CN111077603A - A kind of infrared emissivity adjustable flexible film and preparation method thereof - Google Patents

A kind of infrared emissivity adjustable flexible film and preparation method thereof Download PDF

Info

Publication number
CN111077603A
CN111077603A CN201911405665.XA CN201911405665A CN111077603A CN 111077603 A CN111077603 A CN 111077603A CN 201911405665 A CN201911405665 A CN 201911405665A CN 111077603 A CN111077603 A CN 111077603A
Authority
CN
China
Prior art keywords
micron
particles
doped
layer
flexible film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201911405665.XA
Other languages
Chinese (zh)
Other versions
CN111077603B (en
Inventor
豆书亮
李垚
李晓白
赵九蓬
范青潽
任飞飞
谷金鑫
魏航
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harbin Institute of Technology Shenzhen
Original Assignee
Harbin Institute of Technology Shenzhen
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Institute of Technology Shenzhen filed Critical Harbin Institute of Technology Shenzhen
Priority to CN201911405665.XA priority Critical patent/CN111077603B/en
Publication of CN111077603A publication Critical patent/CN111077603A/en
Application granted granted Critical
Publication of CN111077603B publication Critical patent/CN111077603B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/008—Surface plasmon devices
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
    • G02B5/0236—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element
    • G02B5/0242—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element by means of dispersed particles
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0268—Diffusing elements; Afocal elements characterized by the fabrication or manufacturing method

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Laminated Bodies (AREA)

Abstract

一种红外发射率可调柔性薄膜及其制备方法，它属于智能热控领域。本发明要现有方法提高基于VO2的智能热控器件发射率变化值，需要高精度的真空镀膜系统和微纳结构加工系统，成本高，制备效率低，面积大小受限，且制备温度较高，难以在柔性基底上沉积柔性薄膜，不能满足异形结构应用的问题。一种红外发射率可调柔性薄膜自下而上依次由高反射金属基底层、VO2复合层和表面保护层组成。制备方法：一、微米级W掺杂VO2颗粒的制备；二、VO2复合层膜的制备；三、高反射金属基底层沉积；四、表面保护层沉积。本发明用于红外发射率可调柔性薄膜及其制备。

Figure 201911405665

A flexible film with adjustable infrared emissivity and a preparation method thereof belong to the field of intelligent thermal control. The present invention requires the existing method to improve the emissivity change value of the intelligent thermal control device based on VO 2 , and requires a high-precision vacuum coating system and a micro-nano structure processing system, which has high cost, low preparation efficiency, limited area size, and relatively high preparation temperature. High, it is difficult to deposit flexible films on flexible substrates, which cannot meet the problem of special-shaped structure applications. A flexible film with adjustable infrared emissivity is composed of a high-reflection metal base layer, a VO 2 composite layer and a surface protection layer in sequence from bottom to top. Preparation methods: first, preparation of micron-scale W-doped VO 2 particles; second, preparation of VO 2 composite layer film; third, deposition of high-reflection metal base layer; fourth, deposition of surface protective layer. The invention is used for a flexible film with adjustable infrared emissivity and its preparation.

Figure 201911405665

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, the emissivity change value is only 0.1-0.3, and the application of the intelligent thermal control device 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 problems of the prior methodHigh basis of VO2The 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 micro-scaleMeter grade W doped 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 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, the coating 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: specifically, referring to fig. 1, the flexible film with adjustable infrared emissivity of the present embodiment is composed of a high reflective metal substrate layer and a VO sequentially from bottom to top2A 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 particles are blended with the infrared transparent matrix material and blown to prepare the macroscopic flexible film, which is different from the traditional method that the particles are blown to the film by utilizing micro-particles after being deposited to form the filmThe top-down preparation method of the micron-sized structure prepared by the 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 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 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 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 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: the 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; the VO2The 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 VO2Thickness of composite layerAnd 400 μm.
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:
doping VO with 1g 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 0.1, 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 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 1.85g 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:
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 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.
SaidMicron-sized W-doped 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:
doping VO with 2.0g micron W at 180 deg.C and 70r/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 0.68, 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:
at a temperature of 180 ℃ and a rotational speed of 75r/minUnder the condition, 2.5g micron-sized W is doped with 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 0.23, 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 VO2Shape of the particlesIs 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 0.09g 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/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 0.2, 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 sequence2Composite layer and surface protectionLayer composition;
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/min2The particles are thoroughly blended with 100g of an infrared transparent matrix material and then heated at a temperature of 180 ℃ to 19 ℃Preparing VO by a blowing film method at 0 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 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 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 V isO2The 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 the particles:
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 (10)

