CN103663556A - A-phase vanadium dioxide nanowire preparation method - Google Patents
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Abstract
The invention provides an A-phase vanadium dioxide nanowire preparation method. The A-phase vanadium dioxide nanowire preparation method is characterized in that due to the addition of a surface active agent, an intermediate phase B can be rapidly converted into A-phase vanadium dioxide, and an A-phase vanadium dioxide nanowire with excellent morphology and draw ratio is formed; the prepared A-phase vanadium dioxide nanowire is very pure and stable. The preparation method is simple in raw materials, convenient to operate and easy to control; the crystallinity of the product is good; the nanowire can be widely applied to the fields such as batteries, hydrogen storage, photoelectric switches and the like.
Description
Technical field
The invention belongs to material technology field, particularly a kind of preparation method of A phase vanadium dioxide nanowire.
Background technology
The oxide compound kind of vanadium is various, and this tetravalent oxide of vanadium dioxide wherein has a lot of different structures, Rutile Type structure (R), monoclinic phase structure (M), three monoclinic phases (T), and middle phase A and B.The vanadium dioxide of M/R phase is widely studied owing to having metal-insulator phase transition near room temperature (68 ℃), yet that the identical A phase hypovanadic oxide with phase-change characteristic is but studied is very few, and this is mainly the vanadium dioxide preparation difficulty due to A phase.Up to now, only have the method by Hydrothermal Synthesis can obtain A phase hypovanadic oxide, and the vanadium dioxide of A phase is unstable, prepares purer A phase hypovanadic oxide difficulty especially.
The vanadium dioxide of A phase is Th é obald
1when research Hydrothermal Synthesis barium oxide, first find, afterwards Oka
2-5the vanadium dioxide of finding for the first time A phase also has phase-change characteristic, and transformation temperature is near 165 ℃.By a series of experiment, Oka has provided A phase hypovanadic oxide at concrete crystalline structure and the lattice parameter in phase transformation front and back.
The vanadium dioxide of Vanadium Pentoxide in FLAKES and B phase is because having laminate structure can be for the electrode materials of battery, and the VO2 of A phase has laminate structure too, therefore can be used as equally the electrode materials of battery, Dai
6deng people's research, find that the loading capacity first of A phase vanadium dioxide nanowire can reach 277.1mAh/g, the capacity after 50 circles is 116mAh/g, is a kind of very potential battery electrode material.
In addition, the people's such as Zhang research discovery, before and after phase transformation, the vanadium dioxide of A phase has switch feature equally.
Chinese patent literature CN102757094A
8the preparation method that a kind of stable state A phase hypovanadic oxide nanometer rod is provided, comprising: the aqueous solution containing tetravalent vanadium ion is directly added in water heating kettle and carries out hydro-thermal reaction, and in hydrothermal reaction process, the packing ratio of water heating kettle is 50～90%; Heating up and controlling hydrothermal temperature is 180～220 ℃, and hydro-thermal reaction soaking time is 0～720 hour; Hydro-thermal reaction synthetics is cooling, centrifugal, washing, dry make the stable state A phase hypovanadic oxide nanometer rod that length-to-diameter ratio is 1:1～1000:1.The more difficult control of A phase hypovanadic oxide prepared by this method, especially easily produces dephasign (B phase hypovanadic oxide).What from experiment, our discovery obtained when temperature is lower is B phase hypovanadic oxide, and when temperature is higher, will produce M phase hypovanadic oxide, if therefore temperature is controlled bad dephasign B phase hypovanadic oxide or the M phase hypovanadic oxide of just having.
Yet the preparation manipulation of the A phase hypovanadic oxide of report difficulty and wayward, is difficult to obtain ultrapure A phase vanadium dioxide nanowire now.
Summary of the invention
The deficiency existing in order to solve above-mentioned prior art, the invention provides a kind of preparation method of A phase vanadium dioxide nanowire, because phase B in the middle of making adding of tensio-active agent can change A phase hypovanadic oxide fast into, and forming the A phase vanadium dioxide nanowire of pattern, length-to-diameter ratio excellence, prepared A phase vanadium dioxide nanowire is very pure and highly stable.
The raw material that this preparation method adopts is simple, easy to operate, easily controls, and product advantages of good crystallization, gained nano wire can be widely used in the fields such as battery, Chu Qing and optoelectronic switch.
The present invention is achieved through the following technical solutions solved technical problem:
A preparation method for A phase vanadium dioxide nanowire, usings Vanadium Pentoxide in FLAKES as vanadium source, and oxalic acid reflects preparation A phase vanadium dioxide nanowire as reductive agent, wherein, adds polyoxyethylene glycol to participate in reaction as tensio-active agent.
Add after tensio-active agent, can make the temperature range that produces A phase expand, the vanadium dioxide that impels B phase changes to A phase hypovanadic oxide, and the existence of tensio-active agent also can suppress A in opposite directions M change mutually, therefore adding tensio-active agent can be relatively easy to obtain A phase hypovanadic oxide.
Wherein, the weight of Vanadium Pentoxide in FLAKES and oxalic acid is preferably than being 3:2.Adding oxalic acid is mainly as reductive agent, changes pentavalent vanadium into tetravalence vanadium.
Add the consumption of polyoxyethylene glycol preferred: Vanadium Pentoxide in FLAKES and the ratio of oxalic acid gross weight (g) and polyoxyethylene glycol weight (g) be 5:1, or Vanadium Pentoxide in FLAKES and oxalic acid gross weight (g) be 5:1 with the ratio of polyoxyethylene glycol volume (mL).
Before reaction by above-mentioned vanadium source, reductive agent and surfactant-dispersed in 20ml ultrapure water solution, vigorous stirring 15-20 minute at 60 ℃ of-80 ℃ of temperature, the preferred 300rpm(rev/min of stirring velocity), obtain solution.
Wherein, the polyoxyethylene glycol that the present invention's tensio-active agent used is different molecular weight, comprises poly(oxyethylene glycol) 400, Polyethylene Glycol-600, Macrogol 2000, Macrogol 4000 and polyethylene glycol 6000.The polyoxyethylene glycol of different molecular weight has very large impact to the length-to-diameter ratio of last nano wire, and wherein best is polyethylene glycol 6000.
Above-mentioned solution is joined in tetrafluoroethylene water heating kettle, be warming up to 200 ℃-240 ℃, 2.5 ℃/min of temperature rise rate, insulation 24-60h, is finally down to after room temperature naturally, centrifugation after ultrapure water and alcohol cleaning, be dried, obtain the vanadium dioxide nanowire of A phase.
Wherein, the volume ratio of ultrapure water and alcohol is preferably 5:1, has good cleaning and refining effect.
The present invention obtains the length of A phase vanadium dioxide nanowire at 1-30 μ m, and diameter is at 20-500nm, and length-to-diameter ratio is 20:1-50:1.The A phase hypovanadic oxide obtaining is to belong to tetragonal system, can find out that what obtain is very pure A phase hypovanadic oxide from XRD and DSC collection of illustrative plates.Therefore, the advantage of this method maximum is exactly to obtain easily the A phase hypovanadic oxide that purity is very high.
Compared to existing technology, the invention has the advantages that:
1, the present invention adopts Vanadium Pentoxide in FLAKES as vanadium source, and oxalic acid is as reductive agent, and polyoxyethylene glycol is as tensio-active agent, and raw material is simple.
2, the present invention adopts polyoxyethylene glycol as tensio-active agent, can at lower temperature, synthesize A phase vanadium dioxide nanowire, and the A phase vanadium dioxide nanowire obtaining is highly stable, very high purity.
3, the present invention uses the method for Hydrothermal Synthesis, synthetic method is simple to operation, temperature of reaction low (200 ℃-240 ℃) while adopting polyoxyethylene glycol as tensio-active agent Hydrothermal Synthesis, reaction times short (24-60h), and after interpolation tensio-active agent, can impel B phase hypovanadic oxide to change to A phase hypovanadic oxide, make to react the pure A phase hypovanadic oxide that obtains more easy to control, substantially do not contain dephasign B phase hypovanadic oxide and/or M phase hypovanadic oxide.
4, preparation method of the present invention is easy and simple to handle, cost is low, easily control, product good crystallinity, yield are high, be applicable to scale production and also make state A phase vanadium dioxide nanowire, stable crystal form, there is good ductility, mechanical property and workability, can be widely used in the fields such as battery, catalysis, Chu Qing.
Accompanying drawing explanation
Fig. 1, the XRD figure spectrum of the vanadium dioxide nanowire of gained A phase of the present invention.
The SEM pattern picture of the vanadium dioxide nanowire of Fig. 2, gained A phase of the present invention.
Fig. 3, the SEM pattern picture of the vanadium dioxide nanowire of gained A phase of the present invention.
Fig. 4, the DSC transformation curve figure of the vanadium dioxide nanowire of gained A phase of the present invention.
Fig. 5, the IR figure of the vanadium dioxide nanowire of gained A phase of the present invention.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described:
Accurately weigh 0.3g Vanadium Pentoxide in FLAKES, 0.2g oxalic acid and 0.1mL poly(oxyethylene glycol) 400 and be scattered in 20mL ultrapure water solution, at 60 ℃ of temperature, vigorous stirring is 15 minutes, stirring velocity 300rpm.Above-mentioned solution is joined in 25mL tetrafluoroethylene water heating kettle, packing ratio is 80%, be warming up to 240 ℃, temperature rise rate is 2.5 ℃/min, insulation 60h, finally is down to after room temperature naturally, centrifugation after the ultrapure water of 1L and the cleaning of 200ml alcohol, in baking oven, 80 ℃ are dried 8 hours, obtain the vanadium dioxide nanowire of A phase.If Fig. 1 is the XRD figure spectrum recording, Fig. 2 is SEM pattern picture, can find out that its length is at 1-6 μ m, and diameter is at 20-300nm, and length-to-diameter ratio is 20:1-50:1.
Embodiment 2
Accurately weigh 0.3g Vanadium Pentoxide in FLAKES, 0.2g oxalic acid and 0.1mL Polyethylene Glycol-600 and be scattered in 20mL ultrapure water solution, at 60 ℃ of temperature, vigorous stirring is 15 minutes, stirring velocity 300rpm.Above-mentioned solution is joined in 25mL tetrafluoroethylene water heating kettle, packing ratio is 80%, is warming up to 230 ℃, and temperature rise rate is 2.5 ℃/min, insulation 50h, finally naturally be down to after room temperature, centrifugation after the ultrapure water of 1L and 200ml alcohol clean, in baking oven 80 ℃ dry 8 hours, obtain the vanadium dioxide nanowire of A phase, record its length at 1-10 μ m, diameter is at 20-400nm, and length-to-diameter ratio is 25:1-50:1.
Embodiment 3
Accurately weigh 0.3g Vanadium Pentoxide in FLAKES, 0.2g oxalic acid and 0.1g Macrogol 2000 and be scattered in 20mL ultrapure water solution, at 60 ℃ of temperature, vigorous stirring is 15 minutes, stirring velocity 300rpm.Above-mentioned solution is joined in 25mL tetrafluoroethylene water heating kettle, packing ratio is 80%, be warming up to 225 ℃, temperature rise rate is 2.5 ℃/min, insulation 48h, finally is down to after room temperature naturally, centrifugation after the ultrapure water of a large amount of 1L and the cleaning of 200ml alcohol, in baking oven, 80 ℃ are dried 8 hours, obtain the vanadium dioxide nanowire of A phase.If Fig. 3 is the SEM pattern picture recording, its length is at 5-30 μ m, and diameter is at 50-500nm, and length-to-diameter ratio is 100:1-20:1.
Embodiment 4
Accurately weigh 0.3g Vanadium Pentoxide in FLAKES, 0.2g oxalic acid and 0.1g Macrogol 4000 and be scattered in 20mL ultrapure water solution, at 60 ℃ of temperature, vigorous stirring is 15 minutes, stirring velocity 300rpm.Above-mentioned solution is joined in 25mL tetrafluoroethylene water heating kettle, packing ratio is 80%, be warming up to 215 ℃, temperature rise rate is 2.5 ℃/min, insulation 48h, finally is down to after room temperature naturally, centrifugation after the ultrapure water of 1L and the cleaning of 200ml alcohol, in baking oven, 80 ℃ are dried 8 hours, obtain the vanadium dioxide nanowire of A phase.Record its length at 10-20 μ m, diameter is at 50-200nm, and length-to-diameter ratio is 100:1-200:1.If Fig. 4 is the DSC transformation curve recording, the transformation temperature when heating up is 165.1 ℃, during cooling 118 ℃.
Embodiment 5
Accurately weigh 0.3g Vanadium Pentoxide in FLAKES, 0.2g oxalic acid and 0.1g polyethylene glycol 6000 and be scattered in 20mL ultrapure water solution, at 60 ℃ of temperature, vigorous stirring is 15 minutes, stirring velocity 300rpm.Above-mentioned solution is joined in 25mL tetrafluoroethylene water heating kettle, packing ratio is 80%, be warming up to 210 ℃, temperature rise rate is 2.5 ℃/min, insulation 48h, finally is down to after room temperature naturally, centrifugation after the ultrapure water of 1L and the cleaning of 200ml alcohol, in baking oven, 80 ℃ are dried 8 hours, obtain the vanadium dioxide nanowire of A phase.Record its length at 20-60 μ m, diameter is at 10-600nm, and length-to-diameter ratio is 100:1-2000:1.If Fig. 5 is the IR collection of illustrative plates recording, as can be seen from the figure before and after phase transformation, phase transmitance has obvious change.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Background technology reference:
1.Théobald,F.Journal?of?the?Less?Common?Metals1977,53,(1),55-71.
2.OKA,Y.;OHTANI,T.;YAMAMOTO,N.;TAKADA,T.Journal?of?the?Ceramic?Society?of?Japan1989,97,(1130),1134-1137.
3.Oka,Y.;Yao,T.;Yamamoto,N.Journal?of?Materials?Chemistry1991,1,(5),815-818.
4.Yao,T.;Oka,Y.;Yamamoto,N.Journal?of?Solid?State?Chemistry1994,112,(1),196-198.
5.Oka,Y.;Sato,S.;Yao,T.;Yamamoto,N.Journal?of?Solid?State?Chemistry1998,141,(2),594-598.
6.Dai,L.;Gao,Y.;Cao,C.;Chen,Z.;Luo,H.;Kanehira,M.;Jin,J.;Liu,Y.RSC?Advances2012,2,(12),5265-5270.
7.Yifu,Z.;Meijuan,F.;Fei,N.;Yalan,Z.;Chi,H.;Xinghai,L.;Baojun,W.;Houbin,L.Micro?&?Nano?Letters,IET2011,6,(11),888-891.
8.CN102757094A
Claims (10)
1. a preparation method for A phase vanadium dioxide nanowire, is characterized in that, usings Vanadium Pentoxide in FLAKES as vanadium source, and oxalic acid reflects preparation A phase vanadium dioxide nanowire as reductive agent, wherein, adds polyoxyethylene glycol to participate in reaction as tensio-active agent.
2. preparation method according to claim 1, it is characterized in that, the consumption of polyoxyethylene glycol is: Vanadium Pentoxide in FLAKES and the ratio of oxalic acid gross weight (g) and polyoxyethylene glycol weight (g) be 5:1, or Vanadium Pentoxide in FLAKES and oxalic acid gross weight (g) be 5:1 with the ratio of polyoxyethylene glycol volume (mL).
3. preparation method according to claim 1, is characterized in that, described polyoxyethylene glycol comprises poly(oxyethylene glycol) 400, Polyethylene Glycol-600, Macrogol 2000, Macrogol 4000 and polyethylene glycol 6000.
4. preparation method according to claim 2, is characterized in that, described polyoxyethylene glycol comprises poly(oxyethylene glycol) 400, Polyethylene Glycol-600, Macrogol 2000, Macrogol 4000 and polyethylene glycol 6000.
5. according to the preparation method described in the arbitrary claim of claim 1-4, it is characterized in that, the weight ratio of Vanadium Pentoxide in FLAKES and oxalic acid is 3:2.
6. according to the preparation method described in the arbitrary claim of claim 1-4, it is characterized in that, before reaction by above-mentioned vanadium source, reductive agent and surfactant-dispersed in 20ml ultrapure water solution, vigorous stirring 15-20 minute at 60 ℃ of-80 ℃ of temperature, stirring velocity is 300rpm, obtains solution.
7. preparation method according to claim 5, it is characterized in that, before reaction by above-mentioned vanadium source, reductive agent and surfactant-dispersed in 20ml ultrapure water solution, vigorous stirring 15-20 minute at 60 ℃ of-80 ℃ of temperature, stirring velocity is 300rpm, obtains solution.
8. preparation method according to claim 6, it is characterized in that, described solution is joined in tetrafluoroethylene water heating kettle, be warming up to 200 ℃-240 ℃, 2.5 ℃/min of temperature rise rate, insulation 24-60h, finally naturally be down to after room temperature, centrifugation after ultrapure water and alcohol cleaning, is dried, and obtains the vanadium dioxide nanowire of A phase.
9. preparation method according to claim 7, it is characterized in that, described solution is joined in tetrafluoroethylene water heating kettle, be warming up to 200 ℃-240 ℃, 2.5 ℃/min of temperature rise rate, insulation 24-60h, finally naturally be down to after room temperature, centrifugation after ultrapure water and alcohol cleaning, is dried, and obtains the vanadium dioxide nanowire of A phase.
10. the preparation method described according to Claim 8 or 9 arbitrary claims, is characterized in that, the volume ratio of ultrapure water and alcohol is 5:1, and the length of gained vanadium dioxide nanowire is at 1-30 μ m, and diameter is at 20-500nm, and length-to-diameter ratio is 20:1-50:1.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104192904A (en) * | 2014-08-29 | 2014-12-10 | 武汉科技大学 | Superlong vanadium dioxide nanowire film and preparation method thereof |
| 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 |
| CN105449102A (en) * | 2015-12-04 | 2016-03-30 | 中山大学 | A-phase vanadium dioxide nanowire-based temperature control switch and fabrication method thereof |
| CN106082337A (en) * | 2016-06-08 | 2016-11-09 | 中国科学院合肥物质科学研究院 | VO2(M) nanometer line ordered array and preparation method thereof |
| CN106395901A (en) * | 2016-10-20 | 2017-02-15 | 中国人民解放军国防科学技术大学 | Monoclinic phase vanadium dioxide nanowire and preparation method and application thereof |
| CN108217727A (en) * | 2018-04-12 | 2018-06-29 | 四川星明能源环保科技有限公司 | A phase hypovanadic oxides and preparation method thereof |
| CN108892171A (en) * | 2018-07-11 | 2018-11-27 | 首都师范大学 | A kind of thermodynamics restoring method synthesizing vanadium oxide nano material |
| CN110137486A (en) * | 2019-05-21 | 2019-08-16 | 南京工业大学 | A kind of preparation method of the transition metal oxide nano-material synthesized from top to bottom |
| CN112397707A (en) * | 2020-11-13 | 2021-02-23 | 何叶红 | Porous VO for lithium ion battery2Microspheres and method for preparing same |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104192904A (en) * | 2014-08-29 | 2014-12-10 | 武汉科技大学 | Superlong vanadium dioxide nanowire film and preparation method thereof |
| 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 |
| CN105449102A (en) * | 2015-12-04 | 2016-03-30 | 中山大学 | A-phase vanadium dioxide nanowire-based temperature control switch and fabrication method thereof |
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| CN106395901A (en) * | 2016-10-20 | 2017-02-15 | 中国人民解放军国防科学技术大学 | Monoclinic phase vanadium dioxide nanowire and preparation method and application thereof |
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| CN108892171A (en) * | 2018-07-11 | 2018-11-27 | 首都师范大学 | A kind of thermodynamics restoring method synthesizing vanadium oxide nano material |
| CN110137486A (en) * | 2019-05-21 | 2019-08-16 | 南京工业大学 | A kind of preparation method of the transition metal oxide nano-material synthesized from top to bottom |
| CN112397707A (en) * | 2020-11-13 | 2021-02-23 | 何叶红 | Porous VO for lithium ion battery2Microspheres and method for preparing same |
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