CN111077603B - Flexible film with adjustable infrared emissivity and preparation method thereof - Google Patents

Flexible film with adjustable infrared emissivity and preparation method thereof Download PDF

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CN111077603B
CN111077603B CN201911405665.XA CN201911405665A CN111077603B CN 111077603 B CN111077603 B CN 111077603B CN 201911405665 A CN201911405665 A CN 201911405665A CN 111077603 B CN111077603 B CN 111077603B
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layer
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CN111077603A (en
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豆书亮
李垚
李晓白
赵九蓬
范青潽
任飞飞
谷金鑫
魏航
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Harbin Institute of Technology
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    • G02B5/00—Optical elements other than lenses
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    • G02—OPTICS
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Abstract

A flexible film with adjustable infrared emissivity and a preparation method thereof belong to the field of intelligent thermal control. The present invention aims at improving VO-based performance by the existing method2The emissivity change value of the intelligent thermal control device needs a high-precision vacuum coating system and a micro-nano structure processing system, is high in cost, low in preparation efficiency, limited in area size, high in preparation temperature, difficult to deposit a flexible film on a flexible substrate, and incapable of meeting the application problem of a special-shaped structure. The flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer. The preparation method comprises the following steps: one-micron and micron-scale W-doped VO2Preparing particles; two, VO2Preparing a composite layer film; thirdly, depositing a high-reflection metal substrate layer; and fourthly, depositing a surface protection layer. The invention is used for the infrared emissivity adjustable flexible film and the preparation thereof.

Description

Flexible film with adjustable infrared emissivity and preparation method thereof
Technical Field
The invention belongs to the field of intelligent thermal control.
Background
VO2The material is a thermochromic material, has the characteristics of high transmission of low-temperature infrared bands and high reflection of high-temperature infrared bands, and is very suitable for serving as a variable infrared emissivity device. Generally, VO is mixed2The film is deposited on a substrate with high infrared band reflection and transmits VO at low temperature2The infrared light of the film is reflected by the substrate, and the device has low emissivity; at high temperature, infrared light cannot transmit VO2Film, due to VO2The reflection of the film is lower than that of a high-reflection substrate, the emissivity of the device is increased, and the film is very suitable for intelligent thermal control. However, due to VO2The high temperature reflection of the film is high, resulting in VO-based2The high-temperature emissivity of the intelligent thermal control device is low, and the emissivity is changedThe value is only 0.1-0.3, and the application of the thermal control material in the thermal control field is severely restricted. Recent studies have found that when VO2When the material is in a sub-wavelength structure, the high-temperature metal state of the material has a surface plasma resonance effect, and the absorption at the resonance wavelength can be increased, so that the infrared emissivity is improved. The resonance wavelength and intensity are affected by the size, distribution and shape of the subwavelength structures. Such as by designing to make micron-sized VOs2The super surface utilizes the surface plasma resonance of the super surface between 8 and 14 microns to increase the absorption of the super surface at the wavelength and improve VO2The high-temperature infrared emissivity of the super surface realizes VO2The emissivity change of the intelligent radiator is larger than 0.4. However, the method requires a high-precision vacuum coating system and a micro-nano structure processing system, has high cost, low preparation efficiency, limited area size and high preparation temperature (about 500 ℃), is difficult to deposit a flexible thin film on a flexible substrate, and cannot meet the application of a special-shaped structure.
Disclosure of Invention
The invention aims to solve the problem that the existing method improves the VO-based2The intelligent thermal control device emissivity change value needs a high-precision vacuum coating system and a micro-nano structure processing system, is high in cost, low in preparation efficiency, limited in area size, high in preparation temperature, difficult to deposit a flexible film on a flexible substrate, and incapable of meeting the application problem of a special-shaped structure, and the preparation method of the flexible film with the adjustable infrared emissivity is provided.
The flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 1-10 mu m; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is (0.5-5): 100; the micron-sized W is doped with VO2W in the particles accounts for 0-2.5% of the total atomic number of W and V.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
will V2O5Adding the powder into ultrapure water, then sequentially adding tungstic acid and oxalic acid, fully stirring to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution at 180-250 ℃ for 12-144 h, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2W in the particles accounts for 0 to 2.5 percent of the total atomic number of W and V;
two, VO2Preparing a composite layer:
doping micron-sized W with VO2Fully blending the particles and the infrared transparent matrix material, and then preparing to obtain VO by using a film blowing method2Compounding layers;
the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is (0.5-5): 100;
the micron-sized W is doped with VO2The maximum size of the particles is 1-10 mu m;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The invention has the beneficial effects that:
(1) the invention adopts a bottom-up method, in particular to a micron-sized VO2The method is different from the traditional 'top-down' method of preparing micron-sized structures by depositing films and then utilizing a micro-nano processing technology to prepare the macro flexible filmsThe preparation method does not depend on large-scale vacuum coating equipment and micro-nano structure processing equipment, and is simple in processing method, low in cost, high in preparation efficiency and not limited in area size.
(2) The invention adopts a method of composite material to make micron-sized VO2Particles embedded in an infrared transparent matrix material, except for using VO2The resonance effect of the particle high-temperature surface plasma is enhanced, the resonance absorption of the particle in infrared band light is enhanced, and the particle high-temperature surface plasma is different from the traditional VO2The invention also utilizes the mismatch of the refractive indexes of the interfaces of the particles and the infrared transparent base material to scatter light at the interfaces, thereby increasing the optical path of the light in an infrared band in the base material, further increasing the absorption of the light, enhancing the high-temperature emissivity of the film and enlarging the change value of the infrared emissivity. The flexible film with the adjustable infrared emissivity has low-temperature emissivity which can reach 0.1 at the lowest temperature of 20 ℃, high-temperature emissivity which can reach 0.85 at the highest temperature of 100 ℃, large emissivity change at different temperatures, and the maximum emissivity change from 20 ℃ to 100 ℃ which can be more than 0.65, and is very suitable for serving as an intelligent thermal control coating.
(3) The vacuum coating is to prepare the flexible film with adjustable infrared emissivity at low temperature, and the flexible film can be used as a flexible device, thereby avoiding the defect that the existing intelligent radiator is limited by the preparation temperature and can not be used as the flexible device.
(4) VO reduction by W doping2The phase transition temperature is as low as 20 ℃ to realize the use at room temperature and the temperature lower than the room temperature, and the application of the high-reflection layer and the protective layer in intelligent self-adaptive thermal control is realized by depositing the high-reflection layer and the protective layer.
The invention relates to a flexible film with adjustable infrared emissivity and a preparation method thereof.
Drawings
FIG. 1 is a schematic structural diagram of a flexible film with adjustable infrared emissivity of the invention, wherein 1 is a surface protective layer, and 2 is VO2A composite layer, 3 is a high-reflection metal substrate layer, and 4 is micron-sized W-doped VO2And 5, particles are infrared transparent matrix materials.
Detailed Description
The first embodiment is as follows: detailed description of the invention with reference to FIG. 1The implementation mode is that the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and a VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 1-10 mu m; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is (0.5-5): 100; the micron-sized W is doped with VO2W in the particles accounts for 0-2.5% of the total atomic number of W and V.
The beneficial effects of the embodiment are as follows:
(1) the invention adopts a bottom-up method, in particular to a micron-sized VO2The method is different from the traditional top-down preparation method of preparing a micron-sized structure by depositing a film and then utilizing a micro-nano processing technology, does not depend on large-scale vacuum coating equipment and micro-nano structure processing equipment, and has the advantages of simple processing method, low cost, high preparation efficiency and unlimited area.
(2) The invention adopts a method of composite material to make micron-sized VO2Particles embedded in an infrared transparent matrix material, except for using VO2The resonance effect of the particle high-temperature surface plasma is enhanced, the resonance absorption of the particle in infrared band light is enhanced, and the particle high-temperature surface plasma is different from the traditional VO2The invention also utilizes the mismatch of the refractive indexes of the interfaces of the particles and the infrared transparent base material to scatter light at the interfaces, thereby increasing the optical path of the light in an infrared band in the base material, further increasing the absorption of the light, enhancing the high-temperature emissivity of the film and enlarging the change value of the infrared emissivity. The flexible film with adjustable infrared emissivity has low-temperature emissivity which can reach 0.1 at the lowest temperature of 20 ℃, high-temperature emissivity which can reach 0.85 at the highest temperature of 100 ℃, large emissivity change at different temperatures, and the maximum emissivity change from 20 ℃ to 100 ℃ can be more than 0.65, so that the flexible film is very suitable for being used as an intelligent filmAnd (4) thermal control coating.
(3) The vacuum coating is to prepare the flexible film with adjustable infrared emissivity at low temperature, and the flexible film can be used as a flexible device, thereby avoiding the defect that the existing intelligent radiator is limited by the preparation temperature and can not be used as the flexible device.
(4) VO reduction by W doping2The phase transition temperature is as low as 20 ℃ to realize the use at room temperature and the temperature lower than the room temperature, and the application of the high-reflection layer and the protective layer in intelligent self-adaptive thermal control is realized by depositing the high-reflection layer and the protective layer.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the high-reflection metal substrate layer is Al, Au, Ag, Mg, Ni, Zn or Cu; the surface protective layer is Al2O3、SiO2、ZrO2、Nb2O5、HfO2Or TiO2(ii) a The infrared transparent matrix material is high-density polyethylene or hydrogenated styrene-butadiene block copolymer. The rest is the same as the first embodiment.
The hydrogenated styrene-butadiene block copolymer of the present embodiment is SEBS, and the high density polyethylene is HDPE.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: the thickness of the high-reflection metal substrate layer is 100 nm-500 nm; the thickness of the surface protection layer is 50 nm-200 nm; the VO2The thickness of the composite layer is 200-500 μm. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the micron-sized W is doped with VO2The shape of the particles is rod-shaped, hexagonal star-shaped, polyhedral or spherical. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the embodiment provides a preparation method of a flexible film with adjustable infrared emissivity, which is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
will V2O5Powder is added intoAdding tungstic acid and oxalic acid into ultrapure water in sequence, fully stirring to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution at 180-250 ℃ for 12-144 h, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2W in the particles accounts for 0 to 2.5 percent of the total atomic number of W and V;
two, VO2Preparing a composite layer:
doping micron-sized W with VO2Fully blending the particles and the infrared transparent matrix material, and then preparing to obtain VO by using a film blowing method2Compounding layers;
the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is (0.5-5): 100;
the micron-sized W is doped with VO2The maximum size of the particles is 1-10 mu m;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The sixth specific implementation mode: the fifth embodiment is different from the fifth embodiment in that: the high-reflection metal substrate layer in the step three is Al, Au, Ag, Mg, Ni, Zn or Cu; the surface protective layer in the fourth step is Al2O3、SiO2、ZrO2、Nb2O5、HfO2Or TiO2(ii) a And the infrared transparent base material in the second step is high-density polyethylene or hydrogenated styrene-butadiene block copolymer. The rest is the same as the fifth embodiment.
The seventh embodiment: this embodiment differs from one of the fifth or sixth embodiments in that: step by stepThe thickness of the high-reflection metal substrate layer in the third step is 100 nm-500 nm; the thickness of the surface protective layer in the step four is 50 nm-200 nm; VO described in step two2The thickness of the composite layer is 200-500 μm. The other is the same as the fifth or sixth embodiment.
The specific implementation mode is eight: the difference between this embodiment mode and one of the fifth to seventh embodiment modes is that: the micron-sized W-doped VO in the step one2The shape of the particles is rod-shaped, hexagonal star-shaped, polyhedral or spherical. The rest is the same as the fifth to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the fifth to eighth embodiment in that: v in the step one2O5The ratio of the mass of the powder to the volume of the ultrapure water is (0.010-0.025) g:1 mL. The others are the same as the fifth to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the fifth to ninth embodiments in that: v in the step one2O5The mass ratio of the powder to the oxalic acid is 1 (0.6-1.5). The rest is the same as the fifth to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized VOs2Particle composition, micron order VO2The particles are distributed in the infrared transparent base material; the micron-sized VO2The maximum size of the particles is 1 μm; the micron-sized VO2The mass ratio of the particles to the infrared transparent matrix material is 0.5: 100;
the high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 200 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 100 nm; the infrared transparent base material is high-density polyethylene; saidVO2The thickness of the composite layer was 500. mu.m.
The micron-sized VO2The particles are rod-shaped.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one and micron order VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0g of tungstic acid and 1.75g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 12h at the temperature of 180 ℃, then centrifugally dispersing by using water and ethanol and cleaning the precipitate for 3 times to obtain micron-sized VO2Particles;
the micron-sized VO2The phase transition temperature of the particles is 75 ℃; the micron-sized VO2The shape of the particles is rod-shaped; micron-sized VO2The maximum size of the particles is 1 μm;
two, VO2Preparing a composite layer:
0.5g micron-sized VO is added under the conditions that the temperature is 180 ℃ and the rotating speed is 60r/min2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.12, the high-temperature emissivity at 100 ℃ is 0.42, and the emissivity change value is 0.3 by testing the emissivity from 20 ℃ to 100 ℃.
Example two:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 2 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 1: 100; the micron-sized W is doped with VO2W in the particles accounted for 0.5% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 300 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 200 nm; the infrared transparent base material is hydrogenated styrene-butadiene block copolymer; the VO2The thickness of the composite layer was 400. mu.m.
The micron-sized W is doped with VO2The particles are rod-shaped.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.018g of tungstic acid and 1.80g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, keeping the temperature of the grass green transparent solution at 200 ℃ for 24h, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 65 ℃; the micron-sized W is doped with VO2The shape of the particles is rod; the micron-sized W is doped with VO2The maximum size of the particles is 2 μm;
two, VO2Preparing a composite layer film:
at a temperature of 180 ℃ anddoping VO with W of 1g micron level at the rotation speed of 60r/min2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.1, the high-temperature emissivity at 100 ℃ is 0.42, and the emissivity change value of the flexible film is 0.32 obtained by testing the emissivity from 20 ℃ to 100 ℃.
Example three:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 2 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 1.5: 100; the micron-sized W is doped with VO2W in the particles accounted for 1% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 400 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 50 nm; the infrared transparent base material is high-density polyethylene; the VO2The thickness of the composite layer was 400. mu.m.
The micron-sized W is doped with VO2The shape of the granule is sixA star shape.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.036g of tungstic acid and 1.85g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 48h at 220 ℃, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 54 ℃; the micron-sized W is doped with VO2The shape of the particles is a hexagonal star; the micron-sized W is doped with VO2The maximum size of the particles is 2 μm;
two, VO2Preparing a composite layer film:
doping VO with 1.5g micron W at 180 deg.C and 65r/min2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.15, the high-temperature emissivity at 100 ℃ is 0.60, and the emissivity change value of the flexible film is 0.45 by testing the emissivity from 20 ℃ to 100 ℃.
Example four:
flexible film with adjustable infrared emissivitySequentially consists of a high-reflection metal basal layer and VO2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 5 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 2: 100; the micron-sized W is doped with VO2W in the particles accounted for 1.5% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 500 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 200 nm; the infrared transparent base material is hydrogenated styrene-butadiene block copolymer; the VO2The thickness of the composite layer was 300. mu.m.
The micron-sized W is doped with VO2The shape of the particles is polyhedral.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.054g of tungstic acid and 1.90g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 72h at 240 ℃, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 45 ℃; the micron-sized W is doped with VO2The shape of the particles is polyhedral; the micron-sized W is doped with VO2The maximum size of the particles is 5 μm;
two, VO2Preparing a composite layer film:
under the conditions of 180 ℃ and 70r/min of rotating speed, 2.0g of micronGraded W doped VO2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.15, the high-temperature emissivity at 100 ℃ is 0.68, and the emissivity change value of the flexible film is 0.53 by testing the emissivity from 20 ℃ to 100 ℃.
Example five:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 10 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 2.5: 100; the micron-sized W is doped with VO2W in the particles accounted for 2.0% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 100 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 50 nm; the infrared transparent base material is high-density polyethylene; the VO2The thickness of the composite layer was 300. mu.m.
The micron-sized W is doped with VO2The shape of the particles is spherical.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.072g of tungstic acid and 1.95g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 144h at the temperature of 260 ℃, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 36 ℃; the micron-sized W is doped with VO2The shape of the particles is spherical; the micron-sized W is doped with VO2The maximum size of the particles is 10 μm;
two, VO2Preparing a composite layer film:
doping 2.5g micron-sized W with VO at 180 ℃ and 75r/min of rotation speed2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.23, the high-temperature emissivity at 100 ℃ is 0.85, and the emissivity change value of the flexible film is 0.62 by testing the emissivity from 20 ℃ to 100 ℃.
Example six:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 8 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 0.5: 100; the micron-sized W is doped with VO2W in the particles accounted for 2.5% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 200 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 50 nm; the infrared transparent base material is hydrogenated styrene-butadiene block copolymer; the VO2The thickness of the composite layer was 200. mu.m.
The micron-sized W is doped with VO2The particles are spherical in shape.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.09g of tungstic acid and 1.80g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 144h at 240 ℃, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 28 ℃; the micron-sized W is doped with VO2The shape of the particles is spherical;
two, VO2Preparing a composite layer film:
doping 0.5g micron-sized W with VO at 180 ℃ and at a rotating speed of 75r/min2The particles are fully blended with 100g of infrared transparent matrix material, and then the mixture is heated to 180-190 ℃ to obtain the transparent glassPreparing VO by a film blowing method2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.2, the high-temperature emissivity at 100 ℃ is 0.85, and the emissivity change value of the flexible film is 0.65 by testing the emissivity from 20 ℃ to 100 ℃.
Example seven:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 10 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 1.5: 100; the micron-sized W is doped with VO2W in the particles accounted for 0.5% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 500 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 50 nm; the infrared transparent base material is high-density polyethylene; the VO2The thickness of the composite layer was 200. mu.m.
The micron-sized W is doped with VO2The particles are rod-like in shape.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.018g of tungstic acid and 1.75g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 144h at the temperature of 200 ℃, then repeatedly centrifuging and dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 68 ℃; the micron-sized W is doped with VO2The shape of the particles is rod-like; the micron-sized W is doped with VO2The maximum size of the particles is 10 μm;
two, VO2Preparing a composite layer film:
doping VO with 1.5g micron W at 180 deg.C and 75r/min2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.12, the high-temperature emissivity at 100 ℃ is 0.58, and the emissivity change value of the flexible film is 0.46 obtained by testing the emissivity from 20 ℃ to 100 ℃.
Example eight:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is composed of an infrared transparent baseBulk material and multiple micron-sized W-doped VO2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 8 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 2.5: 100; the micron-sized W is doped with VO2W in the particles accounted for 1% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 500 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 50 nm; the infrared transparent base material is hydrogenated styrene-butadiene block copolymer; the VO2The thickness of the composite layer was 500. mu.m.
The micron-sized W is doped with VO2The particles are rod-shaped.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.036g of tungstic acid and 1.70g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 144h at the temperature of 180 ℃, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 58 ℃; the micron-sized W is doped with VO2The shape of the particles is rod-shaped; the micron-sized W is doped with VO2The maximum size of the particles is 8 μm;
two, VO2Preparing a composite layer film:
doping 2.5g micron-sized W with VO at the temperature of 180 ℃ and the rotating speed of 55r/min2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.12, the high-temperature emissivity at 100 ℃ is 0.80, and the emissivity change value of the flexible film is 0.68 obtained by testing the emissivity from 20 ℃ to 100 ℃.
Example nine:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 5 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 0.5: 100; the micron-sized W is doped with VO2W in the particles represents 2% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 200 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 100 nm; the infrared transparent base material is high-density polyethylene; the VO2The thickness of the composite layer was 500. mu.m.
The micron-sized W is doped with VO2The shape of the particles is a hexagonal star.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of granules：
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.072g of tungstic acid and 1.75g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 36h at the temperature of 240 ℃, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 35 ℃; the micron-sized W is doped with VO2The shape of the particles is a hexagonal star; the micron-sized W is doped with VO2The maximum size of the particles is 5 μm;
two, VO2Preparing a composite layer film:
doping 0.5g micron-sized W with VO at 180 ℃ and 60r/min of rotation speed2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.23, the high-temperature emissivity at 100 ℃ is 0.68, and the emissivity change value of the flexible film is 0.45 by testing the emissivity from 20 ℃ to 100 ℃.
Example ten:
the flexible film with adjustable infrared emissivity consists of a high-reflection metal basal layer and VO from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 3 μm; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is 1.5: 100; the micron-sized W is doped with VO2W in the particles accounted for 1.0% of the total atomic number of W and V.
The high-reflection metal substrate layer is Ag; the thickness of the high-reflection metal substrate layer is 200 nm; the surface protective layer is Al2O3(ii) a The thickness of the surface protection layer is 100 nm; the infrared transparent base material is hydrogenated styrene-butadiene block copolymer; the VO2The thickness of the composite layer was 400. mu.m.
The micron-sized W is doped with VO2The shape of the particles is a hexagonal star.
A preparation method of a flexible film with adjustable infrared emissivity is carried out according to the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
1.3g V2O5Adding the powder into 70mL of ultrapure water, then sequentially adding 0.036g of tungstic acid and 1.80g of oxalic acid, fully stirring for 10h to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution for 24h at 220 ℃, then repeatedly centrifugally dispersing by using water and ethanol and cleaning precipitates for 3 times to obtain micron-sized W-doped VO2Particles;
the micron-sized W is doped with VO2The phase transition temperature of the particles is 55 ℃; the micron-sized W is doped with VO2The shape of the particles is a hexagonal star; the micron-sized W is doped with VO2The maximum size of the particles is 3 μm;
two, VO2Preparing a composite layer film:
doping VO with 1.5g micron W at 180 deg.C and 60r/min2Fully blending the particles with 100g of infrared transparent matrix material, and preparing VO by a film blowing method at the temperature of 180-190 DEG C2Compounding layers;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
The low-temperature emissivity of the flexible film with the adjustable infrared emissivity, which is prepared by the embodiment, at 20 ℃ is 0.15, the high-temperature emissivity at 100 ℃ is 0.55, and the emissivity change value of the flexible film is 0.40 obtained by testing the emissivity from 20 ℃ to 100 ℃.

Claims (6)

1. The flexible film with adjustable infrared emissivity is characterized in that the flexible film with adjustable infrared emissivity is composed of a high-reflection metal basal layer and a VO (volatile organic compound) from bottom to top in sequence2A composite layer and a surface protection layer;
the VO2The composite layer is made of infrared transparent base material and a plurality of micron-sized W-doped VOs2Particle composition, micron-sized W-doped VO2The particles are distributed in the infrared transparent base material; the micron-sized W is doped with VO2The maximum size of the particles is 1-10 mu m; the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is (0.5-5): 100; the micron-sized W is doped with VO2W in the particles accounts for 0 to 2.5 percent of the total atomic number of W and V; the infrared transparent base material in the second step is high-density polyethylene or hydrogenated styrene-butadiene block copolymer;
the flexible film with adjustable infrared emissivity is prepared by the following steps:
one-micron and micron-scale W-doped VO2Preparation of the particles:
will V2O5Adding the powder into ultrapure water, then sequentially adding tungstic acid and oxalic acid, fully stirring to obtain a grass green transparent solution, preserving the temperature of the grass green transparent solution at 180-250 ℃ for 12-144 h, and reacting by using water and ethanolRe-centrifuging to disperse and clean the precipitate to obtain micron-level W-doped VO2Particles;
the micron-sized W is doped with VO2W in the particles accounts for 0 to 2.5 percent of the total atomic number of W and V;
two, VO2Preparing a composite layer:
doping micron-sized W with VO2Fully blending the particles and the infrared transparent matrix material, and then preparing to obtain VO by using a film blowing method2Compounding layers;
the micron-sized W is doped with VO2The mass ratio of the particles to the infrared transparent matrix material is (0.5-5): 100;
the micron-sized W is doped with VO2The maximum size of the particles is 1-10 mu m;
thirdly, depositing a high-reflection metal substrate layer:
with VO2The composite layer is used as a substrate, and a vacuum coating method is used for coating the composite layer on VO2Preparing a high-reflection metal substrate layer on one side of the composite layer;
fourthly, depositing a surface protection layer:
in VO by vacuum coating method2And depositing a surface protection layer on the other side of the composite layer to obtain the flexible film with adjustable infrared emissivity.
2. The flexible infrared emissivity film according to claim 1, wherein said high reflective metal substrate layer in step three is Al, Au, Ag, Mg, Ni, Zn or Cu; the surface protective layer in the fourth step is Al2O3、SiO2、ZrO2、Nb2O5、HfO2Or TiO2。
3. The flexible film with adjustable infrared emissivity as claimed in claim 1, wherein the thickness of the high reflective metal substrate layer in step three is 100nm to 500 nm; the thickness of the surface protective layer in the step four is 50 nm-200 nm; VO described in step two2The thickness of the composite layer is 200-500 μm.
4. The flexible film with adjustable infrared emissivity as claimed in claim 1, wherein in step one, the micron-sized W-doped VO2The shape of the particles is rod-shaped, hexagonal star-shaped, polyhedral or spherical.
5. The flexible film with adjustable infrared emissivity as claimed in claim 1, wherein said V in step one2O5The ratio of the mass of the powder to the volume of the ultrapure water is (0.010-0.025) g:1 mL.
6. The flexible film with adjustable infrared emissivity as claimed in claim 1, wherein said V in step one2O5The mass ratio of the powder to the oxalic acid is 1 (0.6-1.5).
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