1.一种红外发射率可调柔性薄膜，其特征在于一种红外发射率可调柔性薄膜自下而上依次由高反射金属基底层、VO2复合层和表面保护层组成；1. an infrared emissivity adjustable flexible film, it is characterized in that a kind of infrared emissivity adjustable flexible film is made up of high reflection metal base layer, VO composite layer and surface protective layer successively from bottom to top ; 所述的VO2复合层由红外透明基体材料及多个微米级W掺杂VO2颗粒组成，微米级W掺杂VO2颗粒分布于红外透明基体材料内部；所述的微米级W掺杂VO2颗粒的最大尺寸为1μm～10μm；所述的微米级W掺杂VO2颗粒与红外透明基体材料的质量比为(0.5～5):100；所述的微米级W掺杂VO2颗粒中W占W与V的总原子数的0％～2.5％。The VO 2 composite layer is composed of an infrared transparent matrix material and a plurality of micron-scale W-doped VO 2 particles, and the micron-scale W-doped VO 2 particles are distributed inside the infrared transparent matrix material; the micron-scale W-doped VO 2 The maximum size of the particles is 1 μm to 10 μm; the mass ratio of the micron-scale W-doped VO 2 particles to the infrared transparent matrix material is (0.5 to 5): 100; the micron-scale W-doped VO 2 particles are W accounts for 0% to 2.5% of the total atomic number of W and V. 2.根据权利要求1所述的一种红外发射率可调柔性薄膜，其特征在于所述的高反射金属基底层为Al、Au、Ag、Mg、Ni、Zn或Cu；所述的表面保护层为Al2O3、SiO2、ZrO2、Nb2O5、HfO2或TiO2；所述的红外透明基体材料为高密度聚乙烯或氢化苯乙烯-丁二烯嵌段共聚物。2. A kind of infrared emissivity adjustable flexible film according to claim 1, is characterized in that described high reflection metal base layer is Al, Au, Ag, Mg, Ni, Zn or Cu; Described surface protection The layer is Al 2 O 3 , SiO 2 , ZrO 2 , Nb 2 O 5 , HfO 2 or TiO 2 ; the infrared transparent base material is high-density polyethylene or hydrogenated styrene-butadiene block copolymer. 3.根据权利要求1所述的一种红外发射率可调柔性薄膜，其特征在于所述的高反射金属基底层厚度为100nm～500nm；所述的表面保护层厚度为50nm～200nm；所述的VO2复合层厚度为200μm～500μm。3. A flexible film with adjustable infrared emissivity according to claim 1, characterized in that the thickness of the high-reflection metal base layer is 100nm-500nm; the thickness of the surface protection layer is 50nm-200nm; the thickness of the surface protection layer is 50nm-200nm; The thickness of the VO 2 composite layer is 200μm ~ 500μm. 4.根据权利要求1所述的一种红外发射率可调柔性薄膜，其特征在于所述的微米级W掺杂VO2颗粒的形状为棒形、六角星形、多面体形或球形。4 . The flexible film with adjustable infrared emissivity according to claim 1 , wherein the shape of the micron-scale W-doped VO 2 particles is a rod shape, a hexagonal star shape, a polyhedron shape or a spherical shape. 5 . 5.如权利要求1所述的一种红外发射率可调柔性薄膜的制备方法，其特征在于它是按以下步骤进行的：5. the preparation method of a kind of infrared emissivity adjustable flexible film as claimed in claim 1 is characterized in that it is carried out according to the following steps: 一、微米级W掺杂VO2颗粒的制备：1. Preparation of micron-scale W-doped VO 2 particles: 将V2O5粉末加入到超纯水中，然后依次添加钨酸和草酸，充分搅拌后，得到草绿色透明溶液，将草绿色透明溶液在温度为180℃～250℃的条件下，保温12h～144h，然后利用水和乙醇反复离心分散并清洗沉淀物，得到微米级W掺杂VO2颗粒；Add V 2 O 5 powder into ultrapure water, then add tungstic acid and oxalic acid in turn, and after thorough stirring, a grass-green transparent solution is obtained, and the grass-green transparent solution is kept at a temperature of 180℃～250℃ for 12h ~144h, and then repeatedly centrifuged and washed the precipitate with water and ethanol to obtain micron-sized W-doped VO 2 particles; 所述的微米级W掺杂VO2颗粒中W占W与V的总原子数的0％～2.5％；In the micron-scale W-doped VO 2 particles, W accounts for 0% to 2.5% of the total atomic number of W and V; 二、VO2复合层的制备：Second, the preparation of VO 2 composite layer: 将微米级W掺杂VO2颗粒与红外透明基体材料充分共混，然后利用吹膜法制备得到VO2复合层；The micron-scale W-doped VO 2 particles are fully blended with the infrared transparent matrix material, and then the VO 2 