of scattering by the particles, the particle diameter is 200 nm or less, preferably 100 nm or less. The reason for this is that if the particle size of the particles is small, the scattering of light in the visible light region of 400 nm to 780 nm due to geometrical scattering or Mie scattering is reduced, and as a result, the infrared shielding film becomes like a frosted glass and becomes clear. This is because it is possible to avoid the loss of transparency. That is, when the particle diameter is 200 nm or less, geometric scattering or Mie scattering is reduced, and a Rayleigh scattering region is obtained. This is because in the Rayleigh scattering region, the scattered light decreases in inverse proportion to the sixth power of the particle diameter, so that the scattering is reduced and the transparency is improved as the particle diameter decreases. Further, when the particle diameter is 100 nm or less, the scattered light is preferably very small. Thus, from the viewpoint of avoiding light scattering, it is preferable that the particle diameter is small, and industrial production is easy if the particle diameter is 1 nm or more.

  Then, by selecting the particle diameter to be 800 nm or less, the visible light transmittance is 85% for the haze value of the infrared shielding material fine particle dispersion (for example, the above-described infrared shielding film) in which the infrared shielding material fine particles are dispersed in the medium. Below, it can be 30% or less of haze. When the haze value exceeds 30%, it becomes like frosted glass, and clear transparency cannot be obtained.

  Moreover, it is preferable from the viewpoint of improving the weather resistance of the fine particles that the surface of the composite tungsten oxide fine particles according to the present invention is coated with an oxide containing one or more of Si, Ti, Zr, and Al.

2. Surfactant It is preferable to control the wettability and leveling property of the coating material with respect to the substrate in order to obtain good coating properties without the above-mentioned repelling, removal, unevenness and the like. In the physical properties of the paint, the leveling property is improved as the surface tension is high, the viscosity is low, and the drying speed is low, and the wettability is improved by decreasing the contact angle with the substrate surface. In the case of a paint composed of various solvents, in the coating film forming process, the paint is dried and solidified while changing its composition as needed. What is important in the applicability is whether the lipophilicity / hydrophilicity balance (HLB) of the composition immediately before solidification has better surface activity than the physical properties of the coating. However, in addition to surface tension and viscosity (applicability), solvents used in paints are polar (related to filler dispersibility), boiling point and vapor pressure (related to drying speed), resin solubility, and safety. Therefore, it is often difficult to obtain good coating properties by simply adjusting the solvent composition.

  One effective means for controlling the surface tension of the coating material with respect to the substrate is the addition of a surfactant applied in the present invention. The surfactant has a hydrophilic part and a lipophilic part in one molecule, and forms a micelle having the hydrophilic part on the outside in water and a micelle which is reversed inside and outside in a nonpolar solvent. Therefore, since these micelles can incorporate substances having different properties from the external environment, in the presence of a surfactant, both polar and non-polar substances including fillers such as binders and composite tungsten oxide fine particles are contained. The mixed state becomes uniform, and the surface activity (surface tension) of the paint with respect to the substrate surface changes.

  In order for the paint to exhibit good surface activity, the ratio of the lipophilic group (lipophilic part) and the hydrophilic group (hydrophilic part) in the same molecule is important, and if either one becomes too large, the interface Activity is lost. That is, in the surfactant, the balance between the hydrophilic group and the lipophilic group is important, and the strength of the active action is quantitatively shown by the HLB value.

  The purpose of use of the surfactant in the present invention is to volatilize and remove the solvent in order from a low boiling point solvent of [coating liquid (coating liquid)] [thin liquid film] [dry film]. ) In the process of changing the composition, the polar liquid and the non-polar solvent are uniformly mixed until the liquid composition of the coating liquid (paint liquid) loses its fluidity. The purpose is to optimize the energy, that is, to improve the liquid properties.

  By the way, surfactants are roughly classified into ionic (cationic / anionic / zwitteric) hydrophilic parts and nonionic (nonionic) parts. It is classified into a system. The ionic surfactant means a surfactant that dissociates from a counter ion in a liquid and ionizes the main chain. Here, the main chain indicates the side having a higher molecular weight after dissociation.

  Specific examples of the anionic surfactant include surfactants composed of fatty acid salts, sulfate esters, sulfonates, phosphate esters, and the like. Specific examples of the cationic surfactant include quaternary ammonium salt type surfactants and amine salt type surfactants. A zwitterionic (both ions) surfactant has both an anionic site and a cationic site in the molecule, and has a structure in which each of the above is combined. Type surfactants, betaine type surfactants, amine oxide type surfactants and the like. Furthermore, nonionic (nonionic) surfactants have a hydrophilic portion that is not ionized, and specifically include ether type surfactants, polyhydric alcohol type surfactants, ester type surfactants, polyvalent surfactants. In addition to alcohol ester surfactants and alkanolamide surfactants, nonionic fluorine surfactants (perfluoroalkylethylene oxide adducts, etc.), nonionic silicone surfactants and the like can be mentioned.

  When forming an infrared shielding film on the surface of a transparent substrate using a coating material for forming an infrared shielding film, at least one surfactant selected from the cation, anion, amphoteric or nonionic surfactant is contained in a solvent. By dispersing the coating material in the surface, the wettability of the paint on the surface of the base material is improved, thereby improving the coating property, and the infrared shielding film having a precise in-plane uniformity without coating film defects such as repellency, leakage, unevenness, etc. Can be obtained.

  As the surfactant applied in the present invention, either an ionic (cationic, anionic or amphoteric) surfactant or a nonionic surfactant can be used. A silicone surfactant that is an agent is particularly desirable.

  When the above ionic surfactant is used, depending on the type of solvent or binder resin used, the surfactant ions dissociated in the solution may cause electrostatic repulsion between the dispersed composite tungsten oxide particles. The affinity between the composite tungsten oxide fine particles and the solvent may be changed by displacement or adsorption of the surfactant on the surface of the composite tungsten oxide fine particles. Depending on the composition of the coating material, the composite tungsten oxide fine particles are likely to aggregate in the dispersion, which may cause problems such as clouding of the coating film when the coating film is formed. On the other hand, since the nonionic surfactant has a hydrophilic group that is not ionized, the surfactant is not electrostatically adsorbed on the surface of the composite tungsten oxide fine particles to change the dispersibility. However, sufficient surface active effects may not be obtained with the low molecular weight type.

  The silicone-based surfactants are mainly nonionic and exhibit an excellent surfactant effect due to their high solubilizing power in nonpolar solvents. And since the said silicone type surfactant which is a polymeric surfactant can change the lipophilicity and hydrophilicity balance (HLB) according to the functional group, molecular skeleton, and molecular weight of a molecular side chain or a terminal, The optimum one for each solvent system can be selected and used. Furthermore, even if the reactivity to the filler surface is high, it is difficult to deteriorate the dispersibility of the filler due to the steric hindrance effect of the polymer, and bleeding (exudation from the coating film surface over time) and foaming due to excessive addition of surfactant. There is an advantage that there are few (causes of film defects).

  As the silicone surfactant that is a polymer surfactant, a silicone compound in which the hydrophobic group is dimethylpolysiloxane and the hydrophilic group is polyalkylene oxide can be used. Specifically, when one or more silicone surfactants represented by the following chemical formulas (1) to (6) are applied, the dispersibility of the composite tungsten oxide fine particles in the coating material for forming an infrared shielding film is impaired. Therefore, the wettability of the coating material with respect to the transparent substrate surface is improved, and it becomes possible to obtain an infrared shielding film having a precise in-plane uniformity without a coating film defect.

  In addition, you may use other surfactant together in the range which does not impair the said effect.

［但し、化学式（１）〜（６）中において、Ｒはアルキル基または水素を示し、Ｒ’はアルキレン基を示し、また、ａ、ｂはそれぞれ１〜５００の整数、ｍ、ｎはそれぞれ１〜２００の整数である。］
ここで、赤外線遮蔽膜形成用塗料内への界面活性剤の添加量は、塗料全体を１００重量部とした場合に０．００１〜１０重量部の範囲に設定することが望ましく、０．００５〜５重量部の範囲が特に望ましい。添加量が０．００１重量部未満であると基材に対する濡れ性や乾燥時のレベリング性が十分でない場合があり、また、１０重量部を超えて過剰に添加した場合、塗液のＨＬＢが最適範囲から外れ、塗布性が逆に悪化するだけでなく、塗料の泡立ちや完成塗膜のブリーディングを引き起こす原因となる場合があるからである。

[In the chemical formulas (1) to (6), R represents an alkyl group or hydrogen, R ′ represents an alkylene group, a and b are each an integer of 1 to 500, and m and n are 1 respectively. It is an integer of ~ 200. ]
Here, the addition amount of the surfactant in the coating material for forming an infrared shielding film is desirably set in the range of 0.001 to 10 parts by weight when the entire coating is 100 parts by weight, A range of 5 parts by weight is particularly desirable. If the addition amount is less than 0.001 part by weight, the wettability to the substrate and the leveling property at the time of drying may not be sufficient, and if the addition amount exceeds 10 parts by weight, the HLB of the coating solution is optimal. This is because the coating property is not only within the range and the applicability deteriorates, but it may cause foaming of the paint and bleeding of the finished coating film.

