CN109292820B - VO2/ZnO double-layer film and preparation method thereof - Google Patents
VO2/ZnO double-layer film and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of nano thin film materials, and particularly relates to VO with higher infrared modulation efficiency2A/ZnO double-layer film and a preparation method thereof. The preparation method comprises the following steps:adding zinc acetate dihydrate and ethanolamine into methanol to prepare zinc oxide sol; coating a film on a substrate by a Czochralski method by using zinc oxide sol, and performing heat treatment to obtain a zinc oxide film; carrying out reduction annealing treatment on vanadium pentoxide powder in an ammonia atmosphere; mixing the obtained powder with PVP and ethanol, and ball-milling to obtain suspension; the suspension is uniformly dropped on a zinc oxide film for spin coating, VO2a/ZnO bilayer film. The invention has low cost of raw materials and relatively simple preparation process, is suitable for large-area industrial production, and prepares the obtained VO2the/ZnO double-layer film has higher solar light modulation efficiency.
Description
Technical Field
The invention belongs to the technical field of nano thin film materials, and particularly relates to VO with higher infrared modulation efficiency2A/ZnO double-layer film and a preparation method thereof.
Background
The vanadium dioxide block is a thermochromic material with extremely high application prospect, and when the temperature is lower than 68 ℃, the vanadium dioxide block is in a monoclinic system structure, and when the temperature is higher than 68 ℃, the vanadium dioxide block is in a tetragonal system. That is, the vanadium dioxide crystal undergoes a phase change after 68 ℃. The photoelectric property of vanadium dioxide is changed greatly due to the change of crystal system structure, and the change is reversible. The characteristic of reversible phase change of vanadium dioxide and the larger change of photoelectric properties before and after the phase change enable the vanadium dioxide to have wide application prospects in the aspects of photoelectric conversion materials, optical storage, laser protection and window solar control. The transmittance gradually decreases with increasing temperature, but the decrease is small, and the transmittance rapidly decreases when the temperature increases to 72 ℃. When the temperature is reduced, the transmittance is gradually increased along with the reduction of the temperature, when the temperature is reduced to 63 ℃, the transmittance is rapidly increased, and when the temperature is reduced to 56 ℃, the transmittance is restored to the value before the temperature is increased, and a cycle is completed.
At present, the main problems of vanadium dioxide as an intelligent window film are as follows: the phase transition temperature is higher than room temperature (68 ℃); the solar light modulation capability is limited (less than 10%); the sunlight transmittance difference before and after the phase change is small.
Zinc oxide (ZnO) is a traditional metal oxide semiconductor material, has unique performances of photoelectricity, thermoelectricity, piezoelectricity and the like, and has the advantages of wide band gap, high exciton confinement energy, strong radiation resistance, good thermal stability, simple and various preparation methods, rich and cheap preparation raw materials, environmental friendliness and the like. The zinc oxide film is an ideal transparent conductive film with high visible light transmittance and the resistivity of the film is as low as 10-4Omega cm, has good application prospect in various fields such as solar cells, ultraviolet light detection and the like; on the other hand, the zinc oxide is also used for preparing a gas sensor, and has a great prospect when being applied to the gas sensor; meanwhile, the zinc oxide is an excellent material for preparing pressure and acceleration sensors. The process for preparing zinc oxide film is compatible with integrated circuit process, and can be integrated with various semiconductor devices such as silicon, etc., so that it is greatly appreciated by people.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a VO with higher infrared modulation efficiency2A/ZnO double-layer film and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
VO with higher infrared modulation efficiency2The preparation method of the/ZnO double-layer film comprises the following steps:
(1) preparing zinc oxide sol: adding zinc acetate dihydrate into methanol, stirring for a period of time, adding ethanolamine, and continuing stirring until the solution is clear to obtain zinc oxide sol;
(2) preparing a zinc oxide film: soaking a substrate in the zinc oxide sol obtained in the step (1), coating a film by adopting a pulling method, heating on a heating plate to prevent the shrinkage of the film, repeating the steps to obtain a zinc oxide precursor film with a certain thickness, and then putting the zinc oxide precursor film into a tubular furnace for heat treatment to obtain a zinc oxide film;
(3) preparation of VO2Powder: weighing a proper amount of vanadium pentoxide powder and ammonium bicarbonate, placing the vanadium pentoxide powder and the ammonium bicarbonate into a crucible, and carrying out vacuum annealing on the crucible in a vacuum furnace to obtain VO2Pulverizing, and mixing with VO2Mixing the powder with polyvinylpyrrolidone (PVP) and ethanol, ball-milling, centrifuging the obtained mixed solution, and drying the suspension to obtain powder;
(4) uniformly mixing the powder obtained in the step (3) with absolute ethyl alcohol to prepare coating liquid, uniformly dripping the coating liquid on a ZnO film for coating by a spin coating method, and drying to obtain VO2a/ZnO bilayer film.
