CN101955752B - Vanadium dioxide (VO2) phase change material with beam-shaped nanostructure and preparation method thereof - Google Patents

Vanadium dioxide (VO2) phase change material with beam-shaped nanostructure and preparation method thereof Download PDF

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CN101955752B
CN101955752B CN 201010507800 CN201010507800A CN101955752B CN 101955752 B CN101955752 B CN 101955752B CN 201010507800 CN201010507800 CN 201010507800 CN 201010507800 A CN201010507800 A CN 201010507800A CN 101955752 B CN101955752 B CN 101955752B
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phase change
change material
nanostructure
pencil
preparation
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CN101955752A (en
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尹海宏
郁可
张正犁
汪阳
娄蕾
曾敏
朱自强
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East China Normal University
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Abstract

The invention discloses a vanadium dioxide (VO2) phase change material with a beam-shaped nanostructure. The VO2 phase change material with the beam-shaped nanostructure is characterized in that: the length is 18 to 25 mu m and the diameter is 3 to 5 mu m, wherein a nanobeam crystal is formed through the oriented polymerization of VO2 nanowires with the diameter of 10 to 30 nm. The generated VO2 crystal has a special beam-shaped nanostructure with uniform thickness and consistent length and has phase change property. The invention also discloses a preparation method of the VO2 phase change material with the beam-shaped nanostructure. The VO2 phase change material with the beam-shaped nanostructure and the preparation method thereof have the advantages of low cost, simple growth condition, high repeatability, few impurities and the like and have wide application prospects in the fields of nano photoelectron and intelligent temperature-control energy conservation.

