CN106167414B - Preparation method of vanadium dioxide thin film with thermal-reflectivity response - Google Patents
Preparation method of vanadium dioxide thin film with thermal-reflectivity response Download PDFInfo
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Abstract
The invention discloses a preparation method of a vanadium dioxide film with heat-reflectivity response; comprises the steps of pretreatment of glass fiber, impregnation of precursor solution and sintering of impregnated glass fiber cloth. The vanadium dioxide film prepared by the invention has good thermo-optic response performance and has abrupt change of reflectivity near 38 ℃. When the temperature is below 38 ℃, the reflectance is at a high level, when the temperature is above 38 ℃, the reflectance is at a low level, and this property is reversible. The heat-reflectivity response of the greenhouse can be applied to negative feedback regulation of the temperature in the greenhouse, so that the indoor temperature can be maintained to be about 38 ℃, and the development of plants in the greenhouse is facilitated. The preparation method of the vanadium dioxide film with the glass fiber cloth as the carrier and the thermal-reflectivity response has the advantages of energy conservation, low cost, safety, simplicity, stability, short time consumption and the like.
Description
Technical Field
The invention relates to a vanadium dioxide film and a preparation method thereof, in particular to a preparation method of a vanadium dioxide film which takes glass fiber as a carrier and has thermal-reflectivity response.
Background
Vanadium dioxide films have received much attention because of their low phase transition temperature (about 68 ℃). The phase change rate is very high near the phase change temperature, and after phase change occurs, the optical property, the electrical property, the thermal conductivity, the magnetic conductivity and the like of the vanadium dioxide film can be suddenly changed, so that the vanadium dioxide film has very high application value in thermo-optical, thermoelectric and thermomagnetic materials. However, the phase transition temperature is far higher than the room temperature, and the phase transition temperature cannot be used for temperature negative feedback regulation in the greenhouse.
The methods for preparing the vanadium dioxide film mainly include Chemical Vapor Deposition (CVD), ion sputtering and sol-gel methods. The sol-gel method is considered to be one of the simplest methods among these.
The domestic research on the glass fiber is mainly used for the research on structural materials, and the research on functional materials is rather than boring. Through the search of the existing patent documents, the Chinese patent application with the application number of 201410236112.7 discloses an inorganic sol-gel preparation method of a vanadium dioxide film; the prepared vanadium dioxide film has excellent optical regulation performance, the highest visible light transmittance can reach 70 percent, the highest infrared regulation performance can reach 60 percent, and the vanadium dioxide film has wide application prospect in the field of photoelectric functional materials. However, the substrate used in the invention is a transparent substrate, and cannot be applied to the adjustment of reflected light; furthermore, the inventive film requires sintering under a gas-permeable atmosphere, which is more complicated than the present invention. Secondly, the phase transition temperature of the invention is 60-65 ℃, and the invention can not be used for regulating the temperature in a temperature control room.
Disclosure of Invention
The invention aims to overcome the defect that the phase transition temperature of vanadium dioxide is too high to be used for temperature negative feedback regulation in a greenhouse, and provides a preparation method of a vanadium dioxide film which has phase transition temperature of 38 ℃ and thermal-reflectivity response and takes glass fiber as a carrier; the invention uses glass fiber cloth as a carrier, uses a sol-gel method to load a plurality of layers of colloid films on the surface of the glass fiber cloth, and then carries out sintering. The method has the advantages of energy conservation, low price, safety, simplicity, stability, short time consumption and the like.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a preparation method of a vanadium dioxide film with heat-reflectivity response, which takes glass fiber cloth as a carrier and utilizes a sol-gel method to coat the surface of the carrierLoaded multilayer HxV2O5And sintering the precursor colloid at high temperature to obtain the vanadium dioxide film which takes the glass fiber as a carrier and has thermal-reflectivity response.
Preferably, the method comprises the steps of:
s1, pretreating the glass fiber cloth, and removing the impregnating compound on the surface of the glass fiber cloth;
s2, mixing V2O5Heating the powder to obtain a melt V2O5Then pouring into cold water for quenching to obtain HxV2O5Precursor colloid;
s3, immersing the glass fiber cloth processed in the step S1 in HxV2O5Taking out the precursor colloid and drying; repeating the operations of immersing and drying for multiple times;
and S4, sintering the glass fiber cloth obtained in the step S3 at a high temperature under a vacuum condition, and cooling to room temperature to obtain the vanadium dioxide film.
Preferably, in step S1, the glass fiber cloth is alkali-free E-type glass fiber cloth.
Preferably, the density of the alkali-free E-type glass fiber cloth is 100-200 m2/g。
Preferably, in step S1, the preprocessing includes: heating the glass fiber cloth for 2-2.5 hours at the temperature of 500-550 ℃; and then carrying out ultrasonic treatment for 1-2 h. The pretreatment aims at removing the impregnating compound on the surface of the glass fiber and improving the surface adsorption performance of the glass fiber; heating at 500-550 ℃ for 2-2.5 h to remove the surface impregnating compound, and performing ultrasonic treatment for 1-2 h to remove the residue of the impregnating compound adhered to the surface.
Preferably, in step S2, the heating is performed at 750-850 ℃ for 20-40 min. More preferably, the temperature is maintained at 800 ℃ for 30 min.
Preferably, said V2O5The dosage ratio of the powder to cold water is 1g (20-100) ml. More preferably 1g to 60 ml.
Preferably, in step S2, the immersion time is 8 to 12 seconds each time, and the immersion and drying operations are repeated 8 to 12 times. More preferably, the time for each immersion is 10 seconds, and the immersion and drying operations are repeated 10 times.
Preferably, in step S3, the vacuum condition is a vacuum degree less than 10-2Pa。
Preferably, in step S3, the high-temperature sintering includes: heating the mixture from room temperature to 300-600 ℃ at a heating rate of 8-10 ℃/min, and then keeping the temperature at the highest temperature for 1-5 h. More preferably, the temperature is raised to 500 ℃ at the speed of 8 ℃/min, and the temperature is kept for 1.5 h.
Preferably, the thickness of the vanadium dioxide thin film is 130-200 μm.
Preferably, the phase transition temperature of the vanadium dioxide film is 38 ℃.
The invention also relates to the application of the vanadium dioxide film prepared by the preparation method, and the vanadium dioxide film is applied to negative feedback regulation of temperature in a greenhouse.
The mechanism of the negative feedback regulation is as follows: the temperature is lower than 38 ℃, the reflectivity of the product is high, the heat reflected back to the greenhouse is high, and the temperature is increased; the temperature is higher than 38 ℃, the reflectivity of the product is low, the heat reflected back to the greenhouse is low, and the temperature is reduced; eventually, the room temperature of the greenhouse can be maintained around 38 ℃.
The vanadium dioxide film prepared by the invention has good thermo-optic response performance, and has the mutation of reflectivity near 38 ℃: when the temperature is lower than 38 ℃, the reflectivity is at a high level, and when the temperature is higher than 38 ℃, the reflectivity is at a low level, and the property is reversible; therefore, the thermal-reflectivity response of the greenhouse can be applied to negative feedback regulation of the temperature in the greenhouse, so that the indoor temperature can be maintained to be about 38 ℃, and the development of plants in the greenhouse is facilitated.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention obtains the product with 4% V by controlling the process conditions and parameters5+The doped vanadium dioxide film can reduce the phase change temperature to 38 ℃, and can be applied to a temperature negative feedback regulation system in a greenhouse. (ii) a
2. The glass fiber cloth is used as a carrier, and on one hand, the glass fiber cloth does not react with colloid in the sintering process due to the stability of the glass fiber cloth; on the other hand, the flexibility of the glass fiber cloth can make the glass fiber cloth easily paved inside the greenhouse;
3. the vanadium dioxide film has the characteristics of heat-reflectivity response, reversible performance and strong chemical stability; the glass fiber cloth can be applied to negative feedback regulation of temperature in the greenhouse by utilizing the thermal-reflectivity response, and can be produced in large scale and laid in the greenhouse conveniently by utilizing the flexibility of the glass fiber cloth;
4. the preparation method has the advantages of energy conservation, low price, safety, simplicity, stability, short time consumption and the like.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a very depth of field (VHX) diagram of the product obtained in the example of the present invention, wherein a is a macroscopic diagram of the original glass fiber, b is a macroscopic diagram of the vanadium dioxide film of the present invention, c is a macroscopic diagram of the original glass fiber, d is a macroscopic diagram of the vanadium dioxide film of the present invention, e is a macroscopic diagram of the outcrop of the original glass fiber, and f is a macroscopic diagram of the outcrop glass fiber of the attached vanadium dioxide film of the present invention;
FIG. 2 is an SEM image of a product obtained in an example of the present invention, wherein a is an SEM image of an original glass fiber, and b is an SEM image of a vanadium dioxide film of the present invention attached to a glass fiber;
FIG. 3 is an XPS plot of the product obtained in an example of the invention;
FIG. 4 is a TEM image of the product obtained in the example of the present invention;
FIG. 5 is a HRTEM and SAED image of the product obtained in the example of the present invention; wherein, a is HRTEM image, and b is SAED image;
FIG. 6 is an angle-resolved temperature-wavelength-reflectance contour plot for a product obtained in accordance with an embodiment of the present invention, with incident light being normal incidence and reflected light varying with the test angle; wherein, a is a temperature-wavelength-reflectivity contour map at a reflection angle of 0 degree, b is a temperature-wavelength-reflectivity contour map at a reflection angle of 20 degrees, c is a temperature-wavelength-reflectivity contour map at a reflection angle of 40 degrees, and d is a temperature-wavelength-reflectivity contour map at a reflection angle of 60 degrees; the reflected light varies with the change in the test angle;
FIG. 7 is a temperature-wavelength-reflectance contour plot of the product obtained in accordance with an example of the present invention;
FIG. 8 is a graph of total reflected intensity as a function of temperature for the products obtained in accordance with the examples of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
Example 1
Selecting 100m2Taking/g alkali-free E-type glass fiber cloth as a carrier, firstly, placing the carrier in a muffle furnace at 500 ℃ for heat treatment for 2h to remove the wetting agent on the surface of the glass fiber, and then, carrying out ultrasonic treatment on the treated glass fiber cloth for 1h to further remove the wetting agent remained on the surface of the glass fiber. 5g V2O5Heating the powder in a muffle furnace at 800 deg.C for 30min to obtain molten V2O5Quickly quenching in 300ml cold distilled water, stirring for 10min, filtering to remove residue to obtain brown sol solution containing H as main componentxV2O5. And (3) dipping the pretreated glass fiber cloth into the prepared sol solution for 10s, then placing the glass fiber cloth in an oven for drying, setting the temperature of the oven to be 60 ℃, and repeating the operation for 10 times to obtain the dark brown glass fiber cloth. Clamping the dark brown glass fiber cloth quartz plate, putting the quartz plate into a quartz groove, and covering the quartz groove. Carefully placing the quartz cell into a vacuum furnace, and vacuumizing to 10 DEG-2Pa. The temperature of the vacuum furnace is raised from room temperature to 500 ℃, the temperature is kept for 2h, the temperature raising rate is set to be 8 ℃/min, and then the temperature is lowered to the room temperature along with the furnace. The obtained products are shown in (b), (d) and (f) of FIG. 1. The layer of vanadium dioxide on the surface of the glass fiber cloth is very thin, so that the weaving structure of the glass fiber cloth can be seen, and the color is dark blue. As can be appreciated from the SEM image of FIG. 2, the film thickness ranged from 130 to 200 μm. As can be seen from the XPS chart of FIG. 3, it is thinThe membrane is mainly composed of V4+And V5+Is formed of wherein V4+The proportion of the water-soluble organic acid is 96 percent. As can be seen from the TEM of FIG. 4, the thickness of the thin film ranges from 130 to 200 μm; it can be seen from HRTEM of FIG. 5 that VO is in the thin film2The phase is VO with phase transition temperature2And (4) phase(s). The heat-reflectivity response performance of the product can be seen from fig. 6, 7 and 8. FIG. 6 is an angle-resolved temperature-wavelength-reflectance contour plot for a product, from which it can be seen that the thermo-reflectance response is consistent for any angle of reflected light: under the wave band of 650-850 nm, the reflectivity is in a high position when the temperature is lower than 38 ℃, and the reflectivity is reduced by about 30% when the temperature is higher than 38 ℃. It is stated that the performance of its thermo-reflectivity response does not disappear with the change in the angle of reflected light. FIG. 7 is a graph of the total temperature-wavelength-reflectance contour of the product, in accordance with the graph of FIG. 4; fig. 8 is a graph of total reflection intensity as a function of temperature, and it can be seen that the reflection intensity is abruptly changed at 38 c, and the reflection intensity is decreased by 22%. The preparation method does not need special equipment, has low energy consumption, and the obtained product has low cost.
Example 2
Selecting 120m2Taking/g alkali-free E-type glass fiber cloth as a carrier, firstly, placing the carrier in a muffle furnace at 450 ℃ for heat treatment for 3h to remove the wetting agent on the surface of the glass fiber, and then, carrying out ultrasonic treatment on the treated glass fiber cloth for 2h to further remove the wetting agent remained on the surface of the glass fiber. 5g V2O5Heating the powder in a muffle furnace at 750 deg.C for 40min to obtain molten V2O5Quickly quenching in 100ml cold distilled water, stirring for 10min, filtering to remove residue to obtain brown sol solution containing H as main componentxV2O5. And (3) dipping the pretreated glass fiber cloth in the prepared sol solution for 8s, then placing the glass fiber cloth in an oven for drying, setting the temperature of the oven to be 55 ℃, and repeating the operation for 8 times to obtain the dark brown glass fiber cloth. Clamping the dark brown glass fiber cloth quartz plate, putting the quartz plate into a quartz groove, and covering the quartz groove. Carefully placing the quartz cell into a vacuum furnace, and vacuumizing to 10 DEG-2Pa. The temperature of the vacuum furnace is raised from room temperature to 600 ℃, andkeeping the temperature for 1h, setting the heating rate to be 6 ℃/min, and then cooling to room temperature along with the furnace to obtain the product. The thermal-reflectivity response performance of the product is consistent under the reflected light of any angle by observing the equal and high relation of angle-resolved temperature-wavelength-reflectivity: under the wave band of 650-850 nm, when the temperature is lower than 38 ℃, the reflectivity is in a high position, and when the temperature is higher than 38 ℃, the reflectivity is reduced by about 25%; the relation of the total reflection intensity of the product changing with the temperature is inspected, and the reflection intensity is suddenly changed at 38 ℃, so that the reflection intensity is reduced by 20 percent.
Example 3
Selecting 80m2Taking/g alkali-free E-type glass fiber cloth as a carrier, firstly, placing the carrier in a muffle furnace at 550 ℃ for heat treatment for 1h to remove the sizing agent on the surface of the glass fiber, and then, carrying out ultrasonic treatment on the treated glass fiber cloth for 1.5h to further remove the sizing agent remained on the surface of the glass fiber. 5g V2O5Heating the powder in a muffle furnace at 850 deg.C for 20min to obtain molten V2O5Quickly quenching in 500ml cold distilled water, stirring for 10min, filtering to remove residue to obtain brown sol solution containing H as main componentxV2O5. And (3) dipping the pretreated glass fiber cloth into the prepared sol solution for 12s, then placing the glass fiber cloth in an oven for drying, setting the temperature of the oven to 65 ℃, and repeating the operation for 12 times to obtain the dark brown glass fiber cloth. Clamping the dark brown glass fiber cloth quartz plate, putting the quartz plate into a quartz groove, and covering the quartz groove. Carefully placing the quartz cell into a vacuum furnace, and vacuumizing to 10 DEG-2Pa. And (3) heating the temperature of the vacuum furnace from room temperature to 300 ℃, preserving the heat for 5 hours, setting the heating rate to be 12 ℃/min, and then cooling the temperature to room temperature along with the furnace to obtain the product. The thermal-reflectivity response performance of the product is consistent under the reflected light of any angle by observing the equal and high relation of angle-resolved temperature-wavelength-reflectivity: under the wave band of 650-850 nm, when the temperature is lower than 38 ℃, the reflectivity is in a high position, and when the temperature is higher than 38 ℃, the reflectivity is reduced by about 26 percent; the relation of the total reflection intensity of the product changing with the temperature is inspected, and the reflection intensity is changed suddenly at 38 ℃, so that the reflection intensity is reduced by 18 percent.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. The preparation method of the vanadium dioxide film with the glass fiber as the carrier and the thermal-reflectivity response is characterized in that glass fiber cloth is used as the carrier, and a sol-gel method is utilized to load multiple layers of H on the surface of the carrierxV2O5Sintering the precursor colloid at high temperature to obtain the vanadium dioxide film which takes the glass fiber as a carrier and has heat-reflectivity response; the phase transition temperature of the vanadium dioxide film is 38 ℃; the vanadium dioxide film has a sudden change in reflectance at 38 ℃: when the temperature is below 38 ℃, the reflectance is at a high level, when the temperature is above 38 ℃, the reflectance is at a low level, and this property is reversible.
2. The method for preparing the vanadium dioxide thin film with thermal-reflectivity response by using glass fiber as a carrier according to claim 1, wherein the method comprises the following steps:
s1, pretreating the glass fiber cloth, and removing the impregnating compound on the surface of the glass fiber cloth;
s2, mixing V2O5Heating the powder to obtain a melt V2O5Then pouring into cold water for quenching to obtain HxV2O5Precursor colloid;
s3, immersing the glass fiber cloth processed in the step S1 in HxV2O5Taking out the precursor colloid and drying; repeating the operations of immersing and drying for multiple times;
and S4, sintering the glass fiber cloth obtained in the step S3 at a high temperature under a vacuum condition, and cooling to room temperature to obtain the vanadium dioxide film.
3. The glass fiber supported thermal-reflective response dioxide of claim 2The preparation method of the vanadium film is characterized in that in the step S1, the glass fiber cloth is alkali-free E-shaped glass fiber cloth; the density of the alkali-free E-type glass fiber cloth is 100-200 m2/g。
4. The method for preparing vanadium dioxide thin film with thermal-reflectivity response using glass fiber as carrier according to claim 2, wherein the pre-treatment in step S1 comprises: heating the glass fiber cloth for 2-2.5 hours at the temperature of 500-550 ℃; and then carrying out ultrasonic treatment for 1-2 h.
5. The method of claim 2, wherein V is the glass fiber-supported vanadium dioxide film with thermal-reflectivity response2O5The dosage ratio of the powder to cold water is 1g (20-100) ml.
6. The method for preparing a vanadium dioxide thin film with a thermal-reflectivity response by using glass fiber as a carrier according to claim 2, wherein in step S3, the immersion time is 8-12 seconds each time, and the operations of immersion and drying are repeated 8-12 times.
7. The method for preparing vanadium dioxide film with thermal-reflectivity response using glass fiber as carrier according to claim 2, wherein the vacuum condition is less than 10 ° v in step S4-2Pa。
8. The method for preparing vanadium dioxide film with thermal-reflectivity response using glass fiber as carrier according to claim 2, wherein the high temperature sintering step S4 includes: heating the mixture from room temperature to 300-600 ℃ at a heating rate of 8-10 ℃/min, and then keeping the temperature at the highest temperature for 1-5 h.
9. The method for preparing a vanadium dioxide thin film with thermal-reflectivity response by using glass fiber as a carrier according to claim 2, wherein the thickness of the vanadium dioxide thin film is 130-200 μm.
10. The use of the vanadium dioxide film prepared by the preparation method according to claim 1, wherein the vanadium dioxide film is applied to a greenhouse for negative feedback regulation of temperature.
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