CN110342574A - A kind of preparation method of monoclinic phase vanadium dioxide nano-powder - Google Patents
A kind of preparation method of monoclinic phase vanadium dioxide nano-powder Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of monoclinic phase vanadium dioxide nano-powder, belongs to ball-milling method preparation VO2Powder field.The following steps are included: (1) prepares hypovanadic oxide powder using hydro-thermal method；(2) hypovanadic oxide powder prepared by step (1) and grinding aid are mixed；(3) step (2) are mixed gained ingredient to be added in grinding device, mill ball is added, is ground；(4) by the cleaning of abrasive material obtained by step (3), drying to get monoclinic phase vanadium dioxide.Ball-milling method provided by the present invention prepares monoclinic phase VO2, by promoting VO by mechanical force2Phase transition occurs for miscellaneous phase, and reduces material particular diameter constantly due to abrasive action during continuous ball milling.Preparation method of the invention is without heating, energy saving；Phase transition can occur in short period, the time is short, high production efficiency.
Description
Technical field
The invention belongs to ball-milling methods to prepare VO2Powder field, and in particular to arrive a kind of monoclinic phase vanadium dioxide nano-powder
Preparation method.
Background technique
In recent years, in order to reduce modern building room conditioning energy consumption, " smart window " is had received widespread attention.Smart window energy
Enough by stimuli responsives such as light, heat, electricity come the transmitance of intelligent control light and heat, therefore photochromic smart window, heat can be divided into
Mutagens color smart window, electrochromic intelligent window.
Monoclinic phase vanadium dioxide VO2(M) there is excellent thermochromism energy, be metal when environment temperature is higher than phase transition temperature
State reflects near infrared light；It is insulation state lower than phase transition temperature, light is allowed to pass freely through.Since monoclinic phase vanadium dioxide is this
To the ability of environment temperature response regulation sunlight, so, current monoclinic phase vanadium dioxide is optimal thermochromism intelligence
One of window materials.
Vanadium (V) is used as a kind of transition metal element, has active chemical property, V element is according to locating chemical environment table
Reveal+2~+5 valences and its various mixed valences.And VO2In V element be+4 valences, therefore be easy to send out in its preparation process
Raw oxidation obtains the VO of+4/+5 mixed valence2/V2O5Mix products.In addition, VO2There is also a variety of isomrs, such as
VO2(A)、VO2(B)、VO2(D)、VO2(P)、VO2(M) etc..So to prepare pure phase VO2(M), it needs accurately to control preparation process
In process conditions.
Currently, the method for preparing monoclinic phase vanadium dioxide is mainly hydro-thermal method, the particle purity height of preparation, crystallinity
Good, dispersibility is greatly.But its technological parameter is excessive, prepares product often with other miscellaneous phases and appearance of reuniting, is not easy to directly obtain and receive
Meter level VO2(M) powder.VO is made by phase transition at present2Miscellaneous phase is changed into monoclinic phase vanadium dioxide VO2(M), mainly in vacuum or
It is achieved under inert atmosphere by high annealing, but to need to be heated at high temperature energy consumption larger for this method, undoubtedly aggravates production cost,
Product is easy to reunite after another aspect high annealing, also can therefore influence properties of product, such as: article
(Inorg.Chem.Front., 2016,3,1035-1042 | 1039) mention 550 DEG C of high annealing hydro-thermal systems under vacuum conditions
Standby VO2(D) powder 3h obtains particle size in 500nm or more, and reunite more serious VO2(M) powder.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of monoclinic phase vanadium dioxide nano-powder, overcome existing hydro-thermal
Method and high-temperature phase-transitional prepare VO2(M) the shortcomings that powder technology and deficiency.
To achieve the goals above or other purposes, the present invention is achieved by the following technical solutions.
A kind of preparation method of monoclinic phase vanadium dioxide nano-powder, comprising the following steps:
(1) hypovanadic oxide powder is prepared using hydro-thermal method；
(2) hypovanadic oxide powder prepared by step (1) and grinding aid are mixed；
(3) step (2) are mixed gained ingredient to be added in grinding device, mill ball is added, is ground；
(4) by the cleaning of abrasive material obtained by step (3), drying to get monoclinic phase vanadium dioxide.
Further, the hypovanadic oxide powder in step (1) is non-monoclinic phase vanadium dioxide.Preferably, titanium dioxide vanadium powder
Body is selected from VO2(A)、VO2(B)、VO2(D)、VO2One of (P) or it is a variety of.
Wherein, hydro-thermal method is conventional method in the art.
Further, the mass ratio of hypovanadic oxide powder and grinding aid is 1:(0~10).
Further, the mass ratio of ingredient and mill ball is 1:(1~50 in step (3)).
Further, the grinding aid is selected from methanol, isoamyl alcohol, glycerol, acetone, aromatic radical sulfonic acid, lauryl amine, 13
Amine, tetradecy lamine, organosilicon, oleic acid, butyric acid, odium stearate, enuatrol, capric acid, lanolin, aphthenic acids, sodium naphthenate, naphthenic base
Sodium sulfonate, n-hexane, pentyl acetate, sodium metasilicate, sodium hydroxide, sodium chloride, sodium carbonate, lithium hydroxide, lithium chloride, lithium carbonate,
Potassium hydroxide, potassium chloride, potassium carbonate, sodium hexametaphosphate, sodium tripolyphosphate, triethanolamine, polycarboxylate, sodium pyrophosphate, lemon
Lemon acid sodium it is one or more.
Further, mill ball be selected from alumina ceramic grinding ball, zirconium oxide abrasive ball, agate mill ball, stainless-steel grinding ball,
One of polyurethane mill ball, hard alloy mill ball.Preferably, mill ball is selected from alumina ceramic grinding ball, zirconium oxide abrasive
Ball, agate mill ball.
Further, revolving speed is 10-1800r/min in step (3), grinds 5min-24h.
Further, the ball-milling device can be the common ball-milling device in ball milling field.The ball-milling device can be selected from
Ball grinder.
Further, eccentric cleaning, centrifugal speed 50-1800r/ are carried out using centrifuge to abrasive material in step (4)
min.It is dried after cleaning, drying temperature is 30-100 DEG C, time 1-5h.
Ball-milling method provided by the present invention prepares monoclinic phase VO2, by promoting VO by mechanical force2Phase transition occurs for miscellaneous phase,
And reduce material particular diameter constantly due to abrasive action during continuous ball milling.Preparation method of the invention is not necessarily to heating,
Energy saving；Phase transition can occur in short period, the time is short, high production efficiency.
Detailed description of the invention
Fig. 1 is 1 gained hydrothermal synthesis VO of embodiment2(A) X-ray diffraction (XRD) and VO of sample and final products2(A)、
VO2(M) standard card comparison diagram；
Fig. 2 is 2 gained hydrothermal synthesis VO of embodiment2(D) X-ray diffraction (XRD) and VO of sample and final products2(B)、
VO2(M) standard card comparison diagram；
Fig. 3 is 3 gained hydrothermal synthesis VO of embodiment2(D) X-ray diffraction (XRD) and VO of sample and final products2(D)、
VO2(M) standard card comparison diagram；
Fig. 4 is the scanning electron microscope diagram (SEM) of sample and final products obtained by hydro-thermal method in embodiment 1, wherein left
Edge graph is the VO that hydro-thermal method obtains2(A) SEM figure, the right figure is VO after ball-milling treatment2(M) SEM figure；
Fig. 5 is the scanning electron microscope diagram (SEM) of sample and final products obtained by hydro-thermal method in embodiment 2, wherein left
Edge graph is the VO that hydro-thermal method obtains2(B) SEM figure, the right figure is VO after ball-milling treatment2(M) SEM figure；
Fig. 6 is 1 gained hydrothermal synthesis VO of comparative example2(D) X-ray diffraction (XRD) and VO of sample2(D) standard card
Comparison diagram；
Fig. 7 is VO in comparative example 12(D) X-ray diffraction (XRD) and VO of the annealed gained powder of powder2(M) standard
Card comparison diagram；
Fig. 8 is the scanning electron microscope diagram (SEM) of sample and final products obtained by hydro-thermal method in comparative example 1, wherein left
Edge graph is the VO that hydro-thermal method obtains2(D) SEM figure, the right figure are annealing gained VO2(M) SEM figure；
Fig. 9 is the differential scanning calorimetry figure (DSC) of 2 products obtained therefrom of embodiment.
Specific embodiment
Illustrate embodiments of the present invention below by way of particular specific embodiment, those skilled in the art can be by this explanation
Other advantages and efficacy of the present invention can be easily understood for content disclosed by book.The present invention can also be by addition different specific
Embodiment is embodied or practiced, and the various details in this specification can also not carried on the back based on different viewpoints and application
From carrying out various modifications or alterations under spirit of the invention.
It should be noted that in the absence of conflict, the feature in following embodiment and embodiment can be combined with each other.Also
It should be appreciated that term used in the embodiment of the present invention is in order to describe specific specific embodiment, rather than in order to limit
Protection scope of the present invention.The test method of actual conditions is not specified in the following example, usually according to normal condition, or presses
According to condition proposed by each manufacturer.
When embodiment provides numberical range, it should be appreciated that except non-present invention is otherwise noted, two ends of each numberical range
Any one numerical value can be selected between point and two endpoints.Unless otherwise defined, the present invention used in all technologies and
The grasp and record of the invention of scientific term and those skilled in the art to the prior art, can also use and this hair
Any method, equipment and the material of the similar or equivalent prior art of bright method as described in the examples, equipment, material is realized
The present invention.
Instrument model used by X-ray diffraction (XRD) is tested in the embodiment of the present invention: D8FOCUS.
Embodiment 1
A kind of preparation method of monoclinic phase vanadium dioxide nano-powder, including the following steps:
(1) prepared by hydro-thermal:
By V2O5(1.001g) is added in 20mL deionized water, adds the 1.5ml concentrated sulfuric acid, 60-70 DEG C of magnetic stirring apparatus stirs
10min is mixed, 0.520g N is added2H4·HO2Adjusting pH using sodium hydroxide is 3-4, and it is stainless to be transferred to polytetrafluoroethyllining lining
In steel autoclave.Autoclave sealing, reacts for 24 hours, then, autoclave is cooled slowly room temperature, is produced under the conditions of 230 DEG C
Object, twice with deionized water centrifuge washing, ethanol washing is primary, removes residue, and 80 DEG C of dry 10h obtain powder, carries out X-
X ray diffraction (XRD) test, and and VO2(A) standard card compares, as shown in Figure 1, gained powder is VO2(A) powder.
(2) ball-milling treatment:
1) by step (1) the 3.000g VO that repeatedly hydro-thermal obtains2(A) powder is mixed with oleic acid 2.324g.
2) mix is added in ball grinder, mill ball 50g, revolving speed 1000r/min is added, grind 4h.
3) grinding material being transferred to 50ml beaker, 30ml ethyl alcohol is added, magnetic agitation 5min is transferred in centrifuge,
Revolving speed 3000r/min, is centrifuged 10min, and ethyl alcohol cleans three times.
4) above-mentioned washing material is placed in 60 DEG C of baking 10h in constant temperature oven, removes dehydrated alcohol, by mortar grinder,
Obtain final powder, by the powder carry out X-ray diffraction (XRD) test, as a result as shown in Figure 1, it can be seen from the figure that through
It crosses preparation method processing acquisition other phase diffraction maximums of powder of the present invention to disappear, contains only VO2(M) thus diffraction maximum illustrates institute
The powder of acquisition is VO2(M) powder.
Embodiment 2
A kind of preparation method of monoclinic phase vanadium dioxide nano-powder, including the following steps:
(1) prepared by hydro-thermal:
By V2O50.600g, oxalic acid 0.790g are added in 40mL deionized water.With magnetic stirrer 1h, blue is obtained
Transparency liquid is transferred in polytetrafluoroethyllining lining stainless steel autoclave.Autoclave sealing, reacts for 24 hours under the conditions of 210 DEG C,
Then, autoclave is cooled slowly room temperature.Product is obtained, three times with dehydrated alcohol centrifuge washing, removes residue, 55 DEG C true
The dry 12h of sky, obtains powder, carries out X-ray diffraction (XRD) test, and and VO2(B) standard card compares, as shown in Fig. 2, institute
Obtaining powder is VO2(B) powder.
(2) ball-milling treatment:
1) by step (1) the 1.123g VO that repeatedly hydro-thermal obtains2(B) powder is mixed with pentyl acetate 1.234g.
2) mix is added in ball grinder, mill ball 45g, revolving speed 200r/min is added, grind 2h.
3) grinding material being transferred to 50ml beaker, 30ml ethyl alcohol is added, magnetic agitation 5min is transferred in centrifuge,
Revolving speed 3000r/min, is centrifuged 10min, and ethyl alcohol cleans three times.
4) above-mentioned washing material is placed in 60 DEG C of baking 10h in constant temperature oven, removes dehydrated alcohol, by mortar grinder,
Obtain final powder, by the powder carry out X-ray diffraction (XRD) test, as a result as shown in Fig. 2, it can be seen from the figure that through
It crosses preparation method processing acquisition other phase diffraction maximums of powder of the present invention to disappear, contains only VO2(M) thus diffraction maximum illustrates institute
The powder of acquisition is VO2(M) powder.
Embodiment 3
A kind of preparation method of monoclinic phase vanadium dioxide nano-powder, including the following steps:
(1) prepared by hydro-thermal:
By V2O5(0.8014g) is added in 20mL deionized water, and 60-70 DEG C of magnetic stirrer 10min is added
0.5200gN2H4·HO2Adjusting pH using sodium hydroxide is 7-8, is transferred in polytetrafluoroethyllining lining stainless steel autoclave.It is high
Kettle sealing is pressed, is reacted for 24 hours under the conditions of 260 DEG C, then, autoclave is cooled slowly room temperature.Product is obtained, deionized water is used
Twice, ethanol washing is primary for centrifuge washing, removes residue, and 80 DEG C of dry 10h obtain powder, carries out X-ray diffraction (XRD)
Test, and and VO2(D) standard card compares, as shown in figure 3, gained powder is VO2(D) powder.
(2) ball-milling treatment:
1) by step (1) the 2.023g VO that repeatedly hydro-thermal obtains2(D) powder is mixed with butyric acid 2.345g.
2) mix is added in ball grinder, mill ball 60g, revolving speed 1700r/min is added, grind 1h.
3) grinding material being transferred to 50ml beaker, 30ml ethyl alcohol is added, magnetic agitation 5min is transferred in centrifuge,
Revolving speed 3000r/min, is centrifuged 10min, and ethyl alcohol cleans three times.
4) above-mentioned washing material is placed in 60 DEG C of baking 10h in constant temperature oven, removes dehydrated alcohol, by mortar grinder,
Obtain final powder, by the powder carry out X-ray diffraction (XRD) test, as a result as shown in figure 3, it can be seen from the figure that through
It crosses preparation method processing acquisition other phase diffraction maximums of powder of the present invention to disappear, contains only VO2(M) thus diffraction maximum illustrates institute
The powder of acquisition is VO2(M) powder.
Embodiment 4
A kind of preparation method of monoclinic phase vanadium dioxide nano-powder, including the following steps:
(1) prepared by hydro-thermal:
By V2O50.502g, oxalic acid 0.691g are added in 45mL deionized water.With magnetic stirrer 2h, blue is obtained
Transparency liquid is transferred in polytetrafluoroethyllining lining stainless steel autoclave.Autoclave sealing, reacts 12h under the conditions of 200 DEG C,
Then, autoclave is cooled slowly room temperature.Product is obtained, three times with dehydrated alcohol centrifuge washing, removes residue, 55 DEG C true
The dry 12h of sky, tests through X-ray diffraction (XRD), obtains VO2(D)VO2(B) mixed phase powder.
(2) ball-milling treatment:
1) by step (1) VO that repeatedly hydro-thermal obtains2(D) and VO2(B) mixed phase powder 2.023g, with acetone 3.265g
Mixing.
2) mix is added in ball grinder, mill ball 75g, revolving speed 1200r/min is added, grind 30min.
3) grinding material being transferred to 50ml beaker, 30ml ethyl alcohol is added, magnetic agitation 5min is transferred in centrifuge,
Revolving speed 3000r/min, is centrifuged 10min, and ethyl alcohol cleans three times.
4) above-mentioned washing material is placed in 60 DEG C of baking 10h in constant temperature oven, removes dehydrated alcohol, by mortar grinder,
Obtain VO2(M) powder.
Embodiment 5
A kind of preparation method of monoclinic phase vanadium dioxide nano-powder, including the following steps:
(1) prepared by hydro-thermal:
By V2O50.612g, oxalic acid 0.621g are added in 40mL deionized water.With magnetic stirrer 2h, blue is obtained
Transparency liquid is transferred in polytetrafluoroethyllining lining stainless steel autoclave.Autoclave sealing, reacts 18h under the conditions of 200 DEG C,
Then, autoclave is cooled slowly room temperature.Product is obtained, three times with dehydrated alcohol centrifuge washing, removes residue, 55 DEG C true
The dry 12h of sky, tests through X-ray diffraction (XRD), obtains VO2(D) and VO2(A) mixed phase powder.
(2) ball-milling treatment:
1) by step (1) the 3.356g VO that repeatedly hydro-thermal obtains2(D) and VO2(A) mixed phase powder, with glycerol
3.214g mixing.
2) mix is added in ball grinder, mill ball 80g, revolving speed 500r/min is added, grind 5h.
3) grinding material being transferred to 50ml beaker, 30ml ethyl alcohol is added, magnetic agitation 5min is transferred in centrifuge,
Revolving speed 3000r/min, is centrifuged 10min, and ethyl alcohol cleans three times.
4) above-mentioned washing material is placed in 60 DEG C of baking 10h in constant temperature oven, removes dehydrated alcohol, by mortar grinder,
Obtain VO2(M) powder.
Embodiment 6
A kind of preparation method of monoclinic phase vanadium dioxide nano-powder, including the following steps:
(1) prepared by hydro-thermal:
By V2O50.712g, oxalic acid 0.522g are added in 40mL deionized water.With magnetic stirrer 2h, blue is obtained
Transparency liquid is transferred in polytetrafluoroethyllining lining stainless steel autoclave.Autoclave sealing, reacts for 24 hours under the conditions of 240 DEG C,
Then, autoclave is cooled slowly room temperature.Product is obtained, three times with dehydrated alcohol centrifuge washing, removes residue, 55 DEG C true
The dry 12h of sky, tests through X-ray diffraction (XRD), obtains VO2(D) and VO2(M) mixed phase powder.
(2) ball-milling treatment:
1) by step (1) the 1.568g VO that repeatedly hydro-thermal obtains2(D) and VO2(M) mixed phase powder, with n-hexane
5.236g
Mixing.
2) mix is added in ball grinder, mill ball 100g, revolving speed 100r/min is added, grind 6h.
3) grinding material being transferred to 50ml beaker, 30ml ethyl alcohol is added, magnetic agitation 5min is transferred in centrifuge,
Revolving speed 3000r/min, is centrifuged 10min, and ethyl alcohol cleans three times.
4) above-mentioned washing material is placed in 60 DEG C of baking 10h in constant temperature oven, removes dehydrated alcohol, by mortar grinder,
Obtain VO2(M) powder.
Comparative example 1
30mmol ammonium metavanadate and 40mmol oxalic acid are added in 16ml deionized water, is mixed 5 minutes and obtains
17ml presoma.Then precursor solution is transferred in 25ml polytetrafluoroethyllining lining stainless steel autoclave, is heated to 220
DEG C, 18h is kept the temperature, autoclave is cooled to room temperature, and by being centrifugally separating to obtain product, product is transferred to 50ml beaker, is added
30ml ethyl alcohol, magnetic agitation 5min, is transferred in centrifuge, revolving speed 3000r/min, is centrifuged 10min, and ethyl alcohol is cleaned three times, obtained
The product arrived is tested through X-ray diffraction (XRD), as a result as shown in fig. 6, being VO2(D) powder, then under vacuum conditions 550
DEG C high annealing 3h, products therefrom are tested through X-ray diffraction (XRD), as shown in fig. 7, display gained powder is VO2(M) powder
Body.
Performance characterization
1, the curve graph for obtaining 2 products obtained therefrom of embodiment using differential scanning calorimeter is as shown in figure 9, it can be obtained from the figure that institute
The product phase transition temperature of acquisition is obvious, heats phase transition temperature and VO2(M) it approaches for 68 DEG C of standard phase change temperature.
2, sem analysis is carried out to the product of embodiment 1,2 and comparative example 1 respectively, as a result respectively such as Fig. 4, Fig. 5, Fig. 8 institute
Show, comparison diagram 4, Fig. 5 can have found, the product pattern of embodiment 1,2 is band-like from original hydro-thermal institute after ball-milling treatment from pattern
Nano particle is changed into the subcircular particle of diameter 50nm-100nm, illustrates that not only available target produces after ball-milling treatment
Product, while also can change sample topography, reducing partial size.Comparison diagram 4, Fig. 5 and Fig. 8, it is possible to find produced with obtained by 1 high temperature of comparative example
Product partial size (500nm) is compared, and the product cut size (50nm-100nm) through ball-milling treatment is smaller, while particle dispersion is also mentioned
It rises.
In summary, preparation method of the invention can promote VO2Phase transition occurs for miscellaneous phase, obtains pure monoclinic phase VO2,
And reduce material particular diameter constantly due to abrasive action during continuous ball milling.Preparation method of the invention is not necessarily to heating,
Energy saving；Phase transition can occur in short period, the time is short, high production efficiency.
Above-described embodiment is merely exemplary to illustrate the principle of the present invention and its effect, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (7)
1. a kind of preparation method of monoclinic phase vanadium dioxide nano-powder, which comprises the steps of:
(1) hypovanadic oxide powder is prepared using hydro-thermal method；
(2) hypovanadic oxide powder prepared by step (1) and grinding aid are mixed；
(3) step (2) are mixed gained ingredient to be added in grinding device, mill ball is added, is ground；
(4) by the cleaning of abrasive material obtained by step (3), drying to get monoclinic phase vanadium dioxide.
2. preparation method as described in claim 1, which is characterized in that the hypovanadic oxide powder in step (1) is non-monoclinic phase
Vanadium dioxide.
3. preparation method as claimed in claim 2, which is characterized in that hypovanadic oxide powder is selected from VO in step (1)2(A)、VO2
(B)、VO2(D)、VO2One of (P) or it is a variety of.
4. preparation method as described in claim 1, which is characterized in that the mass ratio of hypovanadic oxide powder and grinding aid is 1:
(0~10).
5. preparation method as described in claim 1, which is characterized in that the mass ratio of ingredient and mill ball is 1 in step (3):
(1~50).
6. preparation method as described in claim 1, which is characterized in that the grinding aid be selected from methanol, isoamyl alcohol, glycerol,
Acetone, aromatic radical sulfonic acid, lauryl amine, tridecyl amine, tetradecy lamine, organosilicon, oleic acid, butyric acid, odium stearate, enuatrol, capric acid, sheep
Hair rouge, aphthenic acids, sodium naphthenate, cycloalkylsulfonic acid sodium, n-hexane, pentyl acetate, sodium metasilicate, sodium hydroxide, sodium chloride, carbonic acid
Sodium, lithium hydroxide, lithium chloride, lithium carbonate, potassium hydroxide, potassium chloride, potassium carbonate, sodium hexametaphosphate, sodium tripolyphosphate, three second
Hydramine, polycarboxylate, sodium pyrophosphate, sodium citrate it is one or more.
7. preparation method as described in claim 1, which is characterized in that revolving speed is 10-1800r/min in step (3), when grinding
Between 5min-24h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110734088A (en) * | 2019-10-24 | 2020-01-31 | 成都先进金属材料产业技术研究院有限公司 | M-phase VO prepared by using invalid vanadium battery negative electrolyte2Method (2) |
| CN111186860A (en) * | 2020-01-06 | 2020-05-22 | 济南大学 | Preparation method for preparing monoclinic-phase vanadium dioxide nano powder from precursor obtained by thermal decomposition and ball milling |
| 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 |
| 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 |
| CN112209442A (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 M-phase vanadium dioxide nano powder by salt-assisted ultrasonic pyrolysis method |
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| 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 |
| 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 |
| CN112209442A (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 M-phase vanadium dioxide nano powder by salt-assisted ultrasonic pyrolysis method |
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