Description

A kind of VO with pencil nanostructure 2Phase change material and preparation method thereof
Technical field
The present invention relates to semiconductor material, photoelectron material, phase change material and device technology field, be specifically related to a kind of VO with pencil nanostructure 2Phase change material and preparation method thereof.
Background technology
The VO of monoclinic structure 2Be a kind of thermal induced phase transition type material, when temperature is lower than 68 ℃, VO 2Be in the semi-conductor attitude, be monoclinic structure; When temperature is higher than 68 ℃, VO 2Change metallic state into, have cubic rutile structure, and phase transformation is very fast.Be accompanied by the variation of crystallographic system structure, resistivity, susceptibility, optical transmittance and reflectivity all produce sudden change.These character make VO 2Become a kind of photoelectric conversion material that has wide application prospects, optical storage, laser radiation and smart window material.
Recently, people utilize the whole bag of tricks (solution method, molecular beam epitaxy, pulsed laser deposition, metal-organic chemical vapor deposition equipment etc.) to prepare various one dimension VO 2Nanostructure, for example nano wire, nano belt, nanometer rod etc., and the photoelectric characteristic of these nanostructures studied, but the arrangement of these nano wires, nano belt, nanometer rod is often disorderly and unsystematic, and this randomness is VO 2On the subsequent disposal in the application of nano photoelectric son and intelligent temperature control type devices field, brought very big trouble, and in the past the preparation method can be applied to scale operation method seldom, severe reaction conditions, production cost is high.
The present invention overcomes the above defective of prior art, and a kind of VO with pencil nanostructure is provided 2Phase change material and preparation method thereof, the present invention is easy and simple to handle, and cost is low, high duplication, and the VO that obtains 2The nanometer bundle even thickness, length is consistent, applicable to large-scale industrial production.
Summary of the invention
One of the object of the invention is to provide a kind of VO with pencil nanostructure 2Phase change material, its length is generally 18-25
Figure 202847DEST_PATH_IMAGE001
, diameter is 3-5
Figure 182304DEST_PATH_IMAGE001
, wherein, said nanometer bundle crystal is the VO of 10-30nm by diameter 2The nano wire tactic polymerization is formed.
Figure 962041DEST_PATH_IMAGE003
Another object of the present invention is to be to provide the VO with pencil nanostructure 2The preparation method of phase change material; Promptly be employed in oxalic acid and the propyl carbinol mixed aqueous solution and add vanadium pentoxide powder; Place the autoclave reaction of sealing to obtain black powder, again with black powder through after nitrogen and 500 ℃ of-700 ℃ of environment are calcined down, obtain by VO 2The VO of the pencil nanostructure that the nano wire tactic polymerization forms 2Phase change material.The present invention can solve existing VO 2The arrangement of monodimension nanometer material is unordered, and the problem that preparing method's condition is harsh, cost is high, a kind of low cost, high duplication is provided, is applicable to the novel method of large-scale commercial prodn.
The present invention has the VO of pencil nanostructure 2The preparation method of phase change material comprises that concrete steps are following:
A, configuration reaction soln: the oxalic acid crystal is soluble in water, add propyl carbinol again, add vanadium pentoxide powder then, be stirred to dissolving fully;
B, pour above-mentioned solution into autoclave,, under 240~300 ℃ of temperature, keep reaction 36~72 hours, naturally after the cooling, filter, cleaning obtains black powder shape material putting into air dry oven behind the autoclave good seal;
C, under nitrogen atmosphere, the black powder shape material that obtains under 500 ℃ of-700 ℃ of temperature, was calcined 30-60 minute, promptly make VO with pencil nanostructure 2Phase change material.
The above reaction of the present invention is in the autoclave of sealing, to carry out.
The present invention proposes a kind of VO with pencil nanostructure first 2Phase change material.The present invention has advantages such as cost is low, and growth conditions is simple, and repeatability is high, and impurity is few, and the VO that generates 2Crystal has special pencil nanostructure, has phase-change characteristic.The present invention has the VO of pencil nanostructure 2Nano material is by VO 2Nano wire tactic polymerization bunchy, the diameter of nano wire is even, and the direction height is consistent, can be from now on to design, prepare phase transformation intelligent temperature control type energy saving device and offer convenience, and has broad application prospects in sub-field of nano photoelectric and intelligent temperature control energy-saving field.
With respect to prior art, VO of the present invention 2The beneficial effect of nano material and preparation method thereof comprises: the present invention has proposed nano wire tactic polymerization fasciculation VO first 2Nano material, pattern is novel; And synthetic VO in the prior art 2Mostly nanostructure is single nano wire, nanometer rod and so on, and arranges disorderly and unsystematic; Preparing method's equipment used of the present invention is simple, and common laboratory equipment can both reach requirement; Do not need the very operation of difficulty, operation steps is simple; Do not need catalyzer, save resource; Cost is low, and good reproducibility goes for preparation in enormous quantities.
Description of drawings
Fig. 1 is the X-ray diffractogram that the present invention has the pencil nanostructure;
Fig. 2 is VO of the present invention 2The SEM figure of phase change material;
Fig. 3 is VO of the present invention 2The high power SEM figure of phase change material;
Fig. 4 is VO of the present invention 2The TEM figure of phase change material;
Fig. 5 is VO of the present invention 2The TEM figure of the single nano-wire of phase change material.
Embodiment
Following examples are used for specifically setting forth the present invention, but the present invention is not limited to following examples.All equivalences of doing according to the content of patented claim of the present invention change and modify, and all should belong to the category of the present invention's protection.
Embodiment 1:
The preparation pencil VO of present embodiment 2The phase change material of nanostructure, concrete steps are following:
A, configuration reaction soln: .5g is soluble in water with the oxalic acid crystal 2, adds propyl carbinol 8mL, adds vanadium pentoxide powder 1.5g again, is stirred to dissolving fully;
B, pour above-mentioned solution into autoclave,, under 260 ℃ of temperature, keep reaction 48 hours, naturally after the cooling, filter, cleaning obtains black powder shape material putting into air dry oven behind the autoclave good seal;
C, under nitrogen atmosphere, the black powder shape material that obtains under 550 ℃ of temperature, was calcined 60 minutes, promptly make VO with pencil nanostