CN108975401A - One step hydro-thermal prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology - Google Patents
One step hydro-thermal prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology Download PDFInfo
- Publication number
- CN108975401A CN108975401A CN201811230839.9A CN201811230839A CN108975401A CN 108975401 A CN108975401 A CN 108975401A CN 201811230839 A CN201811230839 A CN 201811230839A CN 108975401 A CN108975401 A CN 108975401A
- Authority
- CN
- China
- Prior art keywords
- constant temperature
- phase transition
- hydro
- phase
- transition temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses an a kind of step hydro-thermals to prepare the adjustable pure phase VO of phase transition temperature2Raw powder's production technology mixes oxalic acid and deionized water 1:39 in mass ratio, carries out magnetic agitation under constant temperature water bath, then vanadium source is added, continue after carrying out magnetic agitation under constant temperature water bath, adjusting bath temperature is 80~100 DEG C, and constant temperature stirs 0.5~2h and obtains presoma；The presoma of preparation is put into reaction kettle, obtains product in 280 DEG C of hydro-thermal reaction 72h；Product is centrifugated, the mixed liquor of the dehydrated alcohol and deionized water that are 1:2~1:5 with volume ratio cleans, and obtains target product after being dried in vacuo 6h at 50 DEG C.Preparation method of the invention is with short production cycle, simple process, reaction condition are mild, green non-pollution, low in cost, is suitble to large-scale production, the powder prepared can prepare the adjustable VO of large area phase transition temperature in conjunction with powder film-forming process2Film, be conducive to breakthrough vanadium dioxide Energy Saving Windows applies bottleneck.
Description
Technical field
The present invention relates to photothermal technique fields, can specifically, the present invention relates to a kind of step hydro-thermal preparation phase transition temperatures
The pure phase VO of tune2Raw powder's production technology.
Background technique
Vanadium dioxide is a kind of transition metal oxide, and metal-semiconductor structural phase transition nearby occurs at 68 DEG C, is lower than
At 68 DEG C, crystal is monocline, and infrared transmittivity is high, and resistivity is high；And when being higher than 68 DEG C, vanadium dioxide crystal is four directions
Structure, infrared transmittivity is low, and resistivity is low.Therefore along with vanadium dioxide before phase change after crystal structure variation, optics and
Very big change, and its phase transition performance and VO can also occur for electric property2Crystalline phase state purity it is closely coupled.Using it not
The synthermal lower change to infrared light transmittance and resistivity, vanadium dioxide is in thermochromism Energy Saving Windows and temperature sensor material
Etc. have broad application prospects.
However so far, it has been reported more than the different crystalline phase states of 20 kinds of oxyvanadium compounds and more than 10 kinds of vanadium dioxide
Road.The only VO of monocline and tetragonal phase2It is undergone phase transition at 68 DEG C or so.It is applied to building energy conservation smart window, needs dioxy
Change the phase transition temperature that vanadium has excellent phase transition performance and near room temperature, so, prepare the adjustable pure phase VO of phase transition temperature2Powder
It has become a hot topic of research always and difficult point.The study found that passing through the adjustable titanium dioxides such as doping, nanometer size effect, stress
Vanadium phase transition temperature.However it can change the phase transition temperature of vanadium dioxide by regulation stress and nanometer size effect, but adjust width
Spend limited, and phase transition performance will receive loss, and cannot realize and continuously adjust, and process repeatability is poor, is not used to reality
Production.
Summary of the invention
In view of this, in order to overcome above-mentioned problems of the prior art, the present invention provides it is a kind of it is with short production cycle,
Simple process, a step hydro-thermal of green non-pollution prepare the adjustable pure phase VO of phase transition temperature2The method of powder.
In order to achieve the above-mentioned object of the invention, this invention takes following technical schemes:
The embodiment of the present invention provides a kind of step hydro-thermal preparation adjustable pure phase VO of phase transition temperature2Raw powder's production technology,
The following steps are included:
Step a, oxalic acid and deionized water 1:39 in mass ratio are mixed, carry out magnetic agitation under constant temperature water bath, then plus
Enter vanadium source, continue after carrying out magnetic agitation under constant temperature water bath, adjusting bath temperature is 80~100 DEG C, and constant temperature stirs 0.5~2h and obtains
Obtain presoma；
Step b, the step a presoma prepared is put into reaction kettle, obtains product in 280 DEG C of hydro-thermal reaction 72h；
Step c, the product of step b is centrifugated, with volume ratio be 1:2~1:5 dehydrated alcohol and deionized water
Mixed liquor cleaning, obtains target product after being dried in vacuo 6h at 50 DEG C.