In the scheme, the mass-to-volume ratio of the zinc acetate dihydrate in the step (1) to the ethanolamine is 5.4876g: 1.5-2.0 mL, and the stirring time is 10-20 h.
In the scheme, the soaking time in the step (2) is 2-3 min, the coating times by the pulling method are 1-3 times, the heating temperature on the heating plate is 300-350 ℃, and the time is 10-30 min.
In the scheme, the heat treatment temperature in the step (2) is 350-400 ℃, and the heat treatment time is 1-1.5 h.
In the scheme, the mass ratio of the vanadium pentoxide powder to the ammonium bicarbonate in the step (3) is 2:1 to 2: 1.5.
In the scheme, the temperature of the vacuum annealing in the step (3) is 450-480 ℃, and the time is 30-60 min.
In the scheme, VO is generated in the ball milling process in the step (3)2The mass ratio of the powder to the polyvinylpyrrolidone (PVP) is 2: 1-1: 1.
In the scheme, the coating process of the spin-coating method in the step (4) is 500-1000 r/min, and the drying time is 5-10 min.
The invention has the following beneficial effects: 1) in the method, the raw materials are simple, the cost is low, and VO2The film is simple in preparation process, and can be prepared by taking vanadium pentoxide as a raw material through one-time annealing and one-time ball milling; the zinc oxide film is prepared by taking zinc acetate dihydrate and ethanolamine as raw materials, the process is simple, and a double-layer film can be prepared by only using a pulling method and a spin-coating method for several times; the requirement on equipment is low; 2) VO prepared by the invention2the/ZnO double-layer film material is characterized in thatThe wide bandgap semiconductor property and the antireflection characteristic of the zinc oxide enable the double-layer film to have better visible light transmittance regulation and control capability, and compared with the traditional vanadium dioxide film, the VO prepared by the method provided by the invention2the/ZnO double-layer film material not only has better visible light transmittance regulation and control capability, but also has higher infrared modulation efficiency.
Drawings
FIG. 1 shows VO prepared in example 1 of the present invention2X-ray diffraction (XRD) pattern of/ZnO bilayer film.
FIG. 2 shows VO prepared in example 1 of the present invention2Sectional Scanning Electron Micrographs (SEM) of the/ZnO bilayer films.
FIG. 3 shows VO prepared in example 1 of the present invention2Visible-infrared transmittance spectrogram of the/ZnO double-layer film at different temperatures.
FIG. 4 shows VO prepared in example 1 of the present invention2And/photographing the ZnO double-layer film.
FIG. 5 shows VO prepared in example 2 of the present invention2Visible-infrared transmittance spectrograms of the/ZnO double-layer film at different temperatures.
FIG. 6 shows VO prepared in example 2 of the present invention2And/photographing the ZnO double-layer film.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
VO with higher infrared modulation efficiency2The preparation method of the/ZnO double-layer film comprises the following steps:
1) preparing zinc oxide sol: weighing 5.4876g of zinc acetate dihydrate, adding into a beaker, adding 50mL of methanol, stirring for 30min, adding 1.5mL of ethanolamine, and continuing stirring for 2 h;
2) coating a film by a clean soda-lime-silica glass pulling method, soaking the glass in zinc oxide sol for 2min, taking out the glass to wipe off one unnecessary surface, and heating the glass on a heating plate at 350 ℃ for 30 min;
3) transferring the film obtained in the step 2) into a muffle furnace, and annealing at 350 ℃ for 1h to obtain a zinc oxide film;
4) weighing 0.5g of vanadium pentoxide and 0.25g of ammonium bicarbonate, and placing the vanadium pentoxide and the ammonium bicarbonate into a crucible;
5) placing the crucible filled with the vanadium pentoxide and the ammonium bicarbonate in a vacuum furnace with the vacuum degree of 50pa, heating to 450 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and cooling to room temperature along with the furnace after the heat preservation is finished to obtain M-phase vanadium dioxide powder;
6) grinding and mixing 0.3g of the M-phase vanadium dioxide powder obtained in the step 5) with 0.15g of PVP and 8ml of ethanol solution for 8 hours, centrifuging the mixed solution at the rotating speed of 8000r/min for 4min, and drying the suspension;
7) taking 0.1g of the dried powder obtained in the step 6), adding 0.9g of absolute ethyl alcohol, performing ultrasonic dispersion for 20min, stirring for 20min under magnetic force to obtain a coating liquid, and spin-coating for 30s at 500r/min on a common soda-lime-silica glass substrate plated with a zinc oxide film by adopting a spin-coating method to prepare a film; coating the film, and drying at 80 deg.C for 5min to obtain VO2a/ZnO bilayer film.
In order to control the prepared VO2the/ZnO double-layer film is more intuitively understood and is characterized by X-ray diffraction (XRD), Scanning Electron Microscope (SEM) and visible-infrared transmittance detector, as shown in figure 1, the XRD pattern of the embodiment of the invention is shown, and the figure shows that the product contains VO2Because the ZnO thin film is thin, the diffraction peak of ZnO is difficult to detect in an XRD (X-ray diffraction) pattern; as shown in FIG. 2, which is an SEM image of an example of the present invention, a section of a double-layered thin film is taken as a shot part, and VO can be seen2The thickness of the film is about 1500nm, while the thickness of the ZnO film at the lower layer is only about 100nm, and the film is relatively uniform; as shown in fig. 3, which is a visible-infrared transmittance spectrogram at different temperatures according to the embodiment of the present invention, it can be seen from the chart that the visible light transmittance of the film is high, the solar modulation efficiency is as high as 20.69% by calculating the visible light transmittance and the solar modulation efficiency of the film, and the calculated visible light transmittance still reaches 50.99%, which indicates that the film has excellent heat-to-color change performance and high transmittance; FIG. 4 shows VO in example 12The uniformity of the visible film is relatively high in the photographed picture of the/ZnO double-layer filmGood results are obtained.
Example 2
VO with higher infrared modulation efficiency2The preparation method of the/ZnO double-layer film comprises the following steps:
1) preparing zinc oxide sol: weighing 5.4876g of zinc acetate dihydrate, adding into a beaker, adding 50mL of methanol, stirring for 30min, adding 2.0mL of ethanolamine, and continuing stirring for 3 h;
2) coating the film by a clean soda-lime-silica glass pulling method, soaking the glass in zinc oxide sol for 3min, taking out the glass to wipe off one unnecessary surface, and heating the glass on a heating plate at 350 ℃ for 1 h: the second coating dipping time is 3min, the heating is carried out at 350 ℃ for 30min, the third coating dipping time is 3min, and then the heating is carried out on a heating plate for 10 min;
3) transferring the film obtained in the step 2) into a muffle furnace, and annealing at 350 ℃ for 1h to obtain a zinc oxide film;
4) weighing 0.5g of vanadium pentoxide and 0.375g of ammonium bicarbonate, and placing the vanadium pentoxide and the ammonium bicarbonate into a crucible;
5) placing the crucible filled with the vanadium pentoxide and the ammonium bicarbonate in a vacuum furnace with the vacuum degree of 50pa, heating to 480 ℃ at the speed of 10 ℃/min, preserving heat for 60min, and cooling to room temperature along with the furnace after the heat preservation is finished to obtain M-phase vanadium dioxide powder;
6) grinding and mixing 0.3g of the powder obtained in the step 5) with 0.15g of PVP and 8mL of ethanol solution for 9h, centrifuging the mixed solution at the rotating speed of 10000r/min for 5min, and drying the suspension;
7) adding 0.1g of the dried powder obtained in the step 6) into 0.9g of absolute ethyl alcohol for ultrasonic dispersion for 20min, then performing magnetic stirring for 20min to obtain a coating liquid, spin-coating the coating liquid on a common soda-lime-silica glass substrate plated with a zinc oxide film at 500r/min for 10s and at 1000r/min for 20s to prepare a film, drying the film on a heating plate at 80 ℃ for 10min after coating to obtain VO2a/ZnO bilayer film.
In order to control the prepared VO2the/ZnO double-layer film has more intuitive understanding, and is characterized by adopting a visible-infrared transmittance detector, as shown in figure 5, a visible-infrared transmittance spectrogram of the invention at different temperatures is shown, and the visible light transmittance of the film can be known from the visible light transmittance spectrogramThe transmittance is high, the solar light modulation efficiency still reaches 18.24 percent by calculating the visible light transmittance and the solar light modulation efficiency of the film, the visible light transmittance obtained by calculation reaches 55.91 percent, the visible light transmittance is improved along with the increase of the number of zinc oxide film layers, and the thermochromic performance of the film is relatively balanced and excellent; FIG. 6 shows VO in example 22The uniformity of the visible film is better when the picture is taken of the/ZnO double-layer film.
It is apparent that the above embodiments are only examples for clearly illustrating and do not limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are therefore intended to be included within the scope of the invention as claimed.
Claims (7)
1. VO with higher infrared modulation efficiency2The preparation method of the/ZnO double-layer film is characterized by comprising the following steps:
(1) preparing zinc oxide sol: adding zinc acetate dihydrate into methanol, stirring for a period of time, adding ethanolamine, and continuing stirring until the solution is clear to obtain zinc oxide sol;
(2) preparing a zinc oxide film: soaking a substrate in the zinc oxide sol obtained in the step (1), coating a film by adopting a pulling method, heating on a heating plate to prevent the shrinkage of the film, repeating the steps to obtain a zinc oxide precursor film with a certain thickness, and then putting the zinc oxide precursor film into a tubular furnace for heat treatment to obtain a zinc oxide film;
(3) preparation of VO2Powder: weighing a proper amount of vanadium pentoxide powder and ammonium bicarbonate, placing the vanadium pentoxide powder and the ammonium bicarbonate into a crucible, and carrying out vacuum annealing on the crucible in a vacuum furnace to obtain VO2Pulverizing, and mixing with VO2Mixing the powder with polyvinylpyrrolidone and ethanol, ball-milling, centrifuging the obtained mixed solution, and drying the suspension to obtain powder; the temperature of the vacuum annealing is 450-480 ℃, and the time is 30-60 min;
(4) uniformly mixing the powder obtained in the step (3) with absolute ethyl alcohol to prepare coating liquid, uniformly dripping the coating liquid on a ZnO film for coating by a spin coating method, and drying to obtain VO2a/ZnO bilayer film.
2. The preparation method according to claim 1, wherein the mass-to-volume ratio of the zinc acetate dihydrate in step (1) to the ethanolamine is 5.4876g: 1.5-2.0 mL.
3. The preparation method according to claim 1, wherein the coating by the Czochralski method in the step (2) is performed 1-3 times, the heating temperature on the heating plate is 300-350 ℃, and the heating time is 10-30 min.
4. The method according to claim 1, wherein the heat treatment in step (2) is performed at a temperature of 350 to 400 ℃ for 1 to 1.5 hours.
5. The preparation method according to claim 1, wherein the mass ratio of the vanadium pentoxide powder to the ammonium bicarbonate in step (3) is 2:1 to 2: 1.5.
6. The method according to claim 1, wherein VO is generated during the ball milling process in the step (3)2The mass ratio of the powder to the polyvinylpyrrolidone is 2: 1-1: 1.
7. The preparation method according to claim 1, wherein the spin coating process in step (4) is 500-1000 r/min, and the drying time is 5-10 min.
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