CN114988717A - Monodisperse vanadium dioxide nanoparticle coating and preparation method thereof - Google Patents
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Abstract
The invention discloses a monodisperse vanadium dioxide nanoparticle coating, which is formed by randomly distributing ellipsoidal vanadium dioxide nanoparticles in a monodisperse state; the coating has a single-layer structure and the thickness is about 30-70 nm; the three-dimensional size distribution of the ellipsoidal vanadium dioxide nanoparticles is 20-200 nm, the particles are separated by air, and the horizontal distance is 50-300 nm; the preparation process comprises the steps of mixing a pentavalent vanadium compound and oxalic acid dihydrate in deionized water for oxidation-reduction reaction to prepare vanadyl oxalate solution; adding a template agent into the vanadyl oxalate aqueous solution, fully stirring and then carrying out ultrasonic treatment to obtain uniform and stable coating liquid; uniformly spin-coating the obtained coating liquid on a cleaned glass substrate, and drying to obtain a precursor film; and placing the obtained precursor film in a tube furnace for annealing to obtain the monodisperse vanadium dioxide nanoparticle coating.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a monodisperse vanadium dioxide nanoparticle coating.
Background
Vanadium dioxide (VO) 2 ) It is considered to be a very promising thermochromic material because it undergoes a reversible phase transition from a high-temperature metallic phase (R phase) to a low-temperature semiconducting phase (M phase) at around 68 ℃, its crystal structure changes from a tetragonal rutile structure to a monoclinic structure, and the electrical, optical and magnetic properties of vanadium dioxide undergo abrupt changes with the change in crystal structure. The series of special properties enable the M-phase vanadium dioxide to show considerable application prospects in the fields of intelligent windows, thermistor switches, infrared detectors, photoelectric switch materials and the like. Wherein, researchers widely research the application of the intelligent window in the field of intelligent windows because the vanadium dioxide film-based thermochromic intelligent window has excellent energy-saving performance.
The problems disturbing the application of the vanadium dioxide thin film in the field of intelligent windows at present are that the intrinsic vanadium dioxide thin film has poor optical performance, including low visible light transmittance and unsatisfactory solar light regulation efficiency, and the application requirements of the intelligent windows are difficult to meet (the visible light transmittance is higher than 60 percent, and the solar light regulation efficiency is higher than 10 percent). In order to solve these problems, scientific research technicians have adopted various methods including preparation of porous vanadium dioxide films, vanadium dioxide composite films, multilayer films, doped vanadium dioxide films, and the like. The design and preparation of the porous film are considered to be the most effective method for improving the visible light transmittance of the vanadium dioxide film, and the principle of increasing the visible light transmittance is to reduce the refractive index of the film by increasing the content of air holes in the film. However, the traditional porous film can only improve the visible light transmittance of the film, but cannot improve the sunlight regulation efficiency of the film at the same time. The film thickness can only be increased in order to increase the solar light regulation efficiency of the film, but the increase of the film thickness in turn reduces the visible light transmittance of the film, and the visible light transmittance and the solar light regulation efficiency of the film cannot be simultaneously improved to obtain the vanadium dioxide film with excellent optical performance.
Disclosure of Invention
The invention aims to provide a monodisperse vanadium dioxide nanoparticle coating and a preparation method thereof, wherein the coating not only has excellent visible light transmittance, but also has considerable sunlight regulation efficiency.
In order to achieve the purpose, the technical scheme is as follows:
a monodisperse vanadium dioxide nanoparticle coating is formed by randomly distributing ellipsoidal vanadium dioxide nanoparticles in a monodisperse state; the coating has a single-layer structure and the thickness is about 30-70 nm;
the three-dimensional size distribution of the ellipsoidal vanadium dioxide nanoparticles is 20-200 nm, the particles are separated by air, and the horizontal distance is 50-300 nm.
The preparation method of the monodisperse vanadium dioxide nanoparticle coating comprises the following steps:
1) mixing a pentavalent vanadium compound and oxalic acid dihydrate in deionized water to carry out redox reaction to prepare vanadyl oxalate solution; adding a template agent into the vanadyl oxalate aqueous solution, fully stirring and then carrying out ultrasonic treatment to obtain uniform and stable coating liquid;
2) uniformly spin-coating the obtained coating liquid on a cleaned glass substrate, and drying to obtain a precursor film;
3) and placing the obtained precursor film in a tube furnace for annealing to obtain the monodisperse vanadium dioxide nanoparticle coating.
According to the scheme, the pentavalent vanadium compound in the step 1) is one of vanadium pentoxide and metavanadate.
According to the scheme, the molar ratio of the pentavalent vanadium compound to oxalic acid dihydrate in the step 1) is 1: (1-3).
According to the scheme, in the step 1), the redox reaction is carried out for 2-12 h at the temperature of 80-120 ℃.
According to the scheme, the concentration of the vanadyl oxalate aqueous solution in the step 1) is 0.05-0.5 mol/L.
According to the scheme, the template agent in the step 1) is one or a mixture of more than two of polyethylene glycol, amino resin and polyvinylpyrrolidone, and the addition amount of the template agent is 2-10% of the mass of the vanadyl oxalate aqueous solution.
According to the scheme, the spin coating process in the step 2) is two-step spin coating, wherein the first step of spin coating is performed at the rotating speed of 500r/min for 10s, and the second step of spin coating is performed at the rotating speed of 2000-5000 r/min for 20-30 s; the drying temperature of the film is 60-100 ℃.
According to the scheme, the annealing temperature in the step 3) is 490-600 ℃, and the time is 30-120 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention directly prepares the monodisperse vanadium dioxide nano-particle coating on the substrate by adopting a simple solution method, the nano-vanadium dioxide particles in the coating are highly dispersed, the crystallinity is good, the particle size is small, and obvious air gaps exist among the particles. The coating with the structure has very high visible light transmittance due to the small refractive index, and meanwhile, the monodisperse vanadium dioxide nano particles show excellent local surface plasma resonance effect when the high-temperature phase is changed into the metal phase, so that the coating can absorb near infrared light at high temperature, the sunlight regulation efficiency of the coating is improved, and the purpose of simultaneously improving the visible light transmittance and the sunlight regulation efficiency is achieved. When the visible light transmittance of the coating is 72.5%, the coating also has 10.1% of sunlight regulation efficiency, and the excellent optical performance enables the coating to meet the application requirements of the vanadium dioxide intelligent window.
The vanadium dioxide particles and the sizes of the gaps in the coating have larger influence on the optical performance of the coating, the smaller the vanadium dioxide particles in the invention, the smaller the occupied space, the larger the gaps, and the sizes of the particles and the gaps can be easily adjusted by changing a plurality of preparation conditions. If the particle size can be reduced and the gap can be increased by reducing the concentration of the vanadyl oxalate solution, reducing the thickness of the film before annealing or increasing the dosage of the template agent, the optical performance of the coating is further optimized, and the vanadium dioxide coating can meet the application requirements of different fields.
The raw materials are simple and easy to obtain, the solution method has low requirements on equipment, the operation is simple and convenient, and the cost is low. Therefore, the method is suitable for large-scale production. And the method can be copied and popularized for preparing other metal oxide coatings with the same structure, and has universality.
Drawings
FIG. 1: XRD pattern of the monodisperse vanadium dioxide nanoparticle coating prepared in example 1.
FIG. 2: SEM image of monodisperse vanadium dioxide nanoparticle coating prepared in example 1.
FIG. 3: the high and low temperature ultraviolet-visible-near infrared transmittance graph of the monodisperse vanadium dioxide nanoparticle coating prepared in example 1.
FIG. 4: SEM image of monodisperse vanadium dioxide nanoparticle coating prepared in example 2.
FIG. 5: the high and low temperature ultraviolet-visible-near infrared light transmittance graph of the monodisperse vanadium dioxide nanoparticle coating prepared in example 2.
FIG. 6: the high and low temperature ultraviolet-visible-near infrared transmittance graph of the monodisperse vanadium dioxide nanoparticle coating prepared in example 3.
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
The specific embodiment provides a monodisperse vanadium dioxide nanoparticle coating which is formed by randomly distributing ellipsoidal vanadium dioxide nanoparticles in a monodisperse state; the coating has a single-layer structure and the thickness is about 30-70 nm; the three-dimensional size distribution of the ellipsoidal vanadium dioxide nanoparticles is 20-200 nm, the particles are separated by air, and the horizontal distance is 50-300 nm.
The specific embodiment also provides a preparation method of the monodisperse vanadium dioxide nanoparticle coating, which comprises the following steps:
1) mixing a pentavalent vanadium compound and oxalic acid dihydrate in deionized water to carry out redox reaction to prepare vanadyl oxalate solution; adding a template agent into the vanadyl oxalate aqueous solution, fully stirring and then carrying out ultrasonic treatment to obtain uniform and stable coating liquid;
2) uniformly spin-coating the obtained coating liquid on a cleaned glass substrate, and drying to obtain a precursor film;
3) and placing the obtained precursor film in a tube furnace for annealing to obtain the monodisperse vanadium dioxide nanoparticle coating.
Specifically, the pentavalent vanadium compound in the step 1) is one of vanadium pentoxide and metavanadate; the molar ratio of the pentavalent vanadium compound to oxalic acid dihydrate is 1: (1-3). The redox reaction is carried out for 2-12 h at 80-120 ℃. The concentration of the vanadyl oxalate aqueous solution is 0.05-0.5 mol/L. The template agent is one or a mixture of more than two of polyethylene glycol, amino resin and polyvinylpyrrolidone, and the addition amount of the template agent is 2-10% of the mass of the vanadyl oxalate aqueous solution.
Specifically, the spin coating process in the step 2) is two-step spin coating, wherein the first step is performed at a rotating speed of 500r/min for 10s, and the second step is performed at a rotating speed of 2000-5000 r/min for 20-30 s. The drying temperature of the film is 60-100 ℃.
Specifically, the annealing temperature in the step 3) is 490-600 ℃, and the time is 30-120 min.
Example 1
1) Weighing 0.455g of vanadium pentoxide and 0.9455g of oxalic acid dihydrate, adding the weighed materials into 160ml of deionized water to obtain a mixed solution, reacting the mixed solution at 80 ℃ for 120min to obtain an vanadyl oxalate aqueous solution, adding a template agent polyvinylpyrrolidone with the mass of 6% of the solution into the vanadyl oxalate aqueous solution, fully stirring for 1h, and carrying out ultrasonic treatment for 1h until the polyvinylpyrrolidone is completely dissolved to obtain a uniform coating solution;
2) uniformly dripping the coating liquid obtained in the step 1) on a cleaned glass substrate, spin-coating and coating by a process of rotating at 500r/min for 10s and then rotating at 3000r/min for 20s, and placing the coated glass substrate on a heating table and drying at 80 ℃ for 20min to obtain a dry precursor film.
3) And (3) annealing the dried precursor film obtained in the step 2) in a tubular furnace at the annealing temperature of 500 ℃ for 1h to obtain the monodisperse vanadium dioxide nanoparticle coating.
Example 2
1) Weighing 0.455g of vanadium pentoxide and 0.9455g of oxalic acid dihydrate, adding the weighed materials into 250ml of deionized water to obtain a mixed solution, reacting the mixed solution at 80 ℃ for 120min to obtain an vanadyl oxalate aqueous solution, adding a template agent polyvinylpyrrolidone with the mass of 6% of the solution into the vanadyl oxalate aqueous solution, fully stirring for 1h, and carrying out ultrasonic treatment for 1h until the polyvinylpyrrolidone is completely dissolved to obtain a uniform coating solution;
2) uniformly dripping the coating liquid obtained in the step 1) on a cleaned glass substrate, spin-coating for coating by a process of rotating for 10s at 500r/min and then rotating for 20s at 4000r/min, and placing the coated glass substrate on a heating table for drying for 20min at 80 ℃ to obtain a dry precursor film.
3) And (3) annealing the dried precursor film obtained in the step 2) in a tubular furnace at the annealing temperature of 500 ℃ for 1h to obtain the monodisperse vanadium dioxide nanoparticle coating.
Example 3
1) Weighing 0.455g of vanadium pentoxide and 0.9455g of oxalic acid dihydrate, adding the weighed materials into 500ml of deionized water to obtain a mixed solution, reacting the mixed solution at 80 ℃ for 120min to obtain an vanadyl oxalate aqueous solution, adding a template agent polyvinylpyrrolidone with the mass of 6% of the solution into the vanadyl oxalate aqueous solution, fully stirring for 1h, and carrying out ultrasonic treatment for 1h until the polyvinylpyrrolidone is completely dissolved to obtain a uniform coating solution;
2) uniformly dripping the coating liquid obtained in the step 1) on a cleaned glass substrate, spin-coating and coating by a process of rotating at 500r/min for 10s and then rotating at 3500r/min for 20s, and placing the coated glass substrate on a heating table and drying at 80 ℃ for 20min to obtain a dry precursor film.
3) And (3) annealing the dried precursor film obtained in the step 2) in a tubular furnace at the annealing temperature of 550 ℃ for 1h to obtain the monodisperse vanadium dioxide nanoparticle coating.
In order to fully understand the structural composition and properties of the monodisperse vanadium dioxide nanoparticle coating prepared in the examples.
And carrying out structure and performance tests on the vanadium dioxide coating obtained in the embodiment, wherein the structure and performance tests comprise X-ray diffraction analysis, a field emission scanning electron microscope and a variable-temperature ultraviolet-visible near-infrared spectrophotometer.
1. X-ray diffraction analysis; an Empyrean X-ray diffraction analyzer from parnacho, the netherlands, with a copper target Cu-K α as a radiation source (λ: 0.154178nm), a nominal output of 4KW, a scanning range of 10-80 °, and a scanning speed of 5 ° per minute.
2. A field emission scanning electron microscope; the surface morphology of the coating was tested by Zeiss Ultra Plus type field emission scanning electron microscope, Zeiss, Germany.
3. A variable temperature ultraviolet visible near infrared spectrophotometer; the UV-3600 type ultraviolet visible near infrared spectrophotometer of Shimadzu corporation of Japan is additionally provided with a programmable temperature rise and fall control device, the transmittance of the coating before and after phase change in the wavelength range of 300-2500nm is respectively tested, and parameters such as visible light transmittance, sunlight regulation efficiency and the like are calculated according to the following integral formula.
T lum/sol ＝∫φ lum/sol (λ)T(λ)dλ/∫φ lum/sol (λ)dλ
ΔT sol ＝T sol (M phase) -T sol (R phase)
Fig. 1 is an XRD chart of the monodisperse vanadium dioxide nanoparticle coating obtained in example 1, from which it can be seen that the diffraction peaks correspond to those of a standard M-phase vanadium dioxide card, illustrating that a vanadium dioxide coating with thermochromic properties is obtained in the present application.
Fig. 2 is an SEM image of the monodisperse vanadium dioxide nanoparticle coating obtained in example 1, and it can be seen from the SEM image that the vanadium dioxide nanoparticles in the coating are in a monodisperse state, and there are large gaps between particles, which is beneficial to improving the visible light transmittance and the solar light modulation efficiency of the coating.
FIG. 3 is a high and low temperature UV-Vis-NIR transmittance spectrum of the monodisperse vanadium dioxide nanoparticle coating obtained in example 1, which shows that the visible light transmittance (380-780nm) of the coating is relatively high. And because the vanadium dioxide nano particles in the coating are in a monodisperse state, the coating has an excellent local surface plasmon resonance effect, and is shown in that a near infrared light region on a transmittance spectrum (90 ℃) has obvious absorption peak valley. The calculation shows that the visible light transmittance of the coating is 72.5%, the solar light adjusting efficiency is 10.1%, and the application requirement of the vanadium dioxide intelligent window is met.
FIG. 4 is an SEM image of the coating of monodisperse vanadium dioxide nanoparticles obtained in example 2, and it can be seen that the vanadium dioxide nanoparticles in the coating are also in a monodisperse state, and the vanadium dioxide particles in the coating have smaller size and larger gaps between the particles compared with example 1.
FIG. 5 is a high and low temperature UV-VIS-NIR transmittance spectrum of the monodisperse vanadium dioxide nanoparticle coating obtained in example 2. it can be seen that, due to the larger porosity and the smaller particle size, the visible light transmittance (380-780nm) of the coating is higher than that of example 1, and the calculated visible light transmittance is as high as 81.5%. The monodisperse vanadium dioxide nano particles in the coating layer also have excellent local surface plasmon resonance effect, and the expression is more obvious due to the smaller size of the vanadium dioxide particles, and the sunlight regulation efficiency obtained by calculation is 9.5%.
Fig. 6 is a high and low temperature uv-vis-nir transmittance spectrum of the monodisperse vanadium dioxide nanoparticle coating obtained in example 3, with the calculated visible light transmittance as high as 97.3% and the solar light regulation efficiency of 4%. In conclusion, the monodisperse vanadium dioxide nanoparticle coating prepared by the method has excellent optical performance and adjustable performance and structure. The raw materials listed in the invention, the upper and lower limits and interval values of the raw materials of the invention, and the upper and lower limits and interval values of the process parameters (such as temperature, time and the like) can all realize the invention, and the examples are not listed.
Claims (9)
1. A monodisperse vanadium dioxide nanoparticle coating is characterized in that ellipsoidal vanadium dioxide nanoparticles are randomly distributed in a monodisperse state; the coating has a single-layer structure and the thickness is about 30-70 nm;
the three-dimensional size distribution of the ellipsoidal vanadium dioxide nanoparticles is 20-200 nm, the particles are separated by air, and the horizontal distance is 50-300 nm.
2. The monodisperse vanadium dioxide nanoparticle coating of claim 1, wherein the monodisperse vanadium dioxide nanoparticle coating is prepared by a method comprising the steps of:
1) mixing a pentavalent vanadium compound and oxalic acid dihydrate in deionized water to carry out redox reaction to prepare vanadyl oxalate solution; adding a template agent into the vanadyl oxalate aqueous solution, fully stirring and then carrying out ultrasonic treatment to obtain uniform and stable coating liquid;
2) uniformly spin-coating the obtained coating liquid on a cleaned glass substrate, and drying to obtain a precursor film;
3) and placing the obtained precursor film in a tube furnace for annealing to obtain the monodisperse vanadium dioxide nanoparticle coating.
3. The monodisperse vanadium dioxide nanoparticle coating of claim 1, wherein the pentavalent vanadium compound in step 1) is one of vanadium pentoxide and metavanadate.
4. The monodisperse vanadium dioxide nanoparticle coating of claim 1, characterized in that the molar ratio of pentavalent vanadium compound to oxalic acid dihydrate in step 1) is 1: (1-3).
5. The monodisperse vanadium dioxide nanoparticle coating of claim 1, wherein the redox reaction in step 1) is carried out at 80-120 ℃ for 2-12 h.
6. The monodisperse vanadium dioxide nanoparticle coating of claim 1, wherein the concentration of the aqueous solution of vanadyl oxalate in step 1) is 0.05 to 0.5 mol/L.
7. The monodisperse vanadium dioxide nanoparticle coating of claim 1, wherein the template in step 1) is one or a mixture of two or more of polyethylene glycol, amino resin and polyvinylpyrrolidone, and the amount of the template added is 2-10% of the mass of the vanadyl oxalate solution.
8. The monodisperse vanadium dioxide nanoparticle coating of claim 1, wherein the spin coating process in step 2) is a two-step spin coating, wherein the first step is performed at a speed of 500r/min for a time of 10s, and the second step is performed at a speed of 2000-5000 r/min for a time of 20-30 s. The drying temperature of the film is 60-100 ℃.
9. The monodisperse vanadium dioxide nanoparticle coating of claim 1, wherein the annealing temperature in step 3) is 490-600 ℃ for 30-120 min.
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