CN102826604A - Preparation method of vanadium dioxide powder - Google Patents
Preparation method of vanadium dioxide powder Download PDFInfo
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- CN102826604A CN102826604A CN2012103644393A CN201210364439A CN102826604A CN 102826604 A CN102826604 A CN 102826604A CN 2012103644393 A CN2012103644393 A CN 2012103644393A CN 201210364439 A CN201210364439 A CN 201210364439A CN 102826604 A CN102826604 A CN 102826604A
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- powder
- vanadium
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- hypovanadic oxide
- oxide powder
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Abstract
The invention discloses a preparation method of vanadium dioxide powder, which comprises the steps of: evenly mixing vanadium pentoxide powder and simple substance vanadium powder, tabletting and then carrying out heat treatment to obtain the vanadium dioxide powder. The vanadium dioxide powder obtained by the method is accurate and controllable in stoichiometric ratio composition as well as simple and easy in control of method, and macro quantity preparation can be realized.
Description
Technical field
But the present invention relates to a kind of method for preparing hypovanadic oxide powder of simple and magnanimity, be specifically related to Vanadium Pentoxide in FLAKES powder and elemental vanadium powder uniform mixing and compressing tablet after thermal treatment is reacted to prepare the method for hypovanadic oxide powder.
Background technology
Because the energy dilemma in the whole world, energy-saving building receives publicity just day by day, but present building has adopted the form of glass curtain wall in large quantities, and therefore how the heat exchange of feed glass window becomes most important to whole energy.High performance light modulation thin-film material; Like low emissivity glass plated film and discoloration coating etc.; Will yield unusually brilliant results in this field, because they can keep room temp and purpose of energy saving thereby play to the seeing through and reflection of the making one's options property of sunshine in the particular range of wavelengths.
In the prior art, vanadium dioxide (VO
2) be one type in the light modulation field very promising thermochromic material because it has a metal/semiconductor phase transformation near 68 ℃, promptly change the monocline phase mutually into from rutile.The variation of 4 ~ 5 one magnitude can take place in the resistivity of vanadium dioxide before and after the phase transformation; Its reflectivity near infrared light also can be undergone mutation simultaneously; Because this characteristic vanadium dioxide film is widely used on the intelligent glass window, can the heat exchange of active adjustment glass port through the nernst cell internal and external temperature.Vanadium dioxide film adopts method preparations such as chemical method such as chemical bath method, crystal pulling method and physics method such as magnetron sputtering method usually.These methods all relate to the precursor hypovanadic oxide powder, and especially the target of physics method prepares raw material.
Hypovanadic oxide powder preparation method now or employing V
2O
5Chemical reduction method in atmosphere reduction or the solution (CN201110024215.3 for example, CN200810202066.3, CN200610125435.4).But these method preparation process are loaded down with trivial details relatively, and some preparation method also need add organic solvent, have adverse influence for environment and operator's health.And the hypovanadic oxide powder stoichiometric ratio of final gained is difficult to control, exist the problem of raw material recovery and reuse and preparation amount limited, and cost keeping also is problem.
Summary of the invention
For but magnanimity prepares accurately controlled hypovanadic oxide powder of stoichiometric ratio, the present invention proposes a kind of preparation method of hypovanadic oxide powder, said method comprises:
(1) with Vanadium Pentoxide in FLAKES powder and elemental vanadium powder uniform mixing;
(2) compressing tablet is after the thermal treatment reaction obtains hypovanadic oxide powder.
In one embodiment of the present invention, said Vanadium Pentoxide in FLAKES powder and elemental vanadium powder carry out uniform mixing according to the vanadium dioxide stoichiometric ratio.
In one embodiment of the present invention, said thermal treatment reaction is in inert atmosphere or airtight oxygen-free environment, to carry out.
In one embodiment of the present invention, the temperature of said thermal treatment reaction is 400 ~ 750 ℃.
In one embodiment of the present invention, the time of said thermal treatment reaction is 1 ~ 24 hour.