composite layer is prepared by the blown film method; 所述的微米级W掺杂VO2颗粒与红外透明基体材料的质量比为(0.5～5):100；The mass ratio of the micron-scale W-doped VO 2 particles to the infrared transparent matrix material is (0.5-5):100; 所述的微米级W掺杂VO2颗粒的最大尺寸为1μm～10μm；The maximum size of the micron-scale W-doped VO 2 particles is 1 μm˜10 μm; 三、高反射金属基底层沉积：3. Deposition of high reflective metal base layer: 以VO2复合层为基底，利用真空镀膜的方法，在VO2复合层一侧制备高反射金属基底层；Using the VO 2 composite layer as the base, a high-reflection metal base layer was prepared on the side of the VO 2 composite layer by vacuum coating; 四、表面保护层沉积：Fourth, the surface protective layer deposition: 利用真空镀膜的方法，在VO2复合层另一侧沉积表面保护层，得到红外发射率可调柔性薄膜。Using the method of vacuum coating, a surface protective layer was deposited on the other side of the VO 2 composite layer to obtain a flexible film with adjustable infrared emissivity. 6.根据权利要求5所述的一种红外发射率可调柔性薄膜的制备方法，其特征在于步骤三中所述的高反射金属基底层为Al、Au、Ag、Mg、Ni、Zn或Cu；步骤四中所述的表面保护层为Al2O3、SiO2、ZrO2、Nb2O5、HfO2或TiO2；步骤二中所述的红外透明基体材料为高密度聚乙烯或氢化苯乙烯-丁二烯嵌段共聚物。6. the preparation method of a kind of infrared emissivity adjustable flexible film according to claim 5 is characterized in that the high reflection metal base layer described in step 3 is Al, Au, Ag, Mg, Ni, Zn or Cu ; the surface protective layer described in step 4 is Al 2 O 3 , SiO 2 , ZrO 2 , Nb 2 O 5 , HfO 2 or TiO 2 ; the infrared transparent base material described in step 2 is high-density polyethylene or hydrogenated polyethylene Styrene-butadiene block copolymer. 7.根据权利要求5所述的一种红外发射率可调柔性薄膜的制备方法，其特征在于步骤三中所述的高反射金属基底层厚度为100nm～500nm；步骤四中所述的表面保护层厚度为50nm～200nm；步骤二中所述的VO2复合层厚度为200μm～500μm。7 . The method for preparing a flexible film with adjustable infrared emissivity according to claim 5 , wherein the thickness of the highly reflective metal base layer described in step 3 is 100 nm to 500 nm; the surface protection described in step 4 The thickness of the layer is 50 nm to 200 nm; the thickness of the VO 2 composite layer described in step 2 is 200 μm to 500 μm. 8.根据权利要求5所述的一种红外发射率可调柔性薄膜的制备方法，其特征在于步骤一中所述的微米级W掺杂VO2颗粒的形状为棒形、六角星形、多面体形或球形。8. The preparation method of a flexible film with adjustable infrared emissivity according to claim 5, wherein the micron-scale W-doped VO particles described in the step 1 are in the shape of a rod, a hexagonal star, a polyhedron shaped or spherical. 9.根据权利要求5所述的一种红外发射率可调柔性薄膜的制备方法，其特征在于步骤一中所述的V2O5粉末的质量与超纯水的体积比为(0.010～0.025)g:1mL。9 . The method for preparing a flexible film with adjustable infrared emissivity according to claim 5 , wherein the mass ratio of the V 2 O 5 powder described in the step 1 to the volume ratio of the ultrapure water is (0.010～0.025 . ) g: 1 mL. 10.根据权利要5所述的一种红外发射率可调柔性薄膜的制备方法，其特征在于步骤一中所述的V2O5粉末与草酸的质量比为1:(0.6～1.5)。10 . The method for preparing a flexible film with adjustable infrared emissivity according to claim 5 , wherein the mass ratio of V 2 O 5 powder and oxalic acid described in step 1 is 1:(0.6-1.5). 11 .
CN201911405665.XA 2019-12-30 2019-12-30 Flexible film with adjustable infrared emissivity and preparation method thereof Active CN111077603B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911405665.XA CN111077603B (en) 2019-12-30 2019-12-30 Flexible film with adjustable infrared emissivity and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911405665.XA CN111077603B (en) 2019-12-30 2019-12-30 Flexible film with adjustable infrared emissivity and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111077603A true CN111077603A (en) 2020-04-28
CN111077603B CN111077603B (en) 2022-01-28

Family

ID=70320336

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911405665.XA Active CN111077603B (en) 2019-12-30 2019-12-30 Flexible film with adjustable infrared emissivity and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111077603B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113186491A (en) * 2021-05-10 2021-07-30 清华大学 Composite layer with continuously adjustable infrared emissivity and application thereof
CN113185863A (en) * 2021-04-13 2021-07-30 电子科技大学 Based on VO2Intelligent temperature control coating with core-shell structure and thermal variable emissivity
CN113943922A (en) * 2021-10-11 2022-01-18 哈尔滨工业大学 Preparation method and repair method of repairable dynamic infrared radiation regulation and control material
CN114987004A (en) * 2022-05-16 2022-09-02 中国人民解放军国防科技大学 Gas-induced-change infrared emissivity device and preparation method and application thereof
CN115200410A (en) * 2022-07-21 2022-10-18 哈尔滨工业大学 Infrared radiation dynamic reconfigurable device and preparation method thereof

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2856802A1 (en) * 2003-06-26 2004-12-31 France Etat Armement FLEXIBLE MATERIAL WITH OPTICAL CONTRAST IN INFRARED
CN1624029A (en) * 2004-10-28 2005-06-08 中山大学 Vanadium dioxide solar thermal intelligent temperature control polymer film
CN101164900A (en) * 2007-10-09 2008-04-23 上海师范大学 Technique for preparing phase-change temperature controllable tungsten doping nano vanadium dioxide powder
CN101900607A (en) * 2010-06-24 2010-12-01 电子科技大学 A vanadium oxide thin film for infrared detector and its manufacturing method
CN103073943A (en) * 2012-01-19 2013-05-01 中国科学院上海硅酸盐研究所 Vanadium dioxide intelligent temperature control coating
CN103435100A (en) * 2013-07-13 2013-12-11 宿州学院 A Method for Lowering the Phase Transition Temperature of Vanadium Dioxide by W6+ Doping
CN104698511A (en) * 2015-01-29 2015-06-10 南京理工大学 Method for improving absorption rate of near infrared band of vanadium oxide film and prepared vanadium oxide film thereof
CN105017698A (en) * 2015-06-11 2015-11-04 付国东 Photo-thermal response type intelligent energy-saving composite film
CN107942428A (en) * 2017-11-15 2018-04-20 江西师范大学 A kind of infrared light perfection absorber and preparation method thereof
CN108198878A (en) * 2016-12-08 2018-06-22 南京理工大学 Promote the square blanket periodic structure of vanadium dioxide light absorption enhancing