In above scheme, in the step a, the vanadium source is vanadic anhydride, ammonium metavanadate or vanadic sulfate；The vanadium
The molar concentration rate of source and oxalic acid is 1:2.
In above scheme, the step a are as follows: step a, mix oxalic acid and deionized water 1:39 in mass ratio, water-bath is permanent
Temperature is lower to carry out magnetic agitation, and vanadium source and tungsten source is then added, continues after carrying out magnetic agitation under constant temperature water bath, adjusts bath temperature
It is 80~100 DEG C, constant temperature stirs 0.5~2h and obtains presoma；
In above scheme, in the step a, the vanadium source is vanadic anhydride, ammonium metavanadate or vanadic sulfate；The vanadium
The molar concentration rate of source and oxalic acid is 1:2；The tungsten source is wolframic acid, ammonium tungstate or sodium tungstate, and the additional amount in the tungsten source is tungsten
Foreign atom percentage be 0.5~1at%.
In above scheme, it is the anhydrous of 1:2~1:5 with volume ratio that the step c, which is to be centrifugated the product of step b,
Ethyl alcohol and the cleaning of the mixed liquor of deionized water are annealed after being dried in vacuo 6h at 50 DEG C using high-purity argon gas, are obtained target and are produced
Object.
In above scheme, in the step c, the processing parameter of the high-purity argon gas annealing are as follows: high-purity argon gas 0.5L/min,
30 DEG C of 94min to 500 DEG C of heatings, constant temperature 1h.
Compared with prior art, preparation method of the invention is with short production cycle, simple process, reaction condition are mild, green
It is pollution-free, low in cost, it is suitble to large-scale production, the powder prepared can prepare big face in conjunction with powder film-forming process
The product adjustable VO of phase transition temperature2Film, be conducive to breakthrough vanadium dioxide Energy Saving Windows applies bottleneck.
Detailed description of the invention
Fig. 1 is the VO that 1-4 of the embodiment of the present invention is obtained2X-ray diffraction (XRD) map of powder；Wherein red and black
Continuous columnar alignment is respectively monoclinic phase VO2(M) standard JCPDS No.65-2358 card and tetragonal phase VO2(R) standard
JCPDS No.76-0677 card；
Fig. 2 is the VO that 1-4 of the embodiment of the present invention is obtained2Scanning electron microscope (SEM) map of powder；
Fig. 3 is the VO that 2-4 of the embodiment of the present invention is obtained2Differential scanning calorimetric analysis (DSC) map of powder；
Fig. 4 is VO prepared by sample that 2-4 of the embodiment of the present invention is obtained2The ultraviolet-visible-near-infrared spectrum of film.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
The embodiment of the present invention provides a kind of step hydro-thermal preparation adjustable pure phase VO of phase transition temperature2Raw powder's production technology,
The following steps are included:
Step a, oxalic acid and deionized water 1:39 in mass ratio are mixed, carry out magnetic agitation under constant temperature water bath, then plus
Enter vanadium source, continue after carrying out magnetic agitation under constant temperature water bath, adjusting bath temperature is 80~100 DEG C, and constant temperature stirs 0.5~2h and obtains
Obtain presoma；
Step b, the step a presoma prepared is put into reaction kettle, obtains product in 280 DEG C of hydro-thermal reaction 72h；
Step c, the product of step b is centrifugated, with volume ratio be 1:2~1:5 dehydrated alcohol and deionized water
Mixed liquor cleaning, obtains target product after being dried in vacuo 6h at 50 DEG C.
In the step a, the vanadium source is vanadic anhydride, ammonium metavanadate or vanadic sulfate；The vanadium source and oxalic acid
Molar concentration rate is 1:2.