In one embodiment of the present invention, said Vanadium Pentoxide in FLAKES powder and elemental vanadium powder are commercially available or homemade.
In the present invention, commercially available or homemade Vanadium Pentoxide in FLAKES powder and elemental vanadium powder are carried out uniform mixing according to the vanadium dioxide stoichiometric ratio, and carry out compressing tablet and handle.The gained lamellar body carries out temperature in inert atmosphere or airtight oxygen-free environment be 400 ~ 750 ℃ thermal treatment, and the treatment time is 1 ~ 24 hour.Thermal treatment finishes the back grinding and obtains hypovanadic oxide powder.
Among the present invention, the hypovanadic oxide powder stoichiometric ratio composition of acquisition is accurately controlled, and simultaneously present method does not relate to solvent, does not have adverse influence for environment and operator's health, and, method of the present invention easy control simple to operate and can realize that magnanimity prepares.
In the present invention; The market value of the Vanadium Pentoxide in FLAKES powder that uses is about 80 yuan/kilogram; The market value of the market value of elemental vanadium and Vanadium Pentoxide in FLAKES powder is suitable, also is about 80 yuan/kilogram, and the market value of the vanadium dioxide that the inventive method makes is about 130 yuan/kilogram.Be appreciated that vanadium dioxide (VO for 1 kilogram of every preparation
2) product just has the price difference about 50 yuan, expenses such as deduction energy consumption and manual work, obviously, it is huge that use the inventive method prepares the profit margin of vanadium dioxide.
From the application's inventive principle, the inventive method is simple in addition, and controllability is higher; Ingredient proportion control through suitable can accurately realize VO
2Prepared in high purity.With respect to the present invention, loaded down with trivial details V
2O
5Chemical reduction method in atmosphere reduction or the solution, the control of purity operability is had relatively high expectations.Thorough mixing among the present invention and compressing tablet sintering all are to promote VO
2The reduction of rapid and uniform preparation and production energy consumption.
Embodiment
Below in conjunction with embodiment the present invention is done further explain.It should be noted that content of the present invention is not limited to these concrete embodiments.Under the prerequisite that does not deviate from background of the present invention and spirit, those skilled in the art can carry out substitutions and modifications of equal value on the basis of reading content of the present invention, and its content is also included within the scope of protection of present invention.
Embodiment 1
According to vanadium dioxide general formula VO
2, take by weighing stoichiometric ratio (V
2O
5With the mol ratio of simple substance V be 2:1) Vanadium Pentoxide in FLAKES powder 10.91 gram restrain with elemental vanadium powder 1.53, insert in the ZIRCONIUM DIOXIDE 99.5 ball milling jar and carried out milling mixing 2 hours.
Powder compression molding behind the ball milling and being transferred to carries out argon atmospher protection thermal treatment in the atmosphere furnace.Thermal treatment temp is 650 ℃, and heat treatment time is 6 hours; Reaction is taken out lamellar body after finishing to reduce to room temperature, grinds and obtains hypovanadic oxide powder.
Embodiment 2
According to vanadium dioxide general formula VO
2, take by weighing stoichiometric ratio (V
2O
5With the mol ratio of simple substance V be 2:1) Vanadium Pentoxide in FLAKES powder 3.64 gram restrain with elemental vanadium powder 0.51, inserted in the agate mortar hand lapping mixing 30 minutes.Powder compression molding behind the mixing also is transferred in the silica tube, and carries out Vacuum Package.
The silica tube of encapsulation is inserted in the retort furnace and heat-treated.Thermal treatment temp is 500 ℃, and heat treatment time is 15 hours; Reaction is opened silica tube taking-up lamellar body after finishing to reduce to room temperature, grinds and obtains hypovanadic oxide powder.
Embodiment 3
According to vanadium dioxide general formula VO
2, take by weighing stoichiometric ratio (V
2O
5With the mol ratio of simple substance V be 2:1) Vanadium Pentoxide in FLAKES powder 873.02 gram and elemental vanadium powder 122.56 grams, insert and carry out roller in the polytetrafluoroethyltank tank and ground mixing 12 hours.
Powder compression molding behind the mixing also is transferred to and carries out nitrogen atmosphere protection thermal treatment in the atmosphere furnace.Thermal treatment temp is 450 ℃, and heat treatment time is 20 hours; Reaction is taken out lamellar body after finishing to reduce to room temperature, grinds and obtains hypovanadic oxide powder.
Embodiment 4
According to vanadium dioxide general formula VO
2, take by weighing stoichiometric ratio (V
2O
5With the mol ratio of simple substance V be 2:1) Vanadium Pentoxide in FLAKES powder 5.09 gram restrain with elemental vanadium powder 0.71, inserted in the agate mortar hand lapping mixing 30 minutes.
Powder compression molding after the grinding and being transferred to carries out argon atmospher protection thermal treatment in the atmosphere furnace.Thermal treatment temp is 700 ℃, and heat treatment time is 4 hours; Reaction is taken out lamellar body after finishing to reduce to room temperature, grinds and obtains hypovanadic oxide powder.
Claims (6)
1. the preparation method of a hypovanadic oxide powder, said method comprises:
(1) with Vanadium Pentoxide in FLAKES powder and elemental vanadium powder uniform mixing;
(2) compressing tablet is after the thermal treatment reaction obtains hypovanadic oxide powder.
2. the preparation method of hypovanadic oxide powder according to claim 1, it is characterized in that: said Vanadium Pentoxide in FLAKES powder and elemental vanadium powder carry out uniform mixing according to the vanadium dioxide stoichiometric ratio.
3. the preparation method of hypovanadic oxide powder according to claim 1 is characterized in that: said thermal treatment is in inert atmosphere or airtight oxygen-free environment, to carry out.
4. the preparation method of hypovanadic oxide powder according to claim 1, it is characterized in that: said heat treated temperature is 400 ~ 750 ℃.
5. the preparation method of hypovanadic oxide powder according to claim 1, it is characterized in that: said heat treatment time is 1 ~ 24 hour.
6. the preparation method of hypovanadic oxide powder according to claim 1, it is characterized in that: said Vanadium Pentoxide in FLAKES powder and elemental vanadium powder are commercially available or homemade.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103644393A CN102826604A (en) | 2012-09-26 | 2012-09-26 | Preparation method of vanadium dioxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103644393A CN102826604A (en) | 2012-09-26 | 2012-09-26 | Preparation method of vanadium dioxide powder |
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| CN102826604A true CN102826604A (en) | 2012-12-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693691A (en) * | 2013-12-20 | 2014-04-02 | 中国科学院上海硅酸盐研究所 | Method of preparing vanadium dioxide by double-temperature area reduction process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880060A (en) * | 2010-07-14 | 2010-11-10 | 中国科学技术大学 | Method for quickly preparing monoclinic phase VO2 |
| CN102336436A (en) * | 2010-07-20 | 2012-02-01 | 中国科学技术大学 | Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame |
-
2012
- 2012-09-26 CN CN2012103644393A patent/CN102826604A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880060A (en) * | 2010-07-14 | 2010-11-10 | 中国科学技术大学 | Method for quickly preparing monoclinic phase VO2 |
| CN102336436A (en) * | 2010-07-20 | 2012-02-01 | 中国科学技术大学 | Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame |
Non-Patent Citations (1)
| Title |
|---|
| D. W. MURPHY等: "Lithium Incorporation V6O13 by and Related Vanadium (+4, +5) Oxide Cathode Materials", 《J. EIECTROCHEM. SOC,》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693691A (en) * | 2013-12-20 | 2014-04-02 | 中国科学院上海硅酸盐研究所 | Method of preparing vanadium dioxide by double-temperature area reduction process |
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| C53 | Correction of patent of invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Huang Fuqiang Inventor after: Liu Zhanqiang Inventor before: Huang Fuqiang |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: HUANG FUQIANG TO: HUANG FUQIANG LIU ZHANQIANG |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20121219 |