US20180335651A1 (en) * 2014-05-28 2018-11-22 National Technology & Engineering Solutions Of Sandia, Llc Thermochromic low-emissivity film
CN108866483A (en) * 2018-06-26 2018-11-23 中国人民解放军国防科技大学 Intelligent thermal control device and preparation method thereof
CN109518148A (en) * 2018-12-14 2019-03-26 哈尔滨工业大学 A method of vanadium dioxide intelligence thermal suite is prepared using high energy pulse reaction magnetocontrol sputtering
CN110156340A (en) * 2019-05-24 2019-08-23 武汉大学 A kind of preparation method of temperature-sensitive VO2 light-cured flexible film

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2856802A1 (en) * 2003-06-26 2004-12-31 France Etat Armement FLEXIBLE MATERIAL WITH OPTICAL CONTRAST IN INFRARED
CN1624029A (en) * 2004-10-28 2005-06-08 中山大学 Vanadium dioxide solar thermal intelligent temperature control polymer film
CN101164900A (en) * 2007-10-09 2008-04-23 上海师范大学 Technique for preparing phase-change temperature controllable tungsten doping nano vanadium dioxide powder
CN101900607A (en) * 2010-06-24 2010-12-01 电子科技大学 A vanadium oxide thin film for infrared detector and its manufacturing method
CN103073943A (en) * 2012-01-19 2013-05-01 中国科学院上海硅酸盐研究所 Vanadium dioxide intelligent temperature control coating
CN103435100A (en) * 2013-07-13 2013-12-11 宿州学院 A Method for Lowering the Phase Transition Temperature of Vanadium Dioxide by W6+ Doping
US20180335651A1 (en) * 2014-05-28 2018-11-22 National Technology & Engineering Solutions Of Sandia, Llc Thermochromic low-emissivity film
CN104698511A (en) * 2015-01-29 2015-06-10 南京理工大学 Method for improving absorption rate of near infrared band of vanadium oxide film and prepared vanadium oxide film thereof
CN105017698A (en) * 2015-06-11 2015-11-04 付国东 Photo-thermal response type intelligent energy-saving composite film
CN108198878A (en) * 2016-12-08 2018-06-22 南京理工大学 Promote the square blanket periodic structure of vanadium dioxide light absorption enhancing
CN107942428A (en) * 2017-11-15 2018-04-20 江西师范大学 A kind of infrared light perfection absorber and preparation method thereof
CN108866483A (en) * 2018-06-26 2018-11-23 中国人民解放军国防科技大学 Intelligent thermal control device and preparation method thereof
CN109518148A (en) * 2018-12-14 2019-03-26 哈尔滨工业大学 A method of vanadium dioxide intelligence thermal suite is prepared using high energy pulse reaction magnetocontrol sputtering
CN110156340A (en) * 2019-05-24 2019-08-23 武汉大学 A kind of preparation method of temperature-sensitive VO2 light-cured flexible film

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
LIU DONGQING, CHENG HAIFENG*, ZHENG WENWEI, ZHANG CHAOYANG: "Infrared Thermochromic Properties of VO2 Thin Films Prepared through Aqueous Sol-gel Process", 《武汉理工大学学报：材料科学英文版》 *
SHULIANG DOU: "A facile method for the preparation of W-doped VO2 films with lowered phase transition temperature, narrowed hysteresis loops and excellent cycle stability", 《MATERIALS CHEMISTRY AND PHYSICS》 *
张芳: "二氧化钒纳米粉体的制备及其掺杂改性的研究", 《中国优秀硕士学位论文全文数据库》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113185863A (en) * 2021-04-13 2021-07-30 电子科技大学 Based on VO2Intelligent temperature control coating with core-shell structure and thermal variable emissivity
CN113186491A (en) * 2021-05-10 2021-07-30 清华大学 Composite layer with continuously adjustable infrared emissivity and application thereof
CN113943922A (en) * 2021-10-11 2022-01-18 哈尔滨工业大学 Preparation method and repair method of repairable dynamic infrared radiation regulation and control material
CN113943922B (en) * 2021-10-11 2023-10-17 哈尔滨工业大学 Preparation method and repair method of a repairable dynamic infrared radiation control material
CN114987004A (en) * 2022-05-16 2022-09-02 中国人民解放军国防科技大学 Gas-induced-change infrared emissivity device and preparation method and application thereof
CN115200410A (en) * 2022-07-21 2022-10-18 哈尔滨工业大学 Infrared radiation dynamic reconfigurable device and preparation method thereof
CN115200410B (en) * 2022-07-21 2024-02-20 哈尔滨工业大学 An infrared radiation dynamically reconfigurable device and its preparation method

Also Published As

Publication number Publication date
CN111077603B (en) 2022-01-28

Similar Documents

Publication Publication Date Title
CN111077603B (en) Flexible film with adjustable infrared emissivity and preparation method thereof
Liu et al. Micro‐nano porous structure for efficient daytime radiative sky cooling
CN105713597B (en) A kind of composite type heat mutagens mill base material and preparation method thereof
CN101974245B (en) High-transparent ultraviolet-blocking energy-saving membrane and solution phase transfer preparation method
CN103978203B (en) A kind of spectrum local decorated thermocolour composite nano-powder and preparation method thereof
CN102064204B (en) Broadband antireflection nano structure and preparation method thereof
TW200913287A (en) Solar cell and manufacturing method thereof
CN101219859A (en) Nano-oily ATO thermal insulation slurry, preparation method and application thereof
CN103554997A (en) Carbon-coated vanadium dioxide nanoparticles and preparation method thereof
CN114231073A (en) Core-shell structure reflective substrate, daytime radiation refrigeration coating, coating and preparation method
TW201234618A (en) Process for particle doping of scattering superstrates
CN106585024A (en) High-temperature low-precipitate optical polyester-based film and preparation method thereof
CN102336528B (en) Vanadium dioxide film, its preparation and its application
CN111453999B (en) Preparation method of intelligent radiator
CN114262165B (en) Omnidirectional reflection red glass
CN103694877B (en) Nanofiber solar energy efficient absorption composite membrane and preparation thereof and spraying method
CN103771722B (en) A kind of transparent light modulation structure with high heat insulating function and preparation method thereof and application
CN116426146A (en) Hybrid colored metallic pigments
CN107805314A (en) A kind of antireflecting coating based on nano silver wire and preparation method thereof
CN118545914A (en) Self-cleaning anti-reflection coating on photovoltaic module surface and preparation method thereof
CN103205249B (en) Method for preparing VO2 core-shell structure
CN102153290A (en) Method for preparing porosity-adjustable nano porous antireflection film by doping organic template
TW201018715A (en) White heat insulation coating
CN115710780A (en) Sun-shading and cooling film and preparation method and application thereof
CN105158825A (en) Anti-reflection structure and construction method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant