CN102336436A - Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame - Google Patents

Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame Download PDF

Info

Publication number
CN102336436A
CN102336436A CN201010234000XA CN201010234000A CN102336436A CN 102336436 A CN102336436 A CN 102336436A CN 201010234000X A CN201010234000X A CN 201010234000XA CN 201010234000 A CN201010234000 A CN 201010234000A CN 102336436 A CN102336436 A CN 102336436A
Authority
CN
China
Prior art keywords
phase
vanadium
containing compound
metallic element
doped
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.)
Granted
Application number
CN201010234000XA
Other languages
Chinese (zh)
Other versions
CN102336436B (en
Inventor
谢毅
白亮飞
宋磊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Science and Technology of China USTC
Original Assignee
University of Science and Technology of China USTC
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by University of Science and Technology of China USTC filed Critical University of Science and Technology of China USTC
Priority to CN 201010234000 priority Critical patent/CN102336436B/en
Publication of CN102336436A publication Critical patent/CN102336436A/en
Application granted granted Critical
Publication of CN102336436B publication Critical patent/CN102336436B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a method for preparing a monoclinic-phase VO2 (vanadium dioxide) and doped powder of monoclinic-phase VO2 by utilizing lean flame, and the method comprises the following steps of: placing a vanadium-containing compound or the vanadium-containing compound doped with a metal element in the lean flame of an organic solvent to carry out a reaction, and cooling to obtain the monoclinic-phase VO2 after the reaction is completed. According to the method, the solid-phase powder of a vanadium-containing raw material is directly arranged in the flame of an organic solvent such as ethanol and the like to react; the reaction process and equipment are quite simple; and the method is a simple and efficient method which can be industrialized easily for preparing VO2 (M) (metal) which is an intelligent window material. The VO2 (M) and the doped powder of VO2 (M), which are prepared by the method, have excellent performances, and are quite important intelligent window materials.

Description

Utilize fuel-rich flame to prepare monocline phase VO 2Method
Technical field
The invention belongs to the flame method preparing technical field, relate to a kind of fuel-rich flame that utilizes and prepare monocline phase VO 2Method.
Background technology
In various smart window materials, has the VO of metal insulator phase-change characteristic 2(M), all receive the extensive concern of academia and industry member owing to optimum transformation temperature always.
VO 2(M) (monocline phase VO 2) be the monocline insulation phase of infrared light transmission at low temperatures, along with the rising of envrionment temperature, more than 68 ℃ the time, VO 2(M) change the cubic metallographic phase (rutile phase) of infrared into, during this transfer, VO 2(M) specific conductivity also can take place 10 5The transformation of the order of magnitude.These character make VO 2(M) have a wide range of applications at electrooptical device and solar energy intelligent window field.Simultaneously, if at VO 2(M) mix elements such as an amount of W, Mo, Cr, Ti in, its transformation temperature can be reduced to 20-30 ℃, and infrared transmittivity changes still very greatly before and after the phase transformation.If adulterated VO 2(M) be applied in the buildings smart window; Utilize the infrared transmittivity of its temperature correlation, make window have the infrared permeation in winter, summer infrared effect; Can effectively reduce buildings warming, summer air-conditioning refrigerating energy consumption; Save a large sum of expense, reached energy-conservation and dp environmental protection, produced significant social and economic benefit.
Up to the present, the method for preparing smart window material hypovanadic oxide powder mainly contains following two kinds: a kind of is vapour deposition VO under logical hydrogen or inert atmosphere protection 2(M), but this method requirement condition is harsh, and complex equipments, cost costliness are difficult to the valence state of control vanadium wherein simultaneously, is difficult to obtain the VO of pure phase 2(M).A kind of in addition is at high temperature to use V 2O 5And V 2O 3Quantitative reaction is perhaps decomposed complicated precursor and prepared, and is too high but this temperature of reaction requires, and generally all more than 700-800 ℃, the reaction metering is restive, and product is very impure.Therefore development is efficient more, raw material is simple, with low cost, product purity is high, can mass-produced smart window material VO 2(M) method is particularly important.
Summary of the invention
The purpose of this invention is to provide a kind of fuel-rich flame that utilizes and prepare monocline phase VO 2Method.
Preparation monocline phase VO provided by the invention 2Method, comprise the steps: to place the fuel-rich flame of organic solvent to react vanadium-containing compound, the reaction finish the cooling after obtain said monocline phase VO 2
This method, said vanadium-containing compound are the compound with pyrolytic, can be selected from V 2O 5, NH 4VO 3, H 2V 3O 8, the methyl ethyl diketone vanadyl (is abbreviated as VO (acac) 2), A phase VO 2(be abbreviated as VO 2(A)), VOSO 4, VOC 2O 4, metastable phase VO 2(be abbreviated as VO 2(B)), paramontroseite (is abbreviated as VO 2(P) or VO 2(paramontroseite)), VOOH, V 2O 3And V (OH) 2NH 2In at least a, this vanadium-containing compound can not be Na 3VO 4Deng not heat decomposable vanadium-containing compound.Said organic solvent is selected from least a in absolute ethyl alcohol, methyl alcohol, Virahol, ether, propylene oxide, hexanaphthene, pimelinketone, toluene pimelinketone, pentane, hexane, octane, acetone, espeleton, mibk, acetonitrile, pyridine, phenol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, benzene,toluene,xylene, ritalin, vinyl acetic monomer, propyl acetate, chlorobenzene, dichlorobenzene