Further, the step a are as follows: step a, mix oxalic acid and deionized water 1:39 in mass ratio, constant temperature water bath
Then vanadium source and tungsten source is added in lower carry out magnetic agitation, continue after carrying out magnetic agitation under constant temperature water bath, adjusts bath temperature and is
80~100 DEG C, constant temperature stirs 0.5~2h and obtains presoma；
In the step a, the vanadium source is vanadic anhydride, ammonium metavanadate or vanadic sulfate；The vanadium source and oxalic acid
Molar concentration rate is 1:2；The tungsten source is wolframic acid, ammonium tungstate or sodium tungstate, and the additional amount in the tungsten source is the foreign atom of tungsten
Percentage is 0.5~1at%.
Foreign atom percentage by adjusting tungsten realizes the regulation to vanadium dioxide crystalline phase state, and then improves titanium dioxide
The phase transition performance of vanadium.The foreign atom percentage of tungsten is 0.5~1at% in vanadium dioxide, and does not generate the second phase (WO3Or
WO2), do not destroy the crystal structure of vanadium dioxide, and phase transition temperature can effectively be adjusted, phase transition temperature is minimum to drop
Down to 30.5 DEG C, close to room temperature, in TcIt is adjusted in the range of=55.8~30.5 DEG C, is that a kind of phase transition performance is more excellent
Material, it is more sharp to be applied to production Thermochromic smart window, temperature sensor etc..
Further, the step c is to be centrifugated the product of step b, the anhydrous second for being 1:2~1:5 with volume ratio
The mixed liquor of pure and mild deionized water cleans, and after being dried in vacuo 6h at 50 DEG C, is annealed using high-purity argon gas, obtains target product.
In the step c, the processing parameter of the high-purity argon gas annealing are as follows: high-purity argon gas 0.5L/min, 30 DEG C of heatings
94min to 500 DEG C, constant temperature 1h.
The regulation to vanadium dioxide crystalline phase state is realized by annealing, and then improves the phase transition performance of vanadium dioxide.
Embodiment 1
The embodiment of the present invention 1 provides a kind of step hydro-thermal preparation adjustable pure phase VO of phase transition temperature2Raw powder's production technology,
The following steps are included:
A, 1.891g oxalic acid is added in beaker, addition 75mL deionized water, 40 DEG C of magnetic agitation 5min of constant temperature water bath,
1.365g vanadic anhydride is added in above-mentioned solution, 40 DEG C of magnetic agitation 15min of constant temperature water bath, adjusting bath temperature is 80
DEG C, constant temperature stirring 0.5h obtains presoma；
B, the step a presoma prepared is put into reaction kettle, in 280 DEG C of hydro-thermal reaction 72h；
C, the product of step b is centrifugated, it is clear with the mixed liquor of the volume ratio dehydrated alcohol for being 1:2 and deionized water
It washes, then after 50 DEG C of vacuum ovens drying process 6h, obtains the impure VO of crystalline phase state2Powder.The X-ray diffraction of product
(XRD) map is as shown in Figure 1, scanning electron microscope (SEM) map is as shown in Figure 2.
Embodiment 2
The embodiment of the present invention 2 provides a kind of step hydro-thermal preparation adjustable pure phase VO of phase transition temperature2Raw powder's production technology,
The following steps are included:
A, 1.891g oxalic acid is added in beaker, addition 75mL deionized water, 40 DEG C of magnetic agitation 5min of constant temperature water bath,
1.755g ammonium metavanadate is added in above-mentioned solution, 40 DEG C of magnetic agitation 15min of constant temperature water bath, adjusting bath temperature is 90 DEG C,
Constant temperature stirring 1h obtains presoma；
B, the step a presoma prepared is put into reaction kettle, in 280 DEG C of hydro-thermal reaction 72h；
C, the product of step b is centrifugated, it is clear with the mixed liquor of the volume ratio dehydrated alcohol for being 1:3 and deionized water
It washes, then after 50 DEG C of vacuum ovens drying process 6h, is put into stove and is made annealing treatment, be passed through protective atmosphere: high-purity argon
Gas 0.5L/min；Heat treatment condition: 30 DEG C 94min to 500 DEG C, constant temperature 1h of heating, cooled to room temperature in furnace obtains phase transformation
The pure phase VO that temperature is 55.8 DEG C2Powder.The optical performance parameter of product is as shown in table 1, X-ray diffraction (XRD) map such as Fig. 1
It is shown, scanning electron microscope (SEM) map as shown in Fig. 2, differential scanning calorimetric analysis (DSC) map as shown in figure 3, purple
Outside-visible-near-infrared spectrum is as shown in Figure 4.
Embodiment 3
The embodiment of the present invention 3 provides a kind of step hydro-thermal preparation adjustable pure phase VO of phase transition temperature2Raw powder's production technology,
The following steps are included:
A, 1.891g oxalic acid is added in beaker, addition 75mL deionized water, 40 DEG C of magnetic agitation 5min of constant temperature water bath,
2.445g vanadic sulfate is added in above-mentioned solution, 0.019g ammonium tungstate, 40 DEG C of magnetic agitations of constant temperature water bath are continuously added
15min, adjusting bath temperature is 100 DEG C, and constant temperature stirring 2h obtains presoma；
B, the step a presoma prepared is put into reaction kettle, in 280 DEG C of hydro-thermal reaction 72h；
C, the product of step b is centrifugated, it is clear with the mixed liquor of the volume ratio dehydrated alcohol for being 1:5 and deionized water
It washes, then after 50 DEG C of vacuum ovens drying process 6h, cooled to room temperature obtains the pure phase VO that phase transition temperature is 48.0 DEG C2
Powder.The optical performance parameter of product is as shown in table 1, and X-ray diffraction (XRD) map is as shown in Figure 1, scanning electron microscope
(SEM) map as shown in Fig. 2, differential scanning calorimetric analysis (DSC) map as shown in figure 3, ultraviolet-visible-near-infrared spectrum such as
Shown in Fig. 4.
Embodiment 4
The embodiment of the present invention 4 provides a kind of step hydro-thermal preparation adjustable pure phase VO of phase transition temperature2Raw powder's production technology,
The following steps are included:
A, 1.891g oxalic acid is added in beaker, addition 75mL deionized water, 40 DEG C of magnetic agitation 5min of constant temperature water bath,
2.445g vanadic sulfate is added in above-mentioned solution, continuously adds 0.038g wolframic acid, 40 DEG C of magnetic agitation 15min of constant temperature water bath,
Adjusting bath temperature is 100 DEG C, and constant temperature stirring 2h obtains presoma；
B, the step a presoma prepared is put into reaction kettle, in 280 DEG C of hydro-thermal reaction 72h；
C, the product of step b is centrifugated, it is clear with the mixed liquor of the volume ratio dehydrated alcohol for being 1:5 and deionized water
It washes, then after 50 DEG C of vacuum ovens drying process 6h, cooled to room temperature obtains the pure phase VO that phase transition temperature is 30.5 DEG C2
Powder.The optical performance parameter of product is as shown in table 1, and X-ray diffraction (XRD) map is as shown in Figure 1, scanning electron microscope
(SEM) map as shown in Fig. 2, differential scanning calorimetric analysis (DSC) map as shown in figure 3, ultraviolet-visible-near-infrared spectrum such as
Shown in Fig. 4.
1 optical performance parameter of table
From Fig. 1 and Fig. 3 it follows that the sample of the annealed processing of embodiment 2,3,4 or the preparation of tungsten source doping step is equal
For pure phase VO2, phase transition temperature is in TcIt is adjusted in the range of=55.8~30.5 DEG C.
Embodiment 3,4 and embodiment 1,2 compare, and explanation is that tungsten source doping is to adjust vanadium dioxide crystalline phase state purity
With the key parameter of phase transition temperature.
From figure 2 it can be seen that VO prepared by embodiment 1,22Powder is rendered as the pattern of block and snowflake, embodiment 3,
The VO of the tungsten source doping of 4 preparations2Powder is rendered as the Rod-like shape of preferred orientation growth；It can be learned from Fig. 3, Fig. 4 and table 1, phase
Than in the embodiment 2 of annealing, the VO of tungsten source doping pure phase sample prepared by embodiment 32Smart membrane has higher visible
Light transmission rate, bigger sunlight regulation rate, closer to the phase transition temperature of room temperature, so its phase transition performance is more excellent, more
Conducive to its practical application on energy saving pad pasting.
Comparative example
The one step hydro-thermal of one kind of this comparative example prepares the adjustable pure phase VO of phase transition temperature2The method of powder, including following step
It is rapid:
A, 1.891g oxalic acid is added in beaker, addition 75mL deionized water, 40 DEG C of magnetic agitation 5min of constant temperature water bath,
1.365g vanadic anhydride is added in above-mentioned solution, 40 DEG C of magnetic agitation 15min of constant temperature water bath, adjusting bath temperature is 80
DEG C, constant temperature stirring 0.5h obtains presoma；
B, the step a presoma prepared is put into reaction kettle, in 280 DEG C of hydro-thermal reaction 72h；
C, the product of step b is centrifugated, it is clear with the mixed liquor of the volume ratio dehydrated alcohol for being 1:2 and deionized water
It washes, then is obtained after 50 DEG C of vacuum ovens drying process 6h, the sample after drying process, which is put into stove, to be made annealing treatment, and is led to
Enter protective atmosphere: high-purity argon gas 0.5L/min；Heat treatment condition: 30 DEG C 94min to 500 DEG C, constant temperature 1h of heating, natural in furnace
It is cooled to room temperature, obtains the pure phase VO that phase transition temperature is 55.8 DEG C2Powder.
Optical performance parameter, differential scanning calorimetric analysis (DSC) map, X-ray diffraction for the product that comparative example obtains
(XRD) map and scanning electron microscope (SEM) map are consistent with the product that embodiment 2 obtains, embodiment 1,2 and comparative example
Three's comparison illustrates annealing for the key parameter of adjusting vanadium dioxide crystalline phase state purity.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (6)
1. an a kind of step hydro-thermal prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology, which is characterized in that including following
Step:
Step a, oxalic acid and deionized water 1:39 in mass ratio are mixed, carries out magnetic agitation under constant temperature water bath, vanadium is then added
Source is continued after carrying out magnetic agitation under constant temperature water bath, and adjusting bath temperature is 80~100 DEG C, before 0.5~2h of constant temperature stirring is obtained
Drive body；
Step b, the step a presoma prepared is put into reaction kettle, obtains product in 280 DEG C of hydro-thermal reaction 72h；
Step c, the product of step b is centrifugated, with the mixing of the volume ratio dehydrated alcohol for being 1:2~1:5 and deionized water
Liquid cleaning, obtains target product after being dried in vacuo 6h at 50 DEG C.
2. step hydro-thermal according to claim 1 prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology, it is special
Sign is, in the step a, the vanadium source is vanadic anhydride, ammonium metavanadate or vanadic sulfate；The vanadium source and oxalic acid rub
Your concentration ratio is 1:2.
3. step hydro-thermal according to claim 1 prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology, it is special
Sign is, the step a are as follows: step a, mixes oxalic acid and deionized water 1:39 in mass ratio, carries out magnetic force under constant temperature water bath
Then vanadium source and tungsten source is added in stirring, continue after carrying out magnetic agitation under constant temperature water bath, and adjusting bath temperature is 80~100 DEG C,
Constant temperature stirs 0.5~2h and obtains presoma.
4. step hydro-thermal according to claim 3 prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology, it is special
Sign is, in the step a, the vanadium source is vanadic anhydride, ammonium metavanadate or vanadic sulfate；The vanadium source and oxalic acid rub
Your concentration ratio is 1:2；The tungsten source is wolframic acid, ammonium tungstate or sodium tungstate, and the additional amount in the tungsten source is the foreign atom hundred of tungsten
Divide than being 0.5~1at%.
5. step hydro-thermal according to any one of claims 1-4 prepares the adjustable pure phase VO of phase transition temperature2The preparation of powder
Method, which is characterized in that the step c is to be centrifugated the product of step b, the dehydrated alcohol for being 1:2~1:5 with volume ratio
It cleans with the mixed liquor of deionized water, after being dried in vacuo 6h at 50 DEG C, is annealed using high-purity argon gas, obtain target product.
6. step hydro-thermal according to claim 5 prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology, it is special
Sign is, in the step c, the processing parameter of the high-purity argon gas annealing are as follows: high-purity argon gas 0.5L/min, 30 DEG C of heatings
94min to 500 DEG C, constant temperature 1h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811230839.9A CN108975401A (en) | 2018-10-22 | 2018-10-22 | One step hydro-thermal prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811230839.9A CN108975401A (en) | 2018-10-22 | 2018-10-22 | One step hydro-thermal prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108975401A true CN108975401A (en) | 2018-12-11 |
Family
ID=64544511
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811230839.9A Pending CN108975401A (en) | 2018-10-22 | 2018-10-22 | One step hydro-thermal prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108975401A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114920296A (en) * | 2022-06-14 | 2022-08-19 | 河南大学 | Vanadium oxide composite powder and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817113A (en) * | 2015-04-14 | 2015-08-05 | 中国科学院广州能源研究所 | Preparation method for non-stoichiometric ratio type nanometer VO2-x powder for regulating and controlling phase transition temperature |
-
2018
- 2018-10-22 CN CN201811230839.9A patent/CN108975401A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817113A (en) * | 2015-04-14 | 2015-08-05 | 中国科学院广州能源研究所 | Preparation method for non-stoichiometric ratio type nanometer VO2-x powder for regulating and controlling phase transition temperature |
Non-Patent Citations (1)
| Title |
|---|
| 王新刚等: ""掺钨VO2 纳米粉体的制备及其热致相变特能的研究"", 《中国陶瓷》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114920296A (en) * | 2022-06-14 | 2022-08-19 | 河南大学 | Vanadium oxide composite powder and preparation method and application thereof |
| CN114920296B (en) * | 2022-06-14 | 2024-01-19 | 河南大学 | Vanadium oxide composite powder and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101700909B (en) | Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method | |
| CN104925867B (en) | A kind of nanometer wolframic acid caesium powder body and preparation method and application | |
| CN109399710A (en) | Witch culture temperature induced color changing VO2Nano material and its preparation method and application | |
| CN104925863A (en) | Preparation method of monoclinic structure vanadium dioxide powder | |
| CN109319838A (en) | A kind of preparation method of rutile phase hypovanadic oxide ultra-fine nano-powder | |
| CN105753050B (en) | The preparation method and its particle of rutile phase hypovanadic oxide nano particle | |
| CN106082306B (en) | A kind of aluminum-doped zinc oxide nanometer powder and its microwave radiation technology preparation method and application | |
| CN106892573A (en) | A kind of preparation method of environment-friendly type thermochromism vanadium dioxide film | |
| CN110422879A (en) | A kind of high latent heat of phase change vanadium oxide powder and preparation method thereof | |
| CN105439458A (en) | Vanadium dioxide temperature control membrane preparation method and vanadium dioxide temperature control film | |
| CN108975401A (en) | One step hydro-thermal prepares the adjustable pure phase VO of phase transition temperature2Raw powder's production technology | |
| CN104724757A (en) | Method for directly synthesizing rutile phase vanadium dioxide nano powder based on solvothermal reaction at low temperature | |
| CN103409768B (en) | The preparation method of phase-M vanadium dioxide nanometre powder | |
| CN107032406B (en) | A kind of micro-nano beam of manganese molybdate and preparation method thereof | |
| CN104817113B (en) | A kind of non-stoichiometric type nanometer VO for regulating and controlling phase transition temperature2-xraw powder's production technology | |
| CN106517325A (en) | W-and-Eu-codoped vanadium dioxide film and preparation method thereof | |
| CN109399709A (en) | A kind of reduction VO2The method of powder heat treatment temperature and phase transition temperature | |
| CN108298582A (en) | One kind is by VO2The preparation method of hollow ball and film that nanoscale twins surround | |
| CN108585054B (en) | VO (volatile organic compound)2(M)-CoFe2O4Composite material and preparation method thereof | |
| CN114231253B (en) | Boron-doped monoclinic phase vanadium dioxide powder and preparation method thereof | |
| CN109517217A (en) | A kind of tungsten-doped vanadium dioxide/graphene complex and the preparation method and application thereof | |
| CN108654663A (en) | A kind of mixed nitrate molten-salt growth method prepares the nitrogen co-doped single-crystal meso-pore TiO of boron2The method of catalysis material | |
| CN106915773A (en) | A kind of preparation method of strontium molybdate skeleton | |
| CN108946810A (en) | Carambola shape M phase fluorine molybdenum codope hypovanadic oxide powder and its preparation method and application | |
| CN108946812A (en) | Alkali tungsten bronze nanometer rods and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181211 |
|
| WD01 | Invention patent application deemed withdrawn after publication |