CN106745253A - A kind of preparation method of M phase hypovanadic oxides - Google Patents
A kind of preparation method of M phase hypovanadic oxides Download PDFInfo
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- CN106745253A CN106745253A CN201710126410.4A CN201710126410A CN106745253A CN 106745253 A CN106745253 A CN 106745253A CN 201710126410 A CN201710126410 A CN 201710126410A CN 106745253 A CN106745253 A CN 106745253A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention relates to a kind of preparation method of M phase hypovanadic oxides, including presoma is prepared and two steps of hydrothermal crystallizing, it is characterised in that prepared presoma directly carries out hydrothermal crystallizing without isolation, wherein, the preparation method of presoma be selected from it is following any one：(A) soluble vanadic salts is soluble in water, after adding reducing agent, reaction to terminate, heating steams solvent, is subsequently adding water, and ultrasonic disperse obtains forerunner's dispersion liquid；(B) soluble vanadic salts and complexant are together added to the water, dissolving forms precursor.Hydrothermal crystallization process of the invention does not have gas to generate, therefore, the solid content of the presoma of hydro-thermal process can be very high, is adapted to industrial-scale production, production cost and improve production efficiency can be directly reduced, to meet the demand of practical application.
Description
Technical field
The invention belongs to technical field of function materials, it is related to a kind of preparation method of M phase hypovanadic oxides.
Background technology
M phase hypovanadic oxides have metal-insulator transition characteristic, when temperature is increased to phase transition temperature, VO2Will be from low
Warm monoclinic phase is changed into high temperature Tetragonal, and this phase transformation is reversible.Before and after phase transformation, in infrared light district, its optical property
Great changes will take place, i.e., be changed into infrared ray obstruct from infrared transmission.Therefore, with the change of environment temperature, based on titanium dioxide
The film of vanadium can be realized regulating and controlling the infrared ray in sunshine, it is had very big use in smart window.
The dispersiveness of the phase purity of powder, degree of crystallization, granular size and particle will directly affect VO2Phase transformation control
Energy.And as the practical application on smart window pad pasting, high-quality VO2The synthesis of the large-scale low-cost of powder, is that it is crucial
Place.Report that various methods prepare VO at present2Dusty material.But it is difficult a step and prepares the M phases two with thermal induced phase transition performance
Vanadium oxide powder, the powder of preparation is difficult to take into account the Optimum Matching of phase purity, particle diameter and dispersiveness, and key is difficult extensive low
Cost synthesizes.Hydro-thermal method can realize controllable growth of the crystal in reaction system, and the powder for synthesizing at high temperature under high pressure has
The advantages of well-crystallized, good dispersion, therefore be also used to synthesize M phase hypovanadic oxides.As patent CN101830510B utilizes water
Heat hair synthesis wire M phase hypovanadic oxide nanobelts.Hydro-thermal reaction is carried out in an enclosed system, so in hydro-thermal process work
Need to avoid the generation of a large amount of gases in journey, the moment pressure that otherwise a large amount of gases are produced will likely cause the blast of reactor,
So as to cause production accident.Therefore, in the hydro-thermal reaction for thering is gas to generate, concentration generally all very low, the institute of precursors
With large-scale production difficult to realize.And in existing M phase hypovanadic oxides hydro-thermal preparation system, such as V2O5With oxalic acid system or with urea
Sluggish precipitation (patent CN103880080A) as precipitating reagent etc., has gas to generate, therefore, the concentration of reaction system is not
Can be too high, so that large-scale industrial production difficult to realize.A kind of liquid phase method is disclosed in patent CN102616849B and is directly synthesized M
The method of phase hypovanadic oxide nano particle, is that one or two the mixture in vanadic anhydride and metavanadate is poured into steaming
Suspension is made in distilled water, reducing agent is then added dropwise, isothermal reaction obtains precursor substance, then carried out hydro-thermal process and produced
Thing.The patent is to carry out hydro-thermal reaction in acid condition, may determine that the particle diameter of products obtained therefrom is larger from its XRD result,
And do not meet nanometer product small particle requirement, also, in acid condition presoma be very easy to dissolving, it is difficult to obtain target
Product.In addition, product is centrifuged being precipitated during this in step 1, can produce a large amount of useless containing vanadium
Liquid, toxicity is big, and is difficult treatment.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of M phase hypovanadic oxides, the letter of the method technique
It is single, low cost, it is adaptable to industrialized production.
To reach above-mentioned purpose, the present invention provides following technical scheme：
A kind of preparation method of M phase hypovanadic oxides, including presoma prepare and two steps of hydrothermal crystallizing, it is prepared before
Drive body directly carries out hydrothermal crystallizing without isolation, wherein, the preparation method of presoma be selected from it is following any one：
(A) soluble vanadic salts is soluble in water, after adding reducing agent, reaction to terminate, heating steams solvent, is subsequently adding
Water, ultrasonic disperse obtains forerunner's dispersion liquid；
(B) soluble vanadic salts and complexant are together added to the water, dissolving forms precursor.
Preferably, in method (A), in terms of the quality of vanadium dioxide, the mass concentration of forerunner's dispersion liquid for 0.5~
30%.
Preferably, in method (A), the soluble vanadic salts be ammonium metavanadate, reducing agent be hydrazine or L-AA, can
Dissolubility vanadic salts is 4~1 with the mol ratio of reducing agent：1.
Preferably, in method (A), soluble vanadic salts is soluble in water under the conditions of 80~100 DEG C, rapidly joins reducing agent,
Reaction 10 minutes, solvent is steamed in 100 DEG C of heating, is then added water, and ultrasonic disperse obtains forerunner's dispersion liquid.
It is further preferred that the time of ultrasonic disperse treatment is 10 minutes.
Preferably, in method (B), in terms of the quality of vanadium dioxide, the mass concentration of precursor is 0.5~30%.
Preferably, in method (B), the complexant is ethylenediamine or triethanolamine, and the soluble vanadic salts is pentavalent vanadium
Salt or tetravalence vanadic salts, pentavalent vanadic salts are selected from ammonium metavanadate, sodium metavanadate, potassium metavanadate, sodium vanadate, alum acid potassium, or five oxidations
Any one in two vanadium；Tetravalence vanadium is selected from vanadic sulfate or vanadyl oxalate；Complexant is 1 with the mol ratio of soluble vanadic salts：8
~2：1.
Preferably, the condition of hydrothermal crystallizing：Temperature is 180~400 DEG C, and process time is 6~240 hours, uses water
The compactedness of hot kettle is 50~80%.
It is further preferred that after the completion of hydrothermal crystallizing, product is obtained using centrifugation or vacuum filtration, with water and second
Alcohol respectively washing 3 times, then washed with acetone 1 time, in 40 DEG C of dryings, obtain final product.
Preferably, when presoma is prepared, dopant is added to be doped to regulate and control the phase transition temperature of gained vanadium dioxide,
Dopant is together dissolved in the water with soluble vanadic salts, and dopant addition is 0~0.1 with the mol ratio of v element.
It is further preferred that the dopant is selected from any in the soluble-salt of tungsten, magnesium, molybdenum, niobium, tantalum, zinc, aluminium or copper
Plant or two kinds.
The beneficial effects of the present invention are：
The present invention can directly obtain M phase hypovanadic oxide nano particles, because the synthetic method for using is hydro-thermal method, product
Crystallized in closed, high temperature and high pressure environment, therefore, the pure thing phase that the product of preparation has had, good crystallization, particle diameter distribution is equal
Even and good dispersiveness.The sample of preparation directly in water, can be prepared into certain density VO by ultrasonic disperse2It is molten
Glue.
Hydrothermal crystallization process of the invention does not have gas to generate, therefore, the solid content of the presoma of hydro-thermal process can be very
Height, is adapted to industrial-scale production, production cost and improve production efficiency can be directly reduced, to meet the need of practical application
Ask.
Presoma prepared by the present invention is separated not over washing, but directly solvent is evaporated or directly containing preceding
The reaction solution of drive body is transferred to reactor carries out hydrothermal crystallizing, it is possible to reduce the substantial amounts of vanadium-containing water produced in washing, while
Also the loss in vanadium source is avoided, but also whole crystallization can be made in the reaction environment of hydro-thermal stage holding forerunner's production procedure
Reaction is carried out in being maintained at appropriate alkaline environment, and this can be prepared, and particle diameter is smaller, be distributed more uniform nanometer M phase titanium dioxides
Vanadium；And nano vanadium dioxide prepared by this environment can be directly dispersing in alkaline aqueous solution, i.e., with dispersiveness high
And stability.
When using complexant when, vanadium source first with complexant formed complex compound, in hydrothermal crystallization process, complex compound it is steady
It is qualitative to be destroyed, and the complexant for using is alkalescence, if vanadium source is tetravalence vanadium, then precipitation can be formed, while crystallization forms M
Phase hypovanadic oxide；If vanadium source is pentavalent vanadium, then complexant may also operate as reduction, then reduction, precipitation and Crystallization Phases
Go on row.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carries out
Explanation：
Fig. 1 is the projection electromicroscopic photograph (TEM) of M phase hypovanadic oxides；
Fig. 2 is the X-ray diffraction analysis (XRD) of M phase hypovanadic oxides；
Fig. 3 is differential scanning calorimetric analysis (DSC) curve of M phase hypovanadic oxides.
Specific embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
Embodiment 1：
1g ammonium metavanadates are weighed, 30mL deionized waters are added, 100 DEG C of dissolvings are heated to, mass concentration is then quickly added into
For 5% hydrazine solution, (mol ratio of hydrazine and ammonium metavanadate is 1：4) 10 minutes, are incubated at 100 DEG C, are steamed in 100 DEG C of heating
Go out solvent；It is subsequently adding deionized water and is made into suspension, ultrasonic disperse 10 minutes obtains forerunner's dispersion liquid (with vanadium dioxide
Quality meter, the mass concentration of forerunner's dispersion liquid is for 5%).The dispersion liquid is transferred in the reactor of 20mL, at 260 DEG C
Hydro-thermal process 24 hours, after the completion of hydrothermal crystallizing, using being centrifugally separating to obtain product, with respectively washing 3 times of water and ethanol, then with third
Ketone is washed 1 time, in 40 DEG C of dryings, you can obtain 0.7g M phases VO2Nano-powder.The diameter of particle of acquisition is as shown in figure 1, majority
In 20nm or so, maximum is also not above 50nm to grain diameter；Fig. 2 is the X diffraction patterns of sample, and all of peak is all M phases
The diffraction maximum of vanadium dioxide, does not have other impurity, and this sample for showing to obtain is pure M phase hypovanadic oxides.The DSC results of sample
The phase transition temperature for showing heating process is 59 DEG C (Fig. 3).
Embodiment 2：
0.1g ammonium metavanadates are weighed, 5mL deionized waters are added, 100 DEG C of dissolvings are heated to, dilution quality is then quickly added into
Concentration is that (mol ratio of hydrazine and ammonium metavanadate is 1 for 5% hydrazine solution：1)；In 100 DEG C of insulations, until solvent steams completely
Go out；It is subsequently adding deionized water and is made into suspension, ultrasonic disperse 10 minutes obtains forerunner's dispersion liquid (with the matter of vanadium dioxide
Gauge, the mass concentration of forerunner's dispersion liquid is for 0.5%).The dispersion liquid is transferred in the reactor of 20mL, in 240 DEG C of water
Heat treatment 48 hours, after the completion of hydrothermal crystallizing, product is obtained using vacuum filtration, is respectively washed 3 times with water and ethanol, then use acetone
Washing 1 time, in 40 DEG C of dryings, you can obtain 0.07gM phases VO2Nano-powder.The powder can in being directly added into 10mL deionized waters
To be made into vanadium dioxide colloid, the colloid has good stability.
Embodiment 3：
2g ammonium metavanadates are weighed, 30mL deionized waters are added, 80 DEG C of dissolvings are heated to, L-AA is then quickly added into
(L-AA is 1 with the mol ratio of ammonium metavanadate：2) 10 minutes, are incubated at 80 DEG C, solvent is steamed in 100 DEG C of heating；Then
Deionized water is added to be made into suspension, ultrasonic disperse 10 minutes obtains forerunner's dispersion liquid (preceding in terms of the quality of vanadium dioxide
The mass concentration of dispersion liquid is driven for 5%).The dispersion liquid is transferred in the reactor of 20mL, in 180 DEG C of hydro-thermal process 240
Hour, after the completion of hydrothermal crystallizing, using product is centrifugally separating to obtain, respectively washed 3 times with water and ethanol, then washed with acetone 1 time,
In 40 DEG C of dryings, you can obtain 1.4gM phases VO2Nano-powder.
Embodiment 4：
4g ammonium metavanadates are weighed, 30mL deionized waters are added, 90 DEG C of dissolvings are heated to, L-AA is then quickly added into
(L-AA is 1 with the mol ratio of ammonium metavanadate：3) 10 minutes, are incubated at 90 DEG C, solvent is steamed in 100 DEG C of heating；Then
Deionized water is added to be made into suspension, ultrasonic disperse 10 minutes obtains forerunner's dispersion liquid (preceding in terms of the quality of vanadium dioxide
The mass concentration of dispersion liquid is driven for 20%).The dispersion liquid is transferred in the reactor of 20mL, it is small in 400 DEG C of hydro-thermal process 6
When, after the completion of hydrothermal crystallizing, product is obtained using vacuum filtration, respectively washed 3 times with water and ethanol, then washed with acetone 1 time, in
40 DEG C of dryings, you can obtain 2.8gM phases VO2Nano-powder.
Embodiment 5：
By ammonium metavanadate 5g and ethylenediamine, (ethylenediamine is 1 with the mol ratio of ammonium metavanadate：8) deionized water is together added
In, dissolving forms precursor, and in terms of the quality of vanadium dioxide, the mass concentration of precursor is 30%.This is disperseed
Liquid is transferred in the reactor of 20mL, in 260 DEG C of hydro-thermal process 24 hours, after the completion of hydrothermal crystallizing, using being centrifugally separating to obtain
Product, is respectively washed 3 times with water and ethanol, then is washed with acetone 1 time, in 40 DEG C of dryings, you can obtain 3.5gM phases VO2Nano powder
Body.
Embodiment 6：
By vanadic anhydride 1.56g and triethanolamine, (triethanolamine is 2 with the mol ratio of vanadic anhydride：1) together add
Enter in deionized water, dissolving forms precursor, and in terms of the quality of vanadium dioxide, the mass concentration of precursor is
30%.The dispersion liquid is transferred in the reactor of 20mL, in 180 DEG C of hydro-thermal process 24 hour 240 hours, hydrothermal crystallizing was completed
Afterwards, product is obtained using vacuum filtration, is respectively washed 3 times with water and ethanol, then washed with acetone 1 time, in 40 DEG C of dryings, you can obtain
Obtain 1.4gM phases VO2Nano-powder.
Embodiment 7：
By vanadic sulfate 2.79g and ethylenediamine, (ethylenediamine is 1 with the mol ratio of vanadic sulfate：1) deionization is together added
In water, dissolving forms precursor, and in terms of the quality of vanadium dioxide, the mass concentration of precursor is 15%.This point
Dispersion liquid is transferred in the reactor of 20mL, in 400 DEG C of hydro-thermal process 6 hours, after the completion of hydrothermal crystallizing, using being centrifugally separating to obtain
Product, is respectively washed 3 times with water and ethanol, then is washed with acetone 1 time, in 40 DEG C of dryings, you can obtain 1.4gM phases VO2Nano powder
Body.
Embodiment 8：
2g ammonium metavanadates and 88.8mg ammonium tungstates are weighed, 30mL deionized waters are added, 100 DEG C of dissolvings is heated to, then soon
Speed adds the hydrazine solution that dilution mass concentration is 5%, and (hydrazine is 1 with the mol ratio of ammonium metavanadate：1)；It is incubated at 100 DEG C, directly
Steamed completely to solvent；It is subsequently adding deionized water and is made into suspension, ultrasonic disperse 10 minutes obtains forerunner's dispersion liquid.
The dispersion liquid is transferred in the reactor of 20mL, in 240 DEG C of hydro-thermal process 48 hours, after the completion of hydrothermal crystallizing, is taken out using vacuum
Filter obtains product, is respectively washed 3 times with water and ethanol, then is washed with acetone 1 time, in 40 DEG C of dryings, you can obtain 1.4gM phases VO2
Nano-powder, the powder phase transition temperature is 25 DEG C or so.The powder can be made into titanium dioxide in being directly added into 10mL deionized waters
Vanadium colloid, the colloid has good stability.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment to be described in detail the present invention, it is to be understood by those skilled in the art that can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (10)
1. a kind of preparation method of M phase hypovanadic oxides, including presoma is prepared and two steps of hydrothermal crystallizing, it is characterised in that
Prepared presoma directly carries out hydrothermal crystallizing without isolation, wherein, the preparation method of presoma be selected from it is following any one：
(A) soluble vanadic salts is soluble in water, after adding reducing agent, reaction to terminate, heating steams solvent, is subsequently adding water, surpasses
Sound disperses, and obtains forerunner's dispersion liquid；
(B) soluble vanadic salts and complexant are together added to the water, dissolving forms precursor.
2. the preparation method of a kind of M phase hypovanadic oxides according to claim 1, it is characterised in that in method (A), with two
The quality meter of vanadium oxide, the mass concentration of forerunner's dispersion liquid is 0.5~30%.
3. the preparation method of a kind of M phase hypovanadic oxides according to claim 1, it is characterised in that described in method (A)
Soluble vanadic salts is ammonium metavanadate, and reducing agent is hydrazine or L-AA, the mol ratio of soluble vanadic salts and reducing agent for 4~
1：1.
4. the preparation method of a kind of M phase hypovanadic oxides according to claim 1, it is characterised in that solvable in method (A)
Property vanadic salts it is soluble in water under the conditions of 80~100 DEG C, rapidly join reducing agent, react 10 minutes, steamed in 100 DEG C of heating molten
Agent, then adds water, ultrasonic disperse, obtains forerunner's dispersion liquid.
5. the preparation method of a kind of M phase hypovanadic oxides according to claim 1, it is characterised in that in method (B), with two
The quality meter of vanadium oxide, the mass concentration of precursor is 0.5~30%.
6. the preparation method of a kind of M phase hypovanadic oxides according to claim 1, it is characterised in that described in method (B)
Complexant is ethylenediamine or triethanolamine, and the soluble vanadic salts is pentavalent vanadic salts or tetravalence vanadic salts, and pentavalent vanadic salts is selected from inclined vanadium
Sour ammonium, sodium metavanadate, potassium metavanadate, sodium vanadate, alum acid potassium, or any one in vanadic anhydride；Tetravalence vanadium is selected from sulfuric acid
Vanadyl or vanadyl oxalate；Complexant is 1 with the mol ratio of soluble vanadic salts：8~2：1.
7. a kind of preparation method of M phase hypovanadic oxides according to claim 1, it is characterised in that the condition of hydrothermal crystallizing：
Temperature is 180~400 DEG C, and process time is 6~240 hours, and the compactedness for using water heating kettle is 50~80%.
8. the preparation method of a kind of M phase hypovanadic oxides according to claim 1, it is characterised in that after the completion of hydrothermal crystallizing,
Product is obtained using centrifugation or vacuum filtration, is respectively washed 3 times with water and ethanol, then washed with acetone 1 time, it is dry in 40 DEG C
It is dry, obtain final product.
9. the preparation method of a kind of M phase hypovanadic oxides according to claim 1, it is characterised in that when presoma is prepared,
Dopant is added to be doped to regulate and control the phase transition temperature of gained vanadium dioxide, dopant is together dissolved in water with soluble vanadic salts
In, dopant addition is 0~0.1 with the mol ratio of v element.
10. the preparation method of a kind of M phase hypovanadic oxides according to claim 9, it is characterised in that the dopant is selected from
Any one or two kinds of in the soluble-salt of tungsten, magnesium, molybdenum, niobium, tantalum, zinc, aluminium or copper.
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| CN107840368A (en) * | 2017-11-21 | 2018-03-27 | 陕西科技大学 | A kind of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder and preparation method thereof |
| US20210002490A1 (en) * | 2018-03-21 | 2021-01-07 | King Abdullah University Of Science And Technology | Vanadium oxide nanoparticle-based ink compositions |
| CN108892171A (en) * | 2018-07-11 | 2018-11-27 | 首都师范大学 | A kind of thermodynamics restoring method synthesizing vanadium oxide nano material |
| CN109336175A (en) * | 2018-11-02 | 2019-02-15 | 湘西土家族苗族自治州产商品质量监督检验所 | A kind of method of the auxiliary thermal reduction preparation M-phase vanadium dioxide powder of microwave |
| CN109502643A (en) * | 2018-11-26 | 2019-03-22 | 深圳大学 | A kind of boron magnesium codope VO2Powder and its preparation method and application |
| CN109502643B (en) * | 2018-11-26 | 2021-03-16 | 深圳大学 | Boron-magnesium co-doped VO2Powder and preparation method and application thereof |
| CN110203972A (en) * | 2019-06-13 | 2019-09-06 | 湖北大学 | The preparation method of phase-M vanadium dioxide nanometre powder |
| CN110272070A (en) * | 2019-07-12 | 2019-09-24 | 西南大学 | A method of optimization nanometer M phase hypovanadic oxide stability |
| CN110272070B (en) * | 2019-07-12 | 2022-02-22 | 西南大学 | Method for optimizing stability of nano M-phase vanadium dioxide |
| CN112174206A (en) * | 2020-10-16 | 2021-01-05 | 成都先进金属材料产业技术研究院有限公司 | Method for directly preparing vanadium dioxide by taking vanadyl acetylacetonate as vanadium source |
| CN112209438A (en) * | 2020-10-16 | 2021-01-12 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing nano vanadium dioxide from ethylene glycol vanadyl |
| CN112125338A (en) * | 2020-10-16 | 2020-12-25 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing M-phase vanadium dioxide by solvothermal method |
| CN112125337A (en) * | 2020-10-16 | 2020-12-25 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing nano vanadium dioxide by using pentavalent vanadium alkoxide as raw material |
| CN112919820A (en) * | 2021-01-21 | 2021-06-08 | 大连工业大学 | Zn-doped VO2Powder and method for preparing composite film by using same |
| CN112919820B (en) * | 2021-01-21 | 2022-05-27 | 大连工业大学 | Zn-doped VO2Powder and method for preparing composite film by using same |
| CN113636597A (en) * | 2021-07-29 | 2021-11-12 | 武汉理工大学 | Preparation method of tantalum-doped vanadium dioxide film |
| CN115159860A (en) * | 2022-07-20 | 2022-10-11 | 贵州民族大学 | Preparation of H-SiO in mild aqueous environment 2 -VO 2 (M) method of coating |
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