and the methylene dichloride, at least a in preferred anhydrous methanol and the ethanol.Said organic solvent is anhydrous solvent.Said preparation monocline phase VO 2Method; Preferably include the method for following steps: in air atmosphere; Vanadium-containing compound is placed at least a fuel-rich flame of said absolute ethyl alcohol and methyl alcohol and with under the condition that air contacts do not react, and reaction finishes and obtains said monocline phase VO after the cooling 2In the said reactions step, the reaction times is 1 minute to 10 hours, is specially preferred 45 minutes 45 minutes-1 hour.
Preparation provided by the invention is doped with the monocline phase VO of metallic element 2Method, comprise the steps: to place the fuel-rich flame of organic solvent to react the vanadium-containing compound that is doped with metallic element, the reaction finish the cooling after obtain the said monocline phase VO that is doped with metallic element 2
In this method, said vanadium-containing compound is the compound with pyrolytic, can be selected from V 2O 5, NH 4VO 3, H 2V 3O 8, (NH 4) 2V 3O 8, the methyl ethyl diketone vanadyl (is abbreviated as VO (acac) 2), A phase VO 2(be abbreviated as VO 2(A)), VOSO 4, VOC 2O 4, metastable phase VO 2(be abbreviated as VO 2(B)), paramontroseite (is abbreviated as VO 2(P) or VO 2(paramontroseite)), VOOH, V 2O 3And V (OH) 2NH 2In at least a, this vanadium-containing compound can not be Na 3VO 4Deng not heat decomposable vanadium-containing compound.Said metallic element is selected from least a in tungsten and the molybdenum element.Said organic solvent is selected from least a in absolute ethyl alcohol, methyl alcohol, Virahol, ether, propylene oxide, hexanaphthene, pimelinketone, toluene pimelinketone, pentane, hexane, octane, acetone, espeleton, mibk, acetonitrile, pyridine, phenol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, benzene,toluene,xylene, ritalin, vinyl acetic monomer, propyl acetate, chlorobenzene, dichlorobenzene and the methylene dichloride, at least a in preferred anhydrous methanol and the ethanol.Said organic solvent is anhydrous solvent.The mol ratio of v element is 0-15 in said metallic element and the said vanadium-containing compound: 100, and preferred 0-10: 100, more preferably 5: 100, the mole dosage of said metallic element was not 0.Said preparation is doped with the monocline phase VO of metallic element 2Method be preferably the method that comprises the steps: in air atmosphere; The vanadium-containing compound that is doped with metallic element is placed at least a fuel-rich flame of said absolute ethyl alcohol and methyl alcohol and with under the condition that air contacts do not react, and reaction finishes and obtains the said monocline phase VO that is doped with metallic element after the cooling 2In the said reactions step, the reaction times is 1 minute to 10 hours, is specially preferred 45 minutes 45 minutes-1 hour.
In this method, the vanadium-containing compound that is doped with metallic element can prepare according to various ordinary methods.As to prepare the Mo doping be 5% VO 2(B) (this doping representes that the mol ratio of Mo and V is 5: 95), can prepare according to following method: at volume is gathering of 35ml to add 2.375mmol V in the tetrafluoro reactor 2O 5, 0.25mmol (NH 4) 2MoO 4, 8mmol H 2C 2O 4With 30ml zero(ppm) water, stir 20min then, reaction kettle is placed metal shell; In 200 ℃ high temperature oven, keep 48h, behind the naturally cooling, centrifugal products therefrom; And respectively wash three times with zero(ppm) water and absolute ethyl alcohol; Keep 6h at 60 ℃ vacuum drying oven then, obtain exsiccant royal purple grey powder, be the Mo doping and be 5% VO 2(B) powder.
Owing in the reaction process of above-mentioned two methods, may produce the dust of trace, so reaction unit preferably places stink cupboard, and the operator need wear masks and the gloves protection.
In practical application, as long as guarantee that vanadium-containing compound all the time among the encirclement of organic solvent fuel-rich flame, can obtain VO 2(M).So used reaction unit is variously can realize the vanadium-containing compound various devices among fuel-rich flame all the time; As can be and be selected from following two kinds of devices any one: a kind of is the device that liquid level constantly descends in combustion processes; Add the device that quartz holder is formed as add glass, iron wire or a 100ml beaker by a 100ml beaker; Another kind is the invariable all the time device of liquid level, like the device of being made up of a glass beaker, liquid level constant communicating vessels, glass (or quartz or iron wire) support.
Principle of the present invention is: in the fuel-rich flame of organic solvent, contain CH 3, C 2H 4, CH 3OH, C 3H 3, C 3H 4, C 2H 4O, C 2H 6O, C 4H 2, C 4H 4, C 4H 6, C 3H 4O, C 3H 6O, C 3H 8O, CO, H 2O, H 2, CO 2, C and O 2Etc. multiple material; These materials have oxidisability a bit; Some has reductibility, and the concentration of various materials presents three-dimensional three-dimensional a distribution, these materials in fuel-rich flame zone in flame in whole flame; Its redox integration capability makes V just can be stabilized in positive tetravalence, and the most stable under the high temperature in positive tetravalence is again VO 2(R) (VO 2(M) high temperature phase), therefore, in fuel-rich flame, put into various vanadium source (like V 2O 5, VO 2(B) or V 2O 3Deng) through after certain reaction times, all can become VO 2(R), after the knock down the flame cooling, promptly obtain purified VO 2(M).
Adopt the inventive method to prepare smart window material vanadium dioxide and adulterated powder thereof; Have the following advantages: directly place the flame of organic solvent such as ethanol to react because the inventive method is the solid phase powder that directly will contain the V raw material; Reaction process and equipment are very simple, get final product a step with business-like V without any other reagent 2O 5Powder, business-like NH 4VO 3Powder or business-like V 2O 3The powder stock direct oxidation is reduced to title product VO 2(M), be a kind of simple, efficient, easy industrialized preparation smart window material VO 2(M) method.The VO that this method is prepared 2(M) having good performance, is very important smart window material.
Description of drawings
Fig. 1 is that a kind of embodiment is by various feedstock production products therefrom VO 2(M) XRD figure spectrum.
Fig. 2 prepares VO among the embodiment 1 with different material 2(M) DSC characterizes.
Fig. 3 is that the XRD figure spectrum and the DSC of embodiment 2 products therefroms characterizes.
Fig. 4 is that the XRD figure spectrum and the DSC of embodiment 3 products therefroms characterizes.
Embodiment
Below in conjunction with specific embodiment the present invention is described further, but the present invention is not limited to following examples.If no special instructions, said method is ordinary method among the following embodiment.Used V among the following embodiment 2O 5, VOSO 4, VO (acac) 2, V 2O 3And NH 4VO 3, all can obtain by open commercial sources purchase.
Used H among the present invention 2V 3O 8, VOC 2O 4, VO 2(A), VO 2(B), VO 2(paramontroseite), VOOH, V (OH) 2NH 2All be to get according to following method preparation:
H 2V 3O 8The preparation method: at volume is to add 53mg VO (acac) in the polytetrafluoroethylkettle kettle of 55ml 2With 50ml zero(ppm) water, then reaction kettle is kept 30min in 90 ℃ High Temperature Furnaces Heating Apparatus, take out the reaction kettle stirring then and make its naturally cooling; Add the HCl that 0.2ml concentration is 1M again, continue to stir after ten minutes, obtain yellowish green solution; Then reaction kettle is packed in the metal shell, place 200 ℃ High Temperature Furnaces Heating Apparatus to keep 12h, behind the naturally cooling; Spinning gained deposition, and respectively wash three times with zero(ppm) water and absolute ethyl alcohol is then at 60 ℃ vacuum drying oven maintenance 6h; Obtain exsiccant greyish-green sheet sample, be H 2V 3O 8
VOC 2O 4The preparation method: at volume is to add 4mmol V in the volumetric flask of 100ml 2O 5, 9mmol H 2C 2O 4With 20ml zero(ppm) water, the 8h that in 70 ℃ oil bath, refluxes then filters gained solution then; Gained filtrating is transferred in the glass beaker of 250ml; Then beaker is placed 90 ℃ baking oven, place the sufficiently long time, let filtrating volatilize fully; Collect the product in the beaker, the powder that gets greyish-green after the grinding is VOC 2O 4
VO 2(A) preparation method: at volume is to add 3mol VO (acac) in the tetrafluoroethylene reaction kettle of 55ml 2With 50ml zero(ppm) water, stir 20min then, reaction kettle is placed metal shell; In 220 ℃ high temperature oven, keep 24h; Behind the naturally cooling, centrifugal products therefrom, and respectively wash three times with zero(ppm) water and absolute ethyl alcohol; At 60 ℃ vacuum drying oven maintenance 6h, obtain the exsiccant brown powder and be VO then 2(A).
VO 2(B) preparation method: at volume is to add 5mol V in the tetrafluoroethylene reaction kettle of 35ml 2O 5, 8mmolH 2C 2O 4With 30ml zero(ppm) water, stir 20min then, reaction kettle is placed metal shell; In 200 ℃ high temperature oven, keep 48h; Behind the naturally cooling, centrifugal product, and respectively wash three times with zero(ppm) water and absolute ethyl alcohol; At 60 ℃ vacuum drying oven maintenance 6h, obtain exsiccant pewter powder and be VO then 2(B).Reference: Zhang, K.F., X.Liu, et al. (2007). " VO 2(R) nanobelts resulting from the irreversible transformation of VO 2(B) nanobelts. " Materials Letters61 (13): 2644-2647.
VO 2(paramontroseite) preparation method: in volume is the tetrafluoroethylene reaction kettle of 55ml, add 4molNa 3VO 4, 20mmol thioacetamide and 50ml zero(ppm) water, stir 20min then, reaction kettle is placed metal shell; In 200 ℃ high temperature oven, keep 12h; Behind the naturally cooling, centrifugal products therefrom, and respectively wash three times with zero(ppm) water and absolute ethyl alcohol; At 60 ℃ vacuum drying oven maintenance 6h, obtain black powder and be VO then 2(paramontroseite).Reference: Wu, C.Z., Z.P.Hu, et al. (2008). " Synthetic paramontroseite VO 2With good aqueous lithium-ion battery performance. " Chemical Communications(33): 3891-3893.
The preparation method of VOOH: at volume is to add 5mol NH in the tetrafluoroethylene reaction kettle of 55ml 4VO 3, the 1.5ml mass percentage concentration is 85% N 2H 42H 2O and 48.5ml zero(ppm) water stir 30min then, and reaction kettle is placed metal shell; In 200 ℃ high temperature oven, keep 12h; Behind the naturally cooling, centrifugal products therefrom, and respectively wash three times with zero(ppm) water and absolute ethyl alcohol; At 60 ℃ vacuum drying oven maintenance 6h, obtain dark gray powder and be VOOH then.Reference: Wu, C.Z., Y.Xie, et al. (2006). " Synthesis ofnew-phased VOOH hollow " dandelions " and their application in lithium-ion batteries. " Advanced Materials18 (13): 1727-1732.
V (OH) 2NH 2The preparation method: at volume is to add 2mmol NH in the beaker of 100ml 4VO 3With 45ml zero(ppm) water, stir 10min after, the speed with 0.5ml/min slowly drips like 1ml 1M HCl then, behind the restir 10min, solution becomes orange-red clear liquor, adds the 2ml mass percentage concentration again and be 85% N 2H 42H 2The O aqueous solution stirs 40min, obtains the light gray green suspension liquid, centrifugal sediment, and respectively wash three times with zero(ppm) water and absolute ethyl alcohol, in 60 ℃ vacuum drying oven, keep 6h then, obtain the light gray powder and be V (OH) 2NH 2Reference: Wu; C.Z.; X.D.Zhang, et al. (2009). " Shape Evolution of New-Phased Lepidocrocite VOOH from Single-Shelled to Double-Shelled Hollow Nanospheres on the Basis of Programmed Reaction-Temperature Strategy. " Inorganic Chemistry48 (13): 6044-6054.
Embodiment 1
After in a 100ml glass beaker that is built-in with highly to the glass stake of 4.5cm, adding the 50ml absolute ethyl alcohol, then respectively with the V of 80mg 2O 5, NH 4VO 3, H 2V 3O 8, VOSO 4, VO (acac) 2, VOC 2O 4, VO 2(A), VO 2(B), VO 2(paramontroseite), V 2O 3, VOOH and V (OH) 2NH 2Powder is spread out and is layered on the simple glass sheet, this sheet glass is placed in the glass stake again, in air atmosphere, lights said absolute ethyl alcohol; Above-mentioned vanadium-containing compound is in the said alcoholic acid fuel-rich flame all the time; And do not contact, behind the burning 45min, the Alcohol Flame lid is gone out with watch-glass with air; The sample on the sheet glass is collected in the cooling back, promptly gets VO after the washing drying 2(M) powder.
Fig. 1 is this embodiment 1 preparation products therefrom VO 2(M) XRD figure spectrum, Fig. 2 prepares products therefrom VO for this embodiment 2(M) DSC characterizes.Can know that by above-mentioned detected result the products therefrom structure is correct, be VO 2(M), and purity be 99%.
Embodiment 2
In the 100ml beaker that has communication apparatus, add highly be the absolute ethyl alcohol of 2ml after, the iron wire shelf that in beaker, to put into a height then be 3.5cm is with the V of 80mg 2O 5Powder and NH 4VO 3Powder is spread out and is layered on the common sheet glass, and sheet glass is put on the iron wire shelf in the beaker; In air atmosphere, light said absolute ethyl alcohol; Above-mentioned vanadium-containing compound is in the said alcoholic acid fuel-rich flame all the time, and does not contact, burn and cover the Alcohol Flame of going out with watch-glass after 1 hour with air; The sample on the sheet glass is collected in the cooling back, promptly gets VO after the washing drying 2(M) powder.
Fig. 3 can be known by above-mentioned detected result that for XRD figure spectrum and the DSC that this embodiment prepares products therefrom characterizes the products therefrom structure is correct, is VO 2(M), and purity be 99%.
Embodiment 3
1) preparation Mo doping is 5% VO 2(B) (this doping representes that the mol ratio of Mo and V is 5: 95): at volume is gathering of 35ml to add 2.375mmol V in the tetrafluoro reactor 2O 5, 0.25mmol (NH 4) 2MoO 4, 8mmolH 2C 2O 4With 30ml zero(ppm) water, stir 20min then, reaction kettle is placed metal shell; In 200 ℃ high temperature oven, keep 48h, behind the naturally cooling, centrifugal products therefrom; And respectively wash three times with zero(ppm) water and absolute ethyl alcohol; Keep 6h at 60 ℃ vacuum drying oven then, obtain exsiccant royal purple grey powder, be the Mo doping and be 5% VO 2(B) powder.
2) in a 100ml glass beaker that is built-in with highly to the glass stake of 4.5cm, add the 50ml anhydrous methanol after, be 5% VO then with the said Mo doping of 80mg 2(B) powder is spread out and is layered on the simple glass sheet, sheet glass is placed in the glass stake again, in air atmosphere, lights said anhydrous methanol; Above-mentioned vanadium-containing compound is in the fuel-rich flame of said methyl alcohol all the time; And do not contact, behind the burning 45min, methyl alcohol flame lid is gone out with watch-glass with air; The sample on the sheet glass is collected in cooling back, promptly gets the Mo doping after the washing drying and be 5% VO 2(M) powder.
Fig. 4 can be known by above-mentioned detected result that for XRD figure spectrum and the DSC that this embodiment prepares products therefrom characterizes the products therefrom structure is correct, is 5% VO for the Mo doping 2(M) powder, and purity is 99%.

Claims (10)

1. one kind prepares monocline phase VO 2Method, comprise the steps: to place the fuel-rich flame of organic solvent to react vanadium-containing compound, the reaction finish the cooling after obtain said monocline phase VO 2
2. method according to claim 1 is characterized in that: said vanadium-containing compound is selected from V 2O 5, NH 4VO 3, H 2V 3O 8, methyl ethyl diketone vanadyl, A phase VO 2, VOSO 4, VOC 2O 4, metastable phase VO 2, paramontroseite, VOOH, V 2O 3And V (OH) 2NH 2In at least a;
Said organic solvent is selected from least a in absolute ethyl alcohol, methyl alcohol, Virahol, ether, propylene oxide, hexanaphthene, pimelinketone, toluene pimelinketone, pentane, hexane, octane, acetone, espeleton, mibk, acetonitrile, pyridine, phenol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, benzene,toluene,xylene, ritalin, vinyl acetic monomer, propyl acetate, chlorobenzene, dichlorobenzene and the methylene dichloride.
3. method according to claim 2 is characterized in that: said organic solvent is selected from least a in anhydrous methanol and the ethanol.
4. according to the arbitrary described method of claim 1-3, it is characterized in that: in the said reactions step, the reaction times is 1 minute to 10 hours, preferred 45 minutes.
5. according to the arbitrary described method of claim 2-4, it is characterized in that: said preparation monocline phase VO 2Method, comprise the steps: that in air atmosphere vanadium-containing compound is placed at least a fuel-rich flame of said absolute ethyl alcohol and methyl alcohol and with under the condition that air contacts do not react, and reaction finishes and obtains said monocline phase VO after the cooling 2
6. one kind prepares the monocline phase VO that is doped with metallic element 2Method, comprise the steps: to place the fuel-rich flame of organic solvent to react the vanadium-containing compound that is doped with metallic element, the reaction finish the cooling after obtain the said monocline phase VO that is doped with metallic element 2
7. method according to claim 6 is characterized in that: said vanadium-containing compound is selected from V 2O 5, NH 4VO 3, H 2V 3O 8, methyl ethyl diketone vanadyl, A phase VO 2, VOSO 4, VOC 2O 4, metastable phase VO 2, paramontroseite, VOOH, V 2O 3And V (OH) 2NH 2In at least a;
Said metallic element is selected from least a in tungsten and the molybdenum element;
Said organic solvent is selected from least a in absolute ethyl alcohol, methyl alcohol, Virahol, ether, propylene oxide, hexanaphthene, pimelinketone, toluene pimelinketone, pentane, hexane, octane, acetone, espeleton, mibk, acetonitrile, pyridine, phenol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, benzene,toluene,xylene, ritalin, vinyl acetic monomer, propyl acetate, chlorobenzene, dichlorobenzene and the methylene dichloride;
The mol ratio of v element is 0-15 in said metallic element and the said vanadium-containing compound: 100, and the mole dosage of said metallic element is not 0.
8. method according to claim 7 is characterized in that: said organic solvent is selected from least a in anhydrous methanol and the ethanol;
The mol ratio of v element is 0-10 in said metallic element and the said vanadium-containing compound: 100, and the mole dosage of said metallic element is not 0.
9. according to claim 6 or 7 described methods, it is characterized in that: in the said reactions step, the reaction times is 1 minute to 10 hours, preferred 45 minutes.
10. according to the arbitrary described method of claim 7-9, it is characterized in that: said preparation is doped with the monocline phase VO of metallic element 2Method; Comprise the steps: in air atmosphere; The vanadium-containing compound that is doped with metallic element is placed at least a fuel-rich flame of said absolute ethyl alcohol and methyl alcohol and with under the condition that air contacts do not react, and reaction finishes and obtains the said monocline phase VO that is doped with metallic element after the cooling 2
CN 201010234000 2010-07-20 2010-07-20 Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame Active CN102336436B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201010234000 CN102336436B (en) 2010-07-20 2010-07-20 Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201010234000 CN102336436B (en) 2010-07-20 2010-07-20 Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame

Publications (2)

Publication Number Publication Date
CN102336436A true CN102336436A (en) 2012-02-01
CN102336436B CN102336436B (en) 2013-12-25

Family

ID=45512444

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201010234000 Active CN102336436B (en) 2010-07-20 2010-07-20 Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame

Country Status (1)

Country Link
CN (1) CN102336436B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102826604A (en) * 2012-09-26 2012-12-19 中国科学院上海硅酸盐研究所 Preparation method of vanadium dioxide powder
CN103420420A (en) * 2013-07-13 2013-12-04 宿州学院 Preparation method for vanadium dioxide nanorod changed from phase B to phase A
CN103420419A (en) * 2013-05-07 2013-12-04 南京航空航天大学 High-temperature hydrothermal mixing synthesis method for vanadium dioxide powder
US20160131978A1 (en) * 2013-07-24 2016-05-12 Jsr Corporation Pattern forming method
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

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101481142A (en) * 2009-02-18 2009-07-15 大连理工大学 Method for preparing hypovanadic oxide doped powder material
CN101559981A (en) * 2009-05-27 2009-10-21 中国科学技术大学 Method for preparing vanadium dioxide and doping powder thereof by combustion method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101481142A (en) * 2009-02-18 2009-07-15 大连理工大学 Method for preparing hypovanadic oxide doped powder material
CN101559981A (en) * 2009-05-27 2009-10-21 中国科学技术大学 Method for preparing vanadium dioxide and doping powder thereof by combustion method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
LI, JING ET AL.: "The character of W-doped one-dimensional VO2(M)", 《JOURNAL OF SOLID STATE CHEMISTRY》 *
刘洋等: "空气环境下制备相变特性VO2薄膜", 《东华大学学报(自然科学版)》 *
林华等: "VO2的相变原理及影响相变的因素", 《功能材料》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102826604A (en) * 2012-09-26 2012-12-19 中国科学院上海硅酸盐研究所 Preparation method of vanadium dioxide powder
CN103420419A (en) * 2013-05-07 2013-12-04 南京航空航天大学 High-temperature hydrothermal mixing synthesis method for vanadium dioxide powder
CN103420420A (en) * 2013-07-13 2013-12-04 宿州学院 Preparation method for vanadium dioxide nanorod changed from phase B to phase A
CN103420420B (en) * 2013-07-13 2016-03-09 宿州学院 The preparation method of a kind of B Vanadium dioxide nanometer rod of A phase in version in opposite directions
US20160131978A1 (en) * 2013-07-24 2016-05-12 Jsr Corporation Pattern forming method
US9891526B2 (en) * 2013-07-24 2018-02-13 Jsr Corporation Pattern forming method
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

Also Published As

Publication number Publication date
CN102336436B (en) 2013-12-25

Similar Documents

Publication Publication Date Title
CN101880060B (en) Method for quickly preparing monoclinic phase VO2
Zhou et al. Structure‐Mediated Charge Separation in Boron Carbon Nitride for Enhanced Photocatalytic Oxidation of Alcohol
CN102336436B (en) Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame
CN106000431B (en) Sheet CdS/BiOCl composite nano materials and preparation method thereof
CN103464213B (en) Polypyrrole-TiO2 magnetically supported photocatalytic composite material and preparation method thereof
Zhang et al. Phosphorus-doped TiO2 for visible light-driven oxidative coupling of benzyl amines and photodegradation of phenol
Lv et al. Titanium-oxo clusters functionalized with catecholate-type ligands: modulating the optical properties through charge-transfer transitions
CN105819508B (en) A kind of spray pyrolysis prepares VO2(M) method of nano-powder and film
CN101559981B (en) Method for preparing vanadium dioxide and doping powder thereof by combustion method
CN107469851A (en) A kind of ultra-thin porous N doping g C3N4Photochemical catalyst and preparation method thereof
CN107899618B (en) Macrocyclic compound photosensitive dye and titanium dioxide-based hybrid material, preparation method thereof and application thereof in photocatalysis
CN102380367B (en) Control synthetic method of high-visible-light-activity mixed crystal type BiVO4 photocatalysts
CN106140141A (en) A kind of oxygen-containing defected ZnWO4catalysis material and preparation method thereof
CN105367591B (en) Cadimium complex monocrystal capable of catalyzing photodegradation of methylene blue, and preparation method thereof
CN101703948A (en) Novel method for preparing compound high-activity photocatalyst
CN103041795A (en) Preparation method of titanium dioxide photocatalyst
Chen et al. Bandgap engineering and oxygen vacancies of NixV2O5+ x (x= 1, 2, 3) for efficient visible light‐driven CO2 to CO with nearly 100% selectivity
CN105797739A (en) Preparation method and application of iron hydroxide/bismuth vanadate composite photocatalyst
Devi et al. Synthesis of BaTiO3/α-S8 composite for enhanced photocatalytic activity under UV/Solar light in comparison with α-S8 and BaTiO3 photocatalysts: Effect of spontaneous polarization
CN105080553A (en) Method for preparing stanniferous double-perovskite type phenol photocatalytic degradation catalyst
CN103007980B (en) Metal doped type visible light denitrification photocatalyst and preparation method and application thereof
Zhang et al. Novel Cerium‐Based Sulfide Nano‐Photocatalyst for Highly Efficient CO2 Reduction
CN104475142A (en) Visible-light-response doped sodium tantalum oxide and preparation method thereof
CN104801347A (en) Catalytic desulfurization agent of carboxylic substituent metal phthalocyanine sensitization Zn2SnO4 powder and preparation method for catalytic desulfurization agent
CN111393663A (en) Perylene bisimide base coordination polymer, preparation method and application thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant