KR20130083422A - Synthetic method of near infrared radiation shielding metal oxide mixture - Google Patents

Synthetic method of near infrared radiation shielding metal oxide mixture Download PDF

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KR20130083422A
KR20130083422A KR1020130076792A KR20130076792A KR20130083422A KR 20130083422 A KR20130083422 A KR 20130083422A KR 1020130076792 A KR1020130076792 A KR 1020130076792A KR 20130076792 A KR20130076792 A KR 20130076792A KR 20130083422 A KR20130083422 A KR 20130083422A
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aluminum oxide
cobalt aluminum
infrared
infrared ray
metal oxide
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KR1020130076792A
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Korean (ko)
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이동훈
고광용
박명성
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(주) 테크포엠
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/62—Metallic pigments or fillers
    • C09C1/622—Comminution, shaping or abrasion of initially uncoated particles, possibly in presence of grinding aids, abrasives or chemical treating or coating agents; Particle solidification from melted or vaporised metal; Classification
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/22—Absorbing filters
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/30—Three-dimensional structures
    • C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

PURPOSE: A manufacturing method of a metal oxide mixture for shielding infrared ray is provided to show an effect to supplement the disadvantage of the existing infrared ray shielding materials. CONSTITUTION: An infrared ray shielding material increases the infrared ray absorption efficiency by mixing cobalt aluminum oxide of a spinel structure in order to increase the effect of the existing metal oxide for shielding infrared ray. The cobalt aluminum oxide has a spinel structure. The infrared ray shielding material has a particle size of 1 μm or less in order to relieve the low visible ray permeability of cobalt aluminum oxide, and to increase the visible ray absorption efficiency. A manufacturing method of a mixture solution of cesium tungsten oxide and cobalt aluminum oxide, which shows the optimal infrared ray shielding performance. [Reference numerals] (AA) Transmittance; (BB) Wavelength (nm)

Description

Synthetic Method of Near Infrared Radiation Shielding Metal Oxide Mixture

The present invention relates to the production of a metal oxide mixture system which is excellent in transmittance and can only selectively shield infrared rays.

Metal oxide infrared shielding materials are widely applied to buildings, electronic film and automotive film. And unlike general organic and inorganic compound materials, not only has excellent high temperature characteristics and stability in the air, but also has the advantage of low denaturation against ultraviolet rays. These infrared shielding metal oxides are typically manufactured / used by atomizing to nano-sized to improve transmittance. In addition, when applied to the surface of the transparent film or glass mixed with an excellent material such as infrared shielding material and resin, it is effectively absorbed and shielded from the outside of the coating film and the infrared rays of the sunlight in the wavelength range of more than 900nm ultraviolet and infrared rays inside the coating film It has a general characteristic of suppressing the generation of heat and the transfer of heat energy by the transmission of.

For example, Patent Documents 1 and 2 are representative methods for showing infrared shielding efficiency as a material synthesized by adding various metal ions based on tungsten trioxide as the infrared shielding material using the most widely used metal oxide. However, these infrared shielding materials also do not effectively absorb / shield near-infrared regions with a wavelength of 900 to 1,500 nm, so that a large amount of wavelengths in the near-infrared region penetrate the infrared shielding coating surface to reduce the shielding efficiency. There is an urgent need for development.

In addition, Patent Document 3 discloses a transparent resin material having near-infrared absorptive performance as a series of tungsten chloride and tin chloride and as an absorbent, for example, a thiol complex of Patent Document 4, an anthraquinone derivative of Patent Document 5, and Patent Document 6 And squarylium compounds.

However, the organic near-infrared absorbent of the prior art has a difficulty in sustaining the effect due to its durability compared to the metal oxide type, the absorption efficiency of the near infrared in the series of tungsten chloride and tin chloride is excellent, but faded when left in a dark place for a long time There was a problem.

Therefore, the development and application of new shielding material, which is a key element, is technically important. Therefore, the degree to which the present invention is required is very large.

(Patent Document 0001) Republic of Korea 10-2011-0095315

(Patent Document 0002) Republic of Korea 10-2011-0099420

(Patent Document 0003) US Patent No. 3692688

(Patent Document 0004) Japanese Patent No. 60-21294

(Patent Document 0005) Japanese Patent No. 61-115985

(Patent Document 0006) Japanese Patent No. 61-218551

The problem to be solved by the present invention in consideration of the above problems is to prepare an infrared shielding metal oxide mixture to maintain the transmittance to visible light, while the infrared shielding effect in the near infrared region of the wavelength 900nm 1,500nm region significantly increased physical properties Eggplant is to provide an infrared shielding metal oxide mixture and a preparation method thereof.

In general, the most ideal infrared shielding coating material should have a high transmittance of visible light in the wavelength range of 300 nm to 900 nm. In addition, the wavelength of the infrared region (wavelength 900nm or more) must be effectively absorbed, and the synthesis method is simple.

As seen from the existing invention, tungsten trioxide is known to have excellent transmittance as an infrared shielding material and to absorb infrared wavelength of more than 1,500 nm. However, the near-infrared ray in the wavelength range of 900nm to 1,500nm shows a relatively gentle absorption peak, which is an improvement and is a technical problem to be overcome in the present invention.

In the present invention, while maintaining the transmittance to visible light, the ultimate goal to further increase the efficiency of the existing infrared shielding material by finding a metal oxide excellent in the absorption / shielding effect in the near infrared region of the wavelength 900nm to 1,500nm range.

As a material for overcoming these technical problems, there is a blue cobalt aluminum oxide having a spinel structure. The metal oxide mixture material showing excellent infrared shielding properties was prepared by maximizing near infrared absorption / shielding in the wavelength range of 900 nm to 1,500 nm, which is a disadvantage of the conventional infrared shielding material.

Through the present invention, cobalt aluminum oxide is mixed to improve the lack of near-infrared absorption efficiency in the wavelength range of 900 nm to 1,500 nm, which is a disadvantage of the conventional tungsten oxide-based infrared shielding material. It shows that the meaning of invention is large.

1 is an electron micrograph of infrared shielding metal oxide fine particles.
A is cesium tungsten metal oxide (CWO)
B is cobalt aluminum oxide (CAO)
2 is a UV-VIS-NIR transmission characteristic spectrum of cobalt aluminum oxide fine particles

3 is a UV-VIS-NIR transmission spectrum according to the composition ratio (CWO wt%: CAO wt%) of the cesium tungsten metal oxide (CWO) and cobalt aluminum oxide (CAO) mixture. A: CWO 100%, B: CWO 75%: CAO 25%, C: CWO 90%: CAO 10%.

The spinel-structured cobalt aluminum oxide (CAO) used in the present invention was mixed with cobalt carbonate and aluminum nitrate in an appropriate molar ratio to heat-treat at high temperature in air to synthesize blue particles. The spinel structure was identified by X-ray diffraction analysis.

The cobalt aluminum oxide thus prepared was subjected to atomization for 48 hours using a ball mill with isopropyl alcohol (IPA) as a solvent to obtain particles having a particle size near 100 nm as shown in FIG. And finally, it was prepared as a dispersion having a concentration of 10wt%.

In addition, tungsten trioxide and cesium chloride were mixed in an appropriate amount and subjected to high temperature heat treatment under reducing conditions to obtain cesium tungsten oxide (CWO). The mixed metal oxide was atomized using a ball mill to obtain particles near a particle size of 100 nm as in B of FIG. 1, and finally a dispersion having a concentration of 10 wt% was prepared.

Pure 10wt% -cobalt aluminum oxide dispersion was dip coated on the surface of PET film, dried and UV-VIS-NIR spectrum was obtained. As shown in the spectrum of FIG. 2, it can be seen that visible light in the wavelength range of 500 nm to 700 nm is absorbed, indicating a slight decrease in transmittance. However, near-infrared radiation in the wavelength range of 900 nm to 1500 nm shows some absorbing spectra.

In the present invention, to maximize the near-infrared absorption / shielding efficiency in the region corresponding to the wavelength 900nm to 1,500nm to eliminate the disadvantages of the conventional metal oxide infrared shielding material to produce a new material with better performance, so the wavelength 900nm of cobalt aluminum oxide The observation of the near-infrared absorption spectrum in the 1,500nm region at was predicted to be a significant contributor to the increase of infrared shielding efficiency.

Pure 10wt% cesium tungsten oxide dispersion was dip coated on the surface of PET film to obtain UV-VIS-NIR spectrum as shown in FIG. As shown in the A spectrum of FIG. 3, the transmittance of the visible light region was high, and the infrared rays of 1,500 nm or more showed low transmittance, indicating that the infrared shielding rate was good. However, it was found that the near-infrared region with a wavelength of 900 nm and 1,500 nm was absorbed / shielded slowly so that near-infrared rays near visible light could not be efficiently absorbed / shielded.

The superior technical characteristics of the infrared shield absorbing material is to increase the infrared shielding efficiency in the near infrared region in the wavelength range of 900 nm to 1500 nm. Therefore, in order to find the optimal composition, a 10 wt% -cesium tungsten oxide dispersion and a 10 wt% cobalt aluminum oxide dispersion are used. Mixed solutions having a composition ratio of%: 0% (A), 90%: 10% (C), and 75%: 25% (B) were prepared, respectively. In addition, each of the UV-VIS-NIR spectra were coated / dried on a PET film using a dip coating method.

Improvement of Infrared Shielding Efficiency According to Cobalt Aluminum Oxide (CAO) Mixing Ratio with Spinel Structure at Each NIR Wavelength 10 wt % CWO 10 wt % CAO By wavelength  Infrared Shielding Efficiency Improvement %(standard Cesium tungsten oxide ; CWO ) 900 nm 1,100 nm 1,300 nm 1,500 nm 100 0 - - - - 90 10 30 48 61 69 75 25 15 25 32 37

The film coated with the mixed dispersion of cesium tungsten oxide and cobalt aluminum oxide showed a near infrared absorption peak in the wavelength range of 900 nm to 1,500 nm, showing excellent infrared shielding efficiency. As shown in C of FIG. 3, the film prepared with the mixed solution containing 10 wt% of cobalt aluminum oxide showed the best efficiency in the near infrared absorption in the wavelength range of 900 nm to 1500 nm. In addition, the absorption of visible light between cobalt aluminum oxide in the wavelength range of 500 nm to 700 nm is accompanied by a loss of transmittance, resulting in a decrease in transmittance reduction compared to a film coated with a mixed solution containing 25 wt% of cobalt aluminum oxide. Seems. Through this, it can be seen that the infrared shielding oxide mixed with an excessive amount of cobalt aluminum oxide having strong absorption of visible light shows rather poor characteristics.

Claims (4)

Infrared shielding material that increases the absorption of infrared rays by mixing spinel-structured cobalt aluminum oxide in order to increase the effect of conventional infrared shielding metal oxide. The cobalt aluminum oxide of claim 1 has a spinel structure, the infrared shielding material. An infrared shielding material having a particle size of 1 µm or less in order to solve the low self-transmittance of visible light of cobalt aluminum oxide and to increase the absorption efficiency of visible light. Method for preparing a mixed solution of cesium tungsten oxide and cobalt aluminum oxide showing an optimal infrared shielding performance.
KR1020130076792A 2013-07-02 2013-07-02 Synthetic method of near infrared radiation shielding metal oxide mixture KR20130083422A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018043955A1 (en) * 2016-08-29 2018-03-08 주식회사 엘엠에스 Optical article for near-infrared cut-off filter included in camera module and camera module near-infrared cut-off filter comprising same
CN108101531A (en) * 2017-12-15 2018-06-01 华南理工大学 A kind of composite spinelle material of high IR emissivity and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018043955A1 (en) * 2016-08-29 2018-03-08 주식회사 엘엠에스 Optical article for near-infrared cut-off filter included in camera module and camera module near-infrared cut-off filter comprising same
CN108101531A (en) * 2017-12-15 2018-06-01 华南理工大学 A kind of composite spinelle material of high IR emissivity and preparation method thereof

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