3. Solvent The solvent applied to the infrared shielding film-forming coating material of the present invention is not particularly limited, and a known organic solvent can be used. Specifically, alcohol solvents such as methanol (MA), ethanol (EA), 1-propanol (NPA), isopropanol (IPA), butanol, pentanol, benzyl alcohol, diacetone alcohol, acetone, methyl ethyl ketone (MEK) , Ketone solvents such as methyl propyl ketone, methyl isobutyl ketone (MIBK), cyclohexanone, isophorone, ester solvents such as 3-methyl-methoxy-propionate (MMP), ethylene glycol monomethyl ether (MCS), ethylene glycol monoethyl ether (ECS), ethylene glycol isopropyl ether (IPC), propylene glycol methyl ether (PGM), propylene glycol ethyl ether (PE), propylene glycol methyl Glycol derivatives such as ether acetate (PGMEA), propylene glycol ethyl ether acetate (PE-AC), formamide (FA), N-methylformamide, dimethylformamide (DMF), dimethylacetamide, N-methyl-2-pyrrolidone ( Amides such as NMP), aromatic hydrocarbons such as toluene and xylene, and halogenated hydrocarbons such as ethylene chloride and chlorobenzene. Among them, organic solvents with low polarity are preferable, and particularly highly hydrophobic ones such as ketones such as MIBK and MEK, aromatic hydrocarbons such as toluene and xylene, glycol ether acetates such as PGMEA and PE-AC, and the like. preferable. These solvents can be used alone or in combination of two or more.

4). Binder resin The paint for forming an infrared shielding film needs to contain a binder component, and a known curable resin can be used as the binder component. For example, a thermosetting resin, a UV curable resin, an electron beam curable resin, or the like can be selected according to the purpose. And as thermosetting resin, resin using the crosslinking reaction of prepolymers, such as a melamine resin, a urethane resin, an epoxy resin, can be mentioned. Examples of thermosetting, UV curable, or electron beam curable resins include polyfunctional polymerizable unsaturated compounds. For example, polyfunctional acrylate or methacrylate [pentaerythritol (meth) acrylate or dipentaerythritol hexa (meth) ) Acrylate etc.]. Furthermore, it is preferable to add a filler, a polymerization initiator, and a polymerization accelerator to these binder components as necessary.

5. Transparent substrate The material of the transparent substrate in the present invention is not particularly limited as long as it is a transparent body, and glass, a resin sheet, or a resin film is preferably used. The resin sheet or resin film is not particularly limited as long as it does not cause problems in the surface state and durability of the required sheet or film. For example, polyester polymers such as polyethylene terephthalate and polyethylene naphthalate Cellulose polymers such as diacetyl cellulose and triacetyl cellulose, polycarbonate polymers, acrylic polymers such as polymethyl methacrylate, styrene polymers such as polystyrene and acrylonitrile / styrene copolymers, polyethylene, polypropylene, and cyclic or norbornene structures Polyolefins, olefin polymers such as ethylene / propylene copolymers, vinyl chloride polymers, amide polymers such as aromatic polyamides, imide polymers, Ruphone polymer, polyether sulfone polymer, polyether ether ketone polymer, polyphenylene sulfide polymer, vinyl alcohol polymer, vinylidene chloride polymer, vinyl butyral polymer, arylate polymer, polyoxymethylene polymer, epoxy polymer Furthermore, the sheet | seat or film which consists of transparent polymers, such as these binary-type, ternary-type various copolymers, a graft copolymer, and a blend, is mentioned. In particular, a polyester biaxially oriented film such as polyethylene terephthalate, polybutylene terephthalate, or polyethylene-2,6-naphthalate is preferable in terms of mechanical properties, optical properties, heat resistance, and economy. The polyester biaxially oriented film may be a copolyester.

6). Preparation and application method of infrared shielding film-forming coating material The infrared shielding film-forming coating material of the present invention is prepared, for example, by dispersing the above-mentioned composite tungsten oxide fine particles in a solvent, adding the above-mentioned surfactant thereto, and further adding a binder resin. It can be prepared by dissolving and mixing. Also, the infrared shielding film is formed by applying the prepared coating material for forming an infrared shielding film to the surface of a transparent substrate such as a resin film, and evaporating the solvent of the applied coating material and curing the binder resin by a predetermined method. Can be formed.

  The coating method for forming the infrared shielding film may be any method as long as the coating material can be uniformly applied to the surface of the transparent substrate such as a resin film. For example, the bar coating method, the gravure roll coating method, the reverse roll coating Method, dip coating method, blade coating method, air knife coating method, wire block coating method, reblocks coating method, reblocking roll coating method, extrusion coating method, rod coating method, wire bar coating method, slide coating method and curtain Examples thereof include a coating method.

7). Infrared shielding body The infrared shielding body of the present invention is obtained by coating the coating material for forming the infrared shielding film on the surface of a transparent substrate such as a resin film, and forming the formed coating film into a plate shape, a film shape, or a thin film shape. The infrared shielding film and the transparent substrate.

  The infrared shielding body of the present invention is free of coating film defects due to repellency, removal, coating unevenness, etc. of the coating material for forming an infrared shielding film, and has a precise in-plane uniformity. Is transparent and has excellent shielding properties in the near infrared region. Therefore, it can be suitably used as an optical filter or the like that requires a function of absorbing near infrared rays.

  Examples of the present invention will be specifically described below.

  In addition, the optical measurement in each Example and the comparative example 1 calculates based on the film for architectural window glass JISA 5759 (1998) (light source: A light), calculates visible light transmittance, and a haze value is based on JISK7105. Based on the measurement. In addition, the average dispersed particle diameter was an average value measured by a measuring device using a dynamic light scattering method (ELS-800 manufactured by Otsuka Electronics Co., Ltd.). The optical properties of a PET film having a thickness of 50 μm, which is a transparent substrate, have a visible light transmittance of 90% and a haze of 0.9%.

8 parts by weight of a composite tungsten oxide powder represented by Cs _0.33 WO ₃ and having a hexagonal crystal structure, 84 parts by weight of toluene, and 8 parts by weight of a dispersant are mixed and subjected to dispersion treatment to obtain an average dispersion A dispersion liquid (A liquid) having a particle diameter of 80 nm was obtained.

  100 parts by weight of this liquid A, 50 parts by weight of an ultraviolet curable resin for hard coat [manufactured by Toagosei Co., Ltd., trade name UV3701], and a silicone-based surfactant represented by the above chemical formula (1) (manufactured by Nihon Unicar) , Trade name: FZ-2164) 0.05 part by weight was mixed to prepare a coating material for forming an infrared shielding film according to Example 1.

  Next, the infrared shielding film-forming paint according to Example 1 was applied onto a PET film (thickness: 50 μm) using a roll coater to form a coating film.

  The coating film was dried at 80 ° C. for 60 seconds to evaporate the solvent, and then cured with a high-pressure mercury lamp to form an infrared shielding film. An infrared shielding film (infrared ray) composed of the infrared shielding film and a PET film. A shield was obtained.

  The surface of the infrared shielding film was visually observed and judged according to the following evaluation criteria.

[Crossing unevenness]
○: Not at all. Δ: Partially confirmed. X: It can be confirmed clearly.

[Nuke (with or without pinholes with a diameter of 1 to 3 mm)]
○: The number of leakage is 5 / m ² or less. Δ: Less than 50 / m ² . X: 50 pieces / m ² or more.

  And when the optical characteristic of the infrared shielding film which concerns on Example 1 was measured, the visible light transmittance | permeability was 70% and it was confirmed that the light of visible region is fully permeate | transmitted. Moreover, haze was 0.8% and showed the outstanding transparency.

  The haze of the infrared shielding film (infrared shielding body) is slightly lower than the haze of the PET film because of the easy adhesion treatment (primer and corona) for improving the adhesion of the coating film to the PET film surface. The haze is generated by surface scattering due to slight unevenness on the surface of the PET film, and the haze of the PET film is 0.9%. When the film is formed, the unevenness of the film surface is filled and smoothed, so the haze of the infrared shielding film (infrared shielding body) is considered to be 0.8%.

  Furthermore, when the infrared shielding film obtained according to the said evaluation criteria was determined, the crossing unevenness was not seen ((circle)), there were few leaks ((circle)), and the favorable applicability | paintability was exhibited.

  100 parts by weight of the above-mentioned A liquid, 50 parts by weight of UV curable resin for hard coat [manufactured by Toagosei Co., Ltd., trade name UV3701], and the above-mentioned silicone surfactant (manufactured by Nihon Unicar, trade name: FZ-2164) ) 0.0016 part by weight was mixed to prepare the infrared shielding film forming paint according to Example 2.

  Next, the coating material for forming an infrared shielding film according to Example 2 was applied onto a PET film (thickness: 50 μm) using a roll coater to form a coating film.

  The coating film was dried at 80 ° C. for 60 seconds to evaporate the solvent, and then cured with a high-pressure mercury lamp to form an infrared shielding film. An infrared shielding film (infrared ray) composed of the infrared shielding film and a PET film. A shield was obtained.

  Next, when the optical characteristic of the infrared shielding film according to Example 2 was measured, the visible light transmittance was 71%, and it was confirmed that the light in the visible light region was sufficiently transmitted. Moreover, haze was 0.8% and showed the outstanding transparency.

  Furthermore, when the infrared shielding film obtained according to the said evaluation criteria was determined, the crossing unevenness was not seen ((circle)), there were few leaks ((circle)), and the favorable applicability | paintability was exhibited.

  100 parts by weight of the above-mentioned A liquid, 50 parts by weight of UV curable resin for hard coat [manufactured by Toagosei Co., Ltd., trade name UV3701], and the above-mentioned silicone surfactant (manufactured by Nihon Unicar, trade name: FZ-2164) ) 16 parts by weight were mixed to prepare an infrared shielding film forming paint according to Example 3.

  Next, the coating material for forming an infrared shielding film according to Example 3 was applied onto a PET film (50 μm thickness) using a roll coater to form a coating film.

  The coating film was dried at 80 ° C. for 60 seconds to evaporate the solvent, and then cured with a high-pressure mercury lamp to form an infrared shielding film. An infrared shielding film (infrared ray) composed of the infrared shielding film and a PET film. A shield was obtained.

  Next, when the optical characteristic of the infrared shielding film according to Example 3 was measured, the visible light transmittance was 71%, and it was confirmed that the light in the visible light region was sufficiently transmitted. Moreover, the haze was 1.0%, indicating excellent transparency.

Furthermore, when the infrared shielding film obtained according to the above-mentioned evaluation criteria was judged, transverse unevenness was partially observed (Δ), but there was little missing (Δ) and a relatively good coating property was exhibited.
[Comparative Example 1]
100 parts by weight of the above liquid A and 50 parts by weight of UV curable resin for hard coat [manufactured by Toagosei Co., Ltd., trade name UV3701] were mixed to prepare an infrared shielding film forming paint according to Comparative Example 1. .

  Next, the infrared shielding film-forming paint according to Comparative Example 1 was applied onto a PET film (50 μm thick) using a roll coater to form a coating film.

  The coating film was dried at 80 ° C. for 60 seconds to evaporate the solvent, and then cured with a high-pressure mercury lamp to form an infrared shielding film. An infrared shielding film (infrared ray) composed of the infrared shielding film and a PET film. A shield was obtained.

  Next, when the optical characteristic of the infrared shielding film according to Comparative Example 1 was measured, the visible light transmittance was 71%, and it was confirmed that the light in the visible light region was sufficiently transmitted. Moreover, haze was 0.8% and showed the outstanding transparency.

  However, when the infrared shielding film obtained according to the above evaluation criteria was determined, transverse unevenness was clearly observed (×), there were many spots (×), and the applicability was poor.

  100 parts by weight of the above-mentioned A liquid, 50 parts by weight of UV curable resin for hard coat [manufactured by Toagosei Co., Ltd., trade name UV3701], and the above-mentioned silicone surfactant (manufactured by Nihon Unicar, trade name: FZ-2164) ) 0.0008 part by weight was mixed to prepare the infrared shielding film forming paint according to Example 4.

  Next, the coating material for forming an infrared shielding film according to Example 4 was applied onto a PET film (thickness: 50 μm) using a roll coater to form a coating film.

  The coating film was dried at 80 ° C. for 60 seconds to evaporate the solvent, and then cured with a high-pressure mercury lamp to form an infrared shielding film. An infrared shielding film (infrared ray) composed of the infrared shielding film and a PET film. A shield was obtained.

  Next, when the optical characteristic of the infrared shielding film according to Example 4 was measured, the visible light transmittance was 71%, and it was confirmed that the light in the visible light region was sufficiently transmitted. Moreover, haze was 0.8% and showed the outstanding transparency.

  Furthermore, when the infrared shielding film obtained according to the above-mentioned evaluation criteria was determined, the crossing unevenness was improved from Comparative Example 1 (Δ), but there was a little more missing (Δ close to x) compared to other examples. The applicability was slightly inferior.

  100 parts by weight of the above-mentioned A liquid, 50 parts by weight of UV curable resin for hard coat [manufactured by Toagosei Co., Ltd., trade name UV3701], and the above-mentioned silicone surfactant (manufactured by Nihon Unicar, trade name: FZ-2164) ) 26 parts by weight were mixed to prepare an infrared shielding film forming paint according to Example 5.

  Next, the coating material for forming an infrared shielding film according to Example 5 was applied onto a PET film (thickness: 50 μm) using a roll coater to form a coating film.

  The coating film was dried at 80 ° C. for 60 seconds to evaporate the solvent, and then cured with a high-pressure mercury lamp to form an infrared shielding film. An infrared shielding film (infrared ray) composed of the infrared shielding film and a PET film. A shield was obtained.

  Next, when the optical characteristic of the infrared shielding film according to Example 5 was measured, the visible light transmittance was 71%, and it was confirmed that the light in the visible light region was sufficiently transmitted. However, the haze was as high as 2.0%, which was slightly poor compared to the other examples.

  Furthermore, when the infrared shielding film obtained according to the above-mentioned evaluation criteria was determined, the crossing unevenness was improved from Comparative Example 1 (Δ), but there was a little more missing (Δ close to x) compared to other examples. The applicability was slightly inferior.

  The infrared shielding body composed of the infrared shielding film formed using the infrared shielding film forming paint according to the present invention and a transparent substrate has a precise in-plane uniformity and is transparent in the visible light region. In the near infrared region, it has excellent shielding properties. Therefore, the infrared shielding body obtained by using the coating material for forming an infrared shielding film according to the present invention is an industry used for optical filters and window materials that transmit light in the visible light region and shield light in the near infrared region. Has the above applicability.

Claims (7)

General formula M _Y WO _Z (where M is H, He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo , Ta, Re, Be, Hf, Os, Bi, I, one or more elements, W is tungsten, O is oxygen, and 0.001 ≦ Y ≦ 1.0, 2.2 ≦ Infrared shielding film formation characterized in that composite tungsten oxide fine particles represented by Z ≦ 3.0) and having a hexagonal crystal structure, a surfactant and a binder resin are dispersed or dissolved in a solvent Paint.   The infrared shielding film-forming coating material according to claim 1, wherein the content of the surfactant is 0.001 to 10 parts by weight when the entire coating material is 100 parts by weight.   3. The infrared shielding film forming paint according to claim 1, wherein the composite tungsten oxide fine particles are fine particles of composite tungsten oxide having a particle diameter of 1 nm to 800 nm.   2. The infrared shielding film-forming coating material according to claim 1, wherein the surfactant is at least one selected from a cation, an anion, both ions, or a nonionic surfactant.   The infrared shielding material according to claim 4, wherein the nonionic surfactant is a silicone surfactant composed of a silicone compound in which a hydrophobic group is dimethylpolysiloxane and a hydrophilic group is polyalkylene oxide. Film forming paint. 6. The infrared shielding film-forming paint according to claim 5, wherein the silicone-based surfactant is at least one selected from the following chemical formulas (1) to (6).

[In the chemical formulas (1) to (6), R represents an alkyl group or hydrogen, R ′ represents an alkylene group, a and b are each an integer of 1 to 500, and m and n are 1 respectively. It is an integer of ~ 200. ]   An infrared shielding film formed by coating the coating material for forming an infrared shielding film according to any one of claims 1 to 6 on a surface of a transparent substrate, and forming the formed coating film into a plate shape, a film shape, or a thin film shape. And an infrared shielding body comprising the transparent substrate.