CN108948418B - Nanoparticle mixture and light-transmitting film - Google Patents
Nanoparticle mixture and light-transmitting film Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a nanoparticle mixture capable of shielding near infrared light and a light-transmitting film containing the nanoparticles. According to the invention, cesium tungstate nanoparticles and indium tin oxide nanoparticles with different doped tin contents are blended to obtain a nanoparticle mixture with a shielding waveband capable of covering the whole near-infrared waveband of 800-3000 nm, and the method has a wide application prospect in the field of building energy conservation.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a nano particle mixture capable of shielding near infrared light, which can be used for preparing a heat insulation window film for building energy conservation.
Background
In a building house, radiant energy of sunlight entering the room through a window is one of the most important causes of excessive indoor temperature in summer. In order to create a comfortable and good indoor environment, the use of refrigeration implementations such as air conditioning consumes a large amount of electrical energy; in addition to huge energy consumption, a large amount of carbon dioxide is discharged into the atmosphere, so that environmental problems such as greenhouse effect and the like become more serious and worse. At present, the building energy consumption occupies 30 percent of the total energy consumption of China, and is the top of various energy consumptions. Therefore, in order to alleviate the increasing energy consumption of buildings, more reasonable utilization of the radiant energy of sunlight is required.
In the solar spectrum, the energy of near-infrared light of 800 nm-3000 nm occupies about 50%, and if the building doors and windows can shield the radiation energy of near-infrared light wave bands while ensuring the visible light transmittance, the use of refrigeration facilities such as air conditioners and the like can be greatly reduced, and the effect of building energy conservation is achieved. The heat-insulating material is generally applied to doors and windows of buildings by doping nano particles capable of selectively absorbing near infrared light in a film, so that the doors and windows can absorb the near infrared light and ensure that the transmittance of visible light is not influenced. The present nanoparticles with selective near-infrared light absorption mainly comprise cesium tungstate nanoparticles (Cs)0.32WO3) And Indium Tin Oxide (ITO) nanoparticles. Although the two types of nanoparticles have high transmittance in visible light, the absorption ranges in the near infrared band are different: cs0.32WO3The nano particles mainly have stronger absorption in near infrared light of 800 nm-1500 nm wave bands, and have limited absorption capacity in the wave bands of 1500 nm-3000 nm; the ITO nano particles hardly absorb at the wave band of 800 nm-1500 nm, and the absorption effect is better at the wave band of 1500 nm-3000 nm. In conclusion, all things are Cs0.32WO3The nano particles and the ITO nano particles can not cover the whole near infrared wave band of 800 nm-3000 nm, and the heat insulation capability and the energy saving efficiency of the building doors and windows are restricted.
Disclosure of Invention
In order to solve the defect that the absorption range of the existing heat-insulating nano material in a near infrared band is narrow, the invention aims to provide a nano particle mixture capable of shielding near infrared light, wherein the nano particle mixture has strong absorption capacity in the whole near infrared band of 800-3000 nm and has the advantages of low material cost and the like.
The invention provides a nanoparticle mixture capable of shielding near infrared light, which comprises a first component, a second component, a third component, a fourth component, a fifth component, a sixth component and a seventh component;
the first component is cesium tungstate nano particles;
the second component is indium tin oxide nano particles, wherein the doping amount m of tin is more than or equal to 8.0 and less than or equal to 12.0 percent;
the third component is Indium Tin Oxide (ITO) nano particles, wherein the doping amount m of tin Sn is more than or equal to 6.0 and m is less than 8.0%;
the fourth component is Indium Tin Oxide (ITO) nano particles, wherein the doping amount m of tin Sn is more than or equal to 4.0 and m is less than 6.0%;
the fifth component is Indium Tin Oxide (ITO) nano particles, wherein the doping amount m of tin Sn is more than or equal to 3.0 and m is less than 4.0%;
the sixth component is Indium Tin Oxide (ITO) nano particles, wherein the doping amount m of tin Sn is more than or equal to 2.0 and m is less than 3.0%;
the seventh component is Indium Tin Oxide (ITO) nano particles, wherein the doping amount m of tin Sn is more than or equal to 0.5 and m is less than 2.0%.
As a better alternative to the above nanoparticle mixture, the cesium tungstate nanoparticles in the first component are constituted by Cs0.32WO3. The skilled person can select appropriate cesium tungstate nanoparticles according to the needs, wherein the proportion of Cs can also be adjusted according to the needs, for example, a doping proportion of 0.25-0.4 is selected.
As a better choice of the nanoparticle mixture, the particle diameters of the cesium tungstate nanoparticles, the first component, the second component, the third component, the fourth component, the fifth component, the sixth component and the seventh component are all between 5nm and 20 nm.
As a better choice of the above nanoparticle mixture, the nanoparticle mixture comprises 15-40 parts by weight of a first component, 10-60 parts by weight of a second component, 1-10 parts by weight of a third component, 5-25 parts by weight of a fourth component, 1-20 parts by weight of a fifth component, 1-8 parts by weight of a sixth component and 1-5 parts by weight of a seventh component. According to the invention, the ITO particles with different maximum absorption peak positions are introduced, so that the nano particles can have the capability of absorbing infrared light in different wavelength ranges.
The invention can select the existing cesium tungstate nano-particles, wherein the proportion of Cs can select the doping proportion of 0.25-0.4, and the skilled person in the art can also select the following method to prepare the cesium tungstate nano-particles:
dissolving tungsten carbonyl and an oxidant in an organic solvent, uniformly mixing to obtain a mixed solution, heating the mixed solution to 150-180 ℃ under the protection of protective gas, adding an octadecene solution of cesium oleate, heating to 250-300 ℃ for reaction for 0.5-48 hours, and cooling and post-treating the obtained reaction solution to obtain cesium tungstate nanoparticles.
As a more preferable alternative to the above method, the octadecene solution of cesium oleate is added when the mixed solution becomes colorless.
As a better alternative of the method, the temperature reduction process is to place the container in which the reaction solution is placed in an ice-water mixture to be rapidly cooled to room temperature. The room temperature is 20-30 ℃. In the course of temperature reduction, the reaction taking place in the reaction system is quenched.
As a better choice of the method, the post-treatment is to obtain the cesium tungstate nano particles by centrifuging and washing the reaction liquid after cooling.
As a better alternative to the above method, the mass ratio of the tungsten carbonyl to the oxidizing agent is 3.53: 6.65.
as a better choice of the technical scheme, the atomic molar ratio of tungsten to cesium in the raw materials for preparing the cesium tungstate nanoparticles is 1: 0.32. When raw materials with different tungsten-cesium ratios are added for reaction, different products can be obtained.
As a better alternative to the above process, the oxidizing agent is Me3NO·2H2O。
As a better alternative to the above method, the organic solvent is oleylamine.
As a better alternative to the above method, the protective gas is an inert gas.
As a better alternative to the above process, the reaction time is from 2 to 5 hours.
As a better alternative to the above process, the reaction time is from 5 to 8 hours.
The reaction time can be adapted by the person skilled in the art as desired, and after reducing the concentration of tungsten carbonyls, the corresponding nucleation time will also be longer.
As a better choice of the method, the reaction temperature is 250-265 ℃.
As a better choice of the method, the reaction temperature is 265 ℃ and 280 ℃.
As a better choice of the method, the reaction temperature is 280-300 ℃.
The skilled person can adapt the reaction temperature according to the needs, and after increasing the reaction temperature, the corresponding particle size of the product will also increase accordingly.
As a better alternative of the method, the concentration of the tungsten carbonyl in the mixed solution is 0.01-0.03 g/mL. Smaller concentrations can be used to prepare cesium tungstate nanoparticles having smaller particle sizes. The mixed solution with the concentration range can prepare cesium tungstate particles with the particle size of 4-12 nm.
As a better choice of the method, the concentration of the tungsten carbonyl in the mixed solution is 0.03-0.05 g/mL. Smaller concentrations can be used to prepare cesium tungstate nanoparticles having smaller particle sizes. The mixed solution with the concentration range can prepare cesium tungstate particles with the particle size of 12-20 nm.
As a better alternative of the method, the concentration of the tungsten carbonyl in the mixed solution is 0.05-0.08 g/mL. The larger concentration can be used for preparing the cesium tungstate nano-particles with smaller particle size. The mixed solution with the concentration range can prepare cesium tungstate particles with the particle size of 18-30 nm.
The nano particle mixture has strong absorption capacity in the near infrared wave band of 800 nm-3000 nm, when the nano particle mixture is used as a heat insulation material and a building window film, 2g of the nano particle mixture is doped into a film with the thickness of 20 micrometers per square meter, and the shielding rate of the nano particle mixture on the near infrared light of 800 nm-3000 nm is not lower than 95%.
The invention also provides a light-transmitting film, wherein when the thickness of the light-transmitting film is calculated according to 20 micrometers, each square meter of the light-transmitting film is doped with 0.1-5g of the nanoparticle mixture.
As a further preferable mode of the light-transmitting film, the substrate of the light-transmitting film is a polymer. The specific polymer can be selected from a series of polymers such as PVC, PE, PP, PB, POM and the like.
As a further preferable aspect of the above light-transmitting film, the thickness of the light-transmitting film is not more than 20 μm. An excessively thick light-transmitting film may cause deterioration in light transmittance, bonding strength and application scenario, and a person skilled in the art may select an appropriate thickness.
As a further preferable aspect of the light-transmitting film, the content of the nanoparticle mixture in the light-transmitting film is 0.1 to 0.5%. The doping proportion can shield the larger part of near infrared light of 800nm to 3000 nm.
As a further preferable aspect of the light-transmitting film, the content of the nanoparticle mixture in the light-transmitting film is 0.5 to 1%. The doping proportion can shield most of near infrared light of 800nm to 3000 nm.
As a further preferable aspect of the light-transmitting film, the content of the nanoparticle mixture in the light-transmitting film is 1.0 to 1.5%. The doping proportion can shield most of near infrared light of 800nm to 3000 nm.
As a further preferable aspect of the light-transmitting film, the content of the nanoparticle mixture in the light-transmitting film is 1.5 to 2%. The doping proportion can shield more than 95% of near infrared light with 800 nm-3000 nm.
The invention utilizes the characteristic that cesium tungstate and indium tin oxide nanoparticles have different absorption capacities in different near-infrared light bands to blend the cesium tungstate nanoparticles and indium tin oxide nanoparticles with different tin doping amounts to obtain a nanoparticle mixture with an absorption range capable of covering the whole near-infrared light band of 800nm to 3000 nm. Compared with single cesium tungstate nanoparticles and single indium tin oxide nanoparticles, the nanoparticle mixture has the advantages of low cost, strong absorption capacity and wide absorption waveband range, and can play a wide role in the fields of building energy conservation and the like.
Drawings
Fig. 1 is an absorption spectrum of the obtained cesium tungstate nanoparticles;
FIG. 2 is an absorption spectrum of the resulting indium tin oxide nanoparticles doped with different tin contents;
FIG. 3 is a transmittance spectrum of a thermal barrier film doped with the nanoparticle mixture of example 1 in a wavelength band of 400nm to 3000 nm;
FIG. 4 is a transmittance spectrum of a thermal barrier film doped with the nanoparticle mixture of example 2 in a wavelength band of 400nm to 3000 nm;
FIG. 5 is a transmittance spectrum of a thermal barrier film doped with the nanoparticle mixture of example 3 in a wavelength band of 400nm to 3000 nm.
Detailed Description
The following examples are only for illustrating the technical solutions of the present invention, and are not intended to limit the scope of the present invention.
In the following examples, cesium tungstate nanoparticles and indium tin oxide nanoparticles with different tin-doped contents are provided by the laboratories of the institute of industry and technology of Beijing university for the intelligent and display functional materials, and the specific preparation method is as follows:
dissolving tungsten carbonyl and an oxidant in an organic solvent, uniformly mixing to obtain a mixed solution, heating the mixed solution to 150-180 ℃ under the protection of protective gas, adding an octadecene solution of cesium oleate, heating to 250-300 ℃ for reaction for 0.5-48 hours, and cooling and post-treating the obtained reaction solution to obtain cesium tungstate nanoparticles.
In the above method, the octadecene solution of cesium oleate is added when the mixed solution becomes colorless.
In the method, the temperature reduction process is to place the container in which the reaction solution is placed in an ice-water mixture to be rapidly cooled to room temperature. The room temperature is 20-30 ℃. In the course of temperature reduction, the reaction taking place in the reaction system is quenched.
In the method, the post-treatment is to obtain the cesium tungstate nano particles by centrifuging and washing the reaction liquid after cooling.
In the above method, the mass ratio of the tungsten carbonyl to the oxidizing agent may be 3.53: 6.65.
in the above method, the atomic molar ratio of tungsten and cesium in the raw material for preparing the cesium tungstate nanoparticles may be 1: 0.32.
In the above method, the oxidant is Me3NO·2H2O。
In the method, the organic solvent is oleylamine, the protective gas is inert gas, and the reaction time is 2-8 h.
In the above method, the reaction time should be prolonged after the concentration of tungsten carbonyl is reduced, and the nucleation time is also prolonged after the concentration of the reactant is reduced.
In the above method, the reaction temperature can be selected from 250-265 deg.C, 265-280 deg.C or 280-300 deg.C as required.
The skilled person can adapt the reaction temperature according to the needs, and after increasing the reaction temperature, the corresponding particle size of the product will also increase accordingly.
As a more preferable alternative to the above method, the concentration of tungsten carbonyl in the mixed solution is 0.01 to 0.03g/mL, 0.03 to 0.05g/mL, or 0.05 to 0.08 g/mL. The larger concentration can be used for preparing the cesium tungstate nano-particles with larger particle size. Selecting mixed solution with different concentration ranges can prepare cesium tungstate particles with the particle size of 5-30 nm.
The typical preparation method of the cesium tungstate nanoparticles comprises the following steps:
(1) to a 50mL four-necked round bottom flask was added 0.352g of tungsten carbonyl, 0.665g of oxidant, and 4mL of oleylamine;
(2) under the protection of inert gas, the solution in the step (1) is heated to 180 ℃, the solution turns yellow and then turns green during heating, and the solution turns colorless when the temperature reaches 180 ℃;
(3) at this point, 2.8mL of the prepared ammonium oleate octadecene solution was rapidly injected into the round bottom flask using a syringe and heating was continued to 290 ℃;
(4) after reacting for 3 hours, the reaction solution was placed in a container in which the reaction solution was placed in an ice-water mixture and rapidly cooled to room temperature, and the reaction was quenched to obtain a dark blue solution.
(5) Adding 10mL of ethanol into the solution to precipitate the nano particles, and centrifuging to obtain the cesium tungstate nano particles.
The preparation method of the indium tin oxide nano particle comprises the following steps:
300mg of indium acetylacetonate and an appropriate amount of tin acetylacetonate chloride were weighed into a round-bottomed flask, and 17ml of octadecene solvent was added and stirred uniformly with a magnet. Subsequently, the solution was heated to 250 ℃ under inert gas protection for 30min, then 1ml of oleic acid was added and the solution was immediately heated to 270 ℃ for 1 h. 3ml oleylamine were then added and the solution was immediately warmed to 290 ℃ and held for 1 h. After the reaction is finished, when the temperature of the solution is reduced to room temperature, 30ml of isopropanol is added to flocculate the nanoparticles. After the nanoparticles are separated by centrifugation, the prepared ITO nanoparticles coated with oleylamine oleic acid can be redispersed in 20.0ml of cyclohexane solvent.
The cesium tungstate and indium tin oxide nanoparticles can be used for obtaining more nanoparticle products at one time by expanding the feeding ratio of each component in the synthesis process.
The absorption spectra of cesium tungstate and nanoparticles doped with different tin contents are shown in fig. 1 and fig. 2, respectively.
In order to better characterize the effect of shielding near infrared light of the nanoparticles, the nanoparticle mixture in examples 1,2, and 3 is added to an ultraviolet polymerizable monomer to prepare a thermal insulation film added with nanoparticles, and the preparation process is specifically as follows:
(1) 2g of the nanoparticle mixture is added into 38g of ultraviolet polymerizable monomer, and the mixture is uniformly mixed. The composition of the uv-polymerizable monomers is shown in table 1.
TABLE 1 compounding ratio of each component of the polymerization monomers used in examples 1,2 and 3
| Name (R) | Ratio/%) |
| HPMA | 34.6 |
| LMA | 25.4 |
| Bis-EMA15 | 18.6 |
| PEGDA600 | 13.4 |
| 651 | 0.5 |
Wherein the HMPA (hydroxy methacrylate) structure is
LMA (Laureylmethacrylate) is
PEDGA600(Polyethylene glycol diacrylate) is
Bis-EMA15(Bisphenol a ethoxylate dimorphylate) is
The initiator 651(2,2-dimethoxy-1,2-diphenylethan-1-one) used is
(2) And (3) placing the mixture between two PET plastic films, and extruding the mixture into a film by using a film laminating machine.
(3) Irradiating the film with 365nm ultraviolet light with a light intensity of 1mw/cm2And the illumination time is 10min, and the heat insulation film added with the near infrared light shielding nano particle mixture is prepared.
Example 1
Mixing the nanoparticle mixture according to the nanoparticles and the corresponding mass fractions shown in Table 1;
TABLE 2 composition ratios of nanoparticle mixtures of example 1
The transmittance spectrum of the heat insulating film to which the nanoparticle mixture of example 1 was added was measured using an ultraviolet-visible-near infrared spectrometer, and as shown in fig. 3, it can be seen that most of the infrared light was intercepted.
Example 2
Mixing the nanoparticle mixture according to the nanoparticles and the corresponding mass fractions shown in Table 3;
TABLE 3 composition ratios of nanoparticle mixtures of example 2
The transmittance spectrum of the heat insulating film to which the nanoparticle mixture of example 2 was added was measured using an ultraviolet-visible-near infrared spectrophotometer, and as shown in fig. 4, it was seen that most of the infrared light was intercepted.
Example 3
Mixing the nanoparticle mixture according to the nanoparticles and the corresponding mass fractions shown in Table 4;
TABLE 4 composition ratios of nanoparticle mixtures of example 3
The transmittance spectrum of the heat insulating film to which the nanoparticle mixture of example 3 was added was measured using an ultraviolet-visible-near infrared spectrophotometer, and as shown in fig. 5, it was seen that most of the infrared light was intercepted.
In the above embodiments, the polymer provides a matrix for the light-transmitting film to transmit light, and therefore, other polymers such as PE, PVC, PB, and the like can be used in place of the above polymer materials.
In the above embodiments, in order to compare the influence of the content of cesium tungstate on the performance of the light-transmitting film, as a general knowledge, the ratio of ITO may also be adjusted as needed, and the inventor has experimentally verified that the ratio of the ITO composition is changed so as to change the infrared absorption capability, such as transmittance, of the light-transmitting film, and a person skilled in the art can adjust the ratio of ITO with reference to fig. 2 to achieve different infrared shielding effects.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A nanoparticle mixture is characterized by comprising 15-40 parts by weight of a first component, 10-60 parts by weight of a second component, 1-10 parts by weight of a third component, 5-25 parts by weight of a fourth component, 1-20 parts by weight of a fifth component, 1-8 parts by weight of a sixth component and 1-5 parts by weight of a seventh component;
the first component is cesium tungstate nano particles;
the second component is indium tin oxide nano particles, wherein the doping amount m of tin is more than or equal to 8.0 and less than or equal to 12.0 percent;
the third component is indium tin oxide nano particles, wherein the doping amount m of tin is more than or equal to 6.0 and m is less than 8.0 percent;
the fourth component is indium tin oxide nano particles, wherein the doping amount m of tin is more than or equal to 4.0 and m is less than 6.0 percent;
the fifth component is indium tin oxide nano particles, wherein the doping amount m of tin is more than or equal to 3.0 and m is less than 4.0 percent;
the sixth component is indium tin oxide nano particles, wherein the doping amount m of tin is more than or equal to 2.0 and m is less than 3.0 percent;
the seventh component is indium tin oxide nano particles, wherein the doping amount m of tin is more than or equal to 0.5 and m is less than 2.0 percent;
the particle diameters of the cesium tungstate nanoparticles and the ITO nanoparticles doped with different Sn contents are both 5 nm-20 nm.
2. A light-transmitting film characterized by: the light-transmitting film is doped with 0.1 to 5g of the nanoparticle mixture of claim 1 per square meter of the light-transmitting film when the thickness of the light-transmitting film is calculated as 20 micrometers.
3. The light-transmitting film of claim 2, wherein: the matrix of the light-transmitting film is a polymer.
4. The light-transmitting film of claim 2, wherein: the content of the nanoparticle mixture in the light-transmitting film is 0.1-0.5%.
5. The light-transmitting film of claim 2, wherein: the content of the nanoparticle mixture in the light-transmitting film is 0.5-1%.
6. The light-transmitting film of claim 2, wherein: the content of the nanoparticle mixture in the light-transmitting film is 1.0-1.5%.
7. The light-transmitting film of claim 2, wherein: the content of the nanoparticle mixture in the light-transmitting film is 1.5-2%.
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| CN101993657A (en) * | 2009-08-14 | 2011-03-30 | 北京建筑技术发展有限责任公司 | Intelligent nano transparent insulating glass coating |
| CN104262874A (en) * | 2014-09-20 | 2015-01-07 | 宣英男 | PVB (polyvinyl butyral) film for dynamically rejecting infrared rays and resisting ultraviolet rays and preparation method thereof |
| CN105502503A (en) * | 2016-01-11 | 2016-04-20 | 大连工业大学 | Hexagonal crystal tungsten bronze short rod nanoparticles and preparation method thereof |
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| CN101993657A (en) * | 2009-08-14 | 2011-03-30 | 北京建筑技术发展有限责任公司 | Intelligent nano transparent insulating glass coating |
| CN104262874A (en) * | 2014-09-20 | 2015-01-07 | 宣英男 | PVB (polyvinyl butyral) film for dynamically rejecting infrared rays and resisting ultraviolet rays and preparation method thereof |
| CN105502503A (en) * | 2016-01-11 | 2016-04-20 | 大连工业大学 | Hexagonal crystal tungsten bronze short rod nanoparticles and preparation method thereof |
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