CN111960690A - High-dispersity tin antimony oxide high-molecular film and preparation method thereof - Google Patents
High-dispersity tin antimony oxide high-molecular film and preparation method thereof Download PDFInfo
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- CN111960690A CN111960690A CN202010660801.6A CN202010660801A CN111960690A CN 111960690 A CN111960690 A CN 111960690A CN 202010660801 A CN202010660801 A CN 202010660801A CN 111960690 A CN111960690 A CN 111960690A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
- C03C2217/445—Organic continuous phases
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
- C03C2217/475—Inorganic materials
- C03C2217/476—Tin oxide or doped tin oxide
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
- C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer
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Abstract
The invention discloses a high-dispersity tin antimony oxide high-molecular film and a preparation method thereof, wherein the film comprises a polyvinyl alcohol high-molecular film and tin antimony oxide nano-particles uniformly dispersed in the film, and the preparation method of the film comprises the following steps: (1) synthesizing tin antimony oxide powder, and dispersing the tin antimony oxide powder in water to obtain tin antimony oxide dispersion liquid; (2) adding polyvinyl alcohol powder into water, and heating until the polyvinyl alcohol powder is completely dissolved to obtain a polyvinyl alcohol solution; (3) and adding the tin antimony oxide dispersion liquid into the polyvinyl alcohol solution, uniformly mixing, and coating on a substrate to obtain the tin antimony oxide polymer film. The film has high light transmission and high dispersibility, high visible light transmission, high ultraviolet light absorption rate and high infrared light reflectivity, can be applied to Low-E glass as a coating film, and has the advantages of simple preparation method, high yield, good repeatability and no secondary pollution.
Description
Technical Field
The invention relates to a high polymer film and a preparation method thereof, in particular to a high-dispersity tin antimony oxide high polymer film and a preparation method thereof.
Background
Glass is an important building material, and with the increasing requirements on the decoration of buildings, the usage amount of glass in the building industry is also increasing. Low-E glass is also called Low-emissivity glass, and is a film product formed by plating a plurality of layers of metal or other compounds on the surface of the glass. The coating layer has the characteristics of high visible light transmission and high mid-far infrared ray reflection, so that compared with common glass and traditional coating glass for buildings, the coating layer has excellent heat insulation effect and good light transmission, and the common coating materials at present comprise indium tin oxide, silver materials and the like, but the coating layer has higher cost and poor stability, and the application of the coating layer in the coating glass is limited.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a high-dispersity tin antimony oxide high-molecular film which is simple in preparation process, high in yield, good in repeatability, environment-friendly and high in light transmittance.
The technical scheme is as follows: the high-dispersity tin antimony oxide high-molecular film comprises a polyvinyl alcohol high-molecular film and tin antimony oxide nano-particles uniformly dispersed in the film.
Wherein the unit area is 5 × 5cm21-300 mg of tin antimony oxide nanoparticles are dispersed on the film.
The preparation method of the high-dispersity tin antimony oxide high-molecular film comprises the following steps:
(1) synthesizing tin antimony oxide powder, and dispersing the tin antimony oxide powder in water to obtain tin antimony oxide dispersion liquid;
(2) adding polyvinyl alcohol powder into water, and heating until the polyvinyl alcohol powder is completely dissolved to obtain a polyvinyl alcohol solution;
(3) and adding the tin antimony oxide dispersion liquid into the polyvinyl alcohol solution, uniformly mixing, and coating on a substrate to obtain the tin antimony oxide polymer film.
Wherein, the synthesis of the tin antimony oxide powder in the step 1 comprises the following steps:
(11) mixing tin particles and antimony trioxide powder, adding sulfuric acid, and heating and stirring in an oil bath;
(12) after the reaction is finished, placing the mixture into an ice-water bath, adding hydrogen peroxide and water, and carrying out hydrothermal reaction;
(13) and after the reaction is finished, carrying out solid separation, drying and grinding to obtain the tin antimony oxide powder.
In the step 11, the mass ratio of the tin particles to the antimony trioxide is 1: 0.2-0.5, wherein the mass of tin particles and the volume ratio of sulfuric acid is 1 g: 5-10 mL, wherein the volume ratio of the mass of the tin particles to the volume of hydrogen peroxide in the step 12 is 1 g: 20-50 mL, wherein the mass-to-volume ratio of tin particles to water is 1 g: 13-35 mL, and the hydrothermal reaction temperature is 150-200 ℃.
Wherein, triethylamine with the volume fraction of 1-10% is added when the tin antimony oxide powder is dissolved in water in the step 1, the mass fraction of the tin antimony oxide powder in the tin antimony oxide solution is 10 g/L-300 g/L, the heating temperature in the step 2 is 70-97 ℃, the concentration of the prepared polyvinyl alcohol solution is 40-60g/L, and the volume ratio of the tin oxide solution to the polyvinyl alcohol solution in the step 3 is 2: 1 to 4.
The synthesis mechanism is as follows: after the tin antimony oxide dispersion liquid and the polyvinyl alcohol solution are mixed, the polyvinyl alcohol is adsorbed on tin antimony oxide nano particles through static electricity, strong steric hindrance repulsion force is generated, acting force between the tin antimony oxide nano particles is reduced, the tin antimony oxide nano particles are more stable and are not easy to aggregate, agglomeration of the nano particles is avoided, the tin antimony oxide nano particles are uniformly dispersed in the polyvinyl alcohol solution, after the film is formed on the substrate, the tin antimony oxide nano particles are uniformly distributed on the polyvinyl alcohol film, and the tin antimony oxide nano particles do not generate agglomeration phenomenon, so that visible light can easily transmit, the film has high transmittance, the uniform tin antimony oxide nano particles can also absorb and reflect infrared light and ultraviolet light, and Low-E glass can be obtained by coating a tin antimony oxide polymer film on a glass substrate, so that the transmission of ultraviolet light and infrared light is blocked.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: 1. the tin antimony oxide high-molecular film has high light transmittance and high dispersibility, has high visible light transmittance, high ultraviolet light absorption rate and high infrared light reflectivity, and can be applied to Low-E glass as a coating film; 2. the preparation method is simple, high in yield and good in repeatability; 3. no secondary pollution is generated.
Drawings
FIG. 1 is a scanning electron microscope photograph of a tin antimony oxide polymer film in example 1;
FIG. 2 is a high transmission electron micrograph of a tin antimony oxide polymer film of example 1;
FIG. 3 is an X-ray diffraction pattern of the tin antimony oxide polymer film, tin antimony oxide powder and polyvinyl alcohol film of example 1;
FIG. 4 is an absorption curve of ultraviolet/visible/infrared for Low-E glass and ordinary glass in examples 1 to 3;
FIG. 5 is a graph showing the transmittance of ultraviolet/visible/infrared rays of Low-E glass and ordinary glass in examples 1 to 3;
FIG. 6 is a graph showing the UV/visible/IR reflectance curves of the Low-E glass and the common glass of examples 1 to 3.
Detailed Description
Example 1
(1) Preparation of tin antimony oxide Dispersion
Firstly weighing 1g of tin particles and 0.2g of antimony trioxide powder, placing the tin particles and the antimony trioxide powder into a 100mL three-neck flask, then adding 8mL of sulfuric acid into the three-neck flask, heating and stirring the mixture for 48 hours at 95 ℃, after the heating and stirring are completed, placing the three-neck flask into an ice water bath, slowly dropwise adding 32mL of hydrogen peroxide into the three-neck flask, after 20 minutes, adding 24mL of ultrapure water into the ice water bath under stirring, finally transferring the mixed solution into a hydrothermal reaction kettle, reacting the mixed solution for 10 hours at 160 ℃, centrifugally separating the mixed solution after the reaction is completed, drying the obtained solid, and grinding the solid into powder to obtain the antimony oxide powder; putting 25mg of tin antimony oxide powder into 450 mu L of ultrapure water, then adding 50 mu L of triethylamine into the ultrapure water, and dispersing the tin antimony oxide into the ultrapure water after violent shaking to obtain a tin antimony oxide dispersion liquid;
(2) weighing 5g of polyvinyl alcohol, dissolving the polyvinyl alcohol in 95mL of ultrapure water, heating and stirring the polyvinyl alcohol for 2h at the temperature of 80 ℃, completely mixing to obtain a polyvinyl alcohol solution, and placing the polyvinyl alcohol solution at normal temperature for later use.
(3) Synthetic tin antimony oxide high molecular film
Adding 500 mu L of polyvinyl alcohol solution into the tin antimony oxide dispersion liquid, oscillating for 30min, uniformly coating the mixed solution on a target 5 x 5cm glass sheet, and drying at room temperature for 24h to obtain a tin antimony oxide polymer film deposited on the glass sheet, wherein the obtained glass is the tin antimony oxide coated Low-E glass. It can be seen from fig. 1(a) that the thin film has an obvious lamellar structure, and it can be seen from fig. 1(b) that the circle marked part on the tin antimony oxide nano polymer film has the uniformly dispersed tin antimony oxide particles deposited, which proves that the tin antimony oxide nanoparticles are uniformly dispersed on the nano polymer film, and it can be seen from fig. 2(a) and fig. 2(b) that the regular lattice stripes of the tin antimony oxide nanoparticles can be seen in the high power transmission diagram, and they are uniformly distributed in the whole system in a net shape, which shows that the tin antimony oxide is highly dispersed in the polymer film, and it can be seen from fig. 3 that the characteristic peaks of polyvinyl alcohol and tin antimony oxide can be observed on the tin antimony oxide nano polymer film, which shows that the synthesis of the tin antimony oxide nano polymer film does not affect the structures of the tin antimony oxide and the polyvinyl alcohol film.
Example 2
The difference between this example and example 1 is: the volume of antimony trioxide powder is 0.5g, the volume of sulfuric acid is 10mL, the volume of hydrogen peroxide is 50mL, and the volume of ultrapure water is 35mL when preparing the tin oxide antimony powder, the mass of the tin oxide antimony powder is 10mg, the volume of the ultrapure water is 480 muL, and the volume of triethylamine is 20 muL when preparing the tin oxide antimony dispersion liquid.
Example 3
The difference between this example and example 1 is: the volume of sulfuric acid is 5mL, hydrogen peroxide is 20mL, ultrapure water is 13mL when preparing the tin antimony oxide powder, the mass of the tin antimony oxide powder is 5mg when preparing the tin antimony oxide dispersion liquid, the volume of the ultrapure water is 490 mu L, and the volume of triethylamine is 10 mu L.
Example 4
The difference between this example and example 1 is: the polyvinyl alcohol solution used in the synthesis of the tin antimony oxide polymer film was 250. mu.L.
Example 5
The difference between this example and example 1 is: the polyvinyl alcohol solution used in the synthesis of the tin antimony oxide polymer film was 1000. mu.L.
Example 6
The difference between this example and example 1 is: triethylamine was not used in the preparation of the tin antimony oxide dispersion.
Example 7
The difference between this example and example 1 is: the mass of the tin antimony oxide powder when preparing the tin antimony oxide dispersion was 150 mg.
Comparative example
The difference between this example and example 1 is: without preparing tin antimony oxide nano-particles, 5g of polyvinyl alcohol and 500 mu L of ultrapure water are used for directly synthesizing pure polyvinyl alcohol polymer film
It can be seen from fig. 4 to 6 that compared with the common glass coated with the polyvinyl alcohol film, the tin antimony oxide coated Low-E glass has better absorption and reflection effects on ultraviolet light and infrared light, and has little influence on visible transmission. And with the increase of the quantity of tin oxide antimony, the absorption and reflection effects of the Low-E glass on ultraviolet light and infrared light are enhanced, and the influence on the transmittance of visible light is small, which proves that the tin oxide antimony coated Low-E glass has good Low-radiation performance.
Claims (9)
1. The high-dispersity tin antimony oxide high-molecular film is characterized by comprising a polyvinyl alcohol high-molecular film and tin antimony oxide nanoparticles dispersed in the film.
2. The highly dispersible tin antimony oxide polymer film as claimed in claim 1, wherein the thickness per unit area is 5X 5cm25-150 mg of tin antimony oxide nanoparticles are dispersed on the filmAnd (4) granulating.
3. The preparation method of the high-dispersity tin antimony oxide high-molecular film according to claim 1 is characterized by comprising the following steps of:
(1) synthesizing tin antimony oxide powder, and dispersing the tin antimony oxide powder in water to obtain tin antimony oxide dispersion liquid;
(2) adding polyvinyl alcohol powder into water, and heating until the polyvinyl alcohol powder is completely dissolved to obtain a polyvinyl alcohol solution;
(3) and adding the tin antimony oxide dispersion liquid into the polyvinyl alcohol solution, uniformly mixing, and coating on a substrate to obtain the tin antimony oxide polymer film.
4. The method for preparing the highly dispersible tin antimony oxide polymer film according to claim 3, wherein the step 1 of synthesizing tin antimony oxide powder comprises the following steps:
(11) mixing tin particles and antimony trioxide powder, adding sulfuric acid, and heating and stirring in an oil bath;
(12) after the reaction is finished, placing the mixture into an ice-water bath, adding hydrogen peroxide and water, and carrying out hydrothermal reaction;
(13) and after the reaction is finished, carrying out solid separation, drying and grinding to obtain the tin antimony oxide powder.
5. The method for preparing a highly dispersible tin antimony oxide polymer film according to claim 4, wherein the mass ratio of the tin particles to the antimony trioxide in the step 11 is 1: 0.2-0.5, wherein the mass of the tin particles and the volume ratio of sulfuric acid is 1 g: 5-10 mL.
6. The method for preparing the high-dispersity tin antimony oxide high-molecular film according to claim 4, wherein the volume ratio of tin particles to hydrogen peroxide in the step 12 is 1 g: 20-50 mL, wherein the mass-to-volume ratio of tin particles to water is 1 g: 13-35 mL, and the hydrothermal reaction temperature is 150-200 ℃.
7. The method for preparing a highly dispersible tin antimony oxide polymer film according to claim 3, wherein triethylamine is added in a volume fraction of 1-10% during the preparation of the tin antimony oxide dispersion in step 1, and the concentration of tin antimony oxide in the tin antimony oxide dispersion is 10 g/L-300 g/L.
8. The method for preparing a highly dispersible tin antimony oxide polymer film according to claim 3, wherein the heating temperature in step 2 is 70-97 ℃, and the concentration of the prepared polyvinyl alcohol solution is 40-60 g/L.
9. The method for preparing a highly dispersible tin antimony oxide polymer film according to claim 3, wherein the volume ratio of the tin antimony oxide dispersion to the polyvinyl alcohol solution in step 3 is 2: 1 to 4.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113999407A (en) * | 2021-11-18 | 2022-02-01 | 江苏科技大学 | Temperature-sensitive intelligent Low-E glass and preparation method and application thereof |
EP4375317A1 (en) * | 2022-11-25 | 2024-05-29 | ETH Zurich | Heating device for de-misting or anti-misting devices such as vehicle lightings |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113999407A (en) * | 2021-11-18 | 2022-02-01 | 江苏科技大学 | Temperature-sensitive intelligent Low-E glass and preparation method and application thereof |
EP4375317A1 (en) * | 2022-11-25 | 2024-05-29 | ETH Zurich | Heating device for de-misting or anti-misting devices such as vehicle lightings |
WO2024110669A1 (en) * | 2022-11-25 | 2024-05-30 | Eth Zurich | Heating device for de-misting or anti-misting devices such as vehicle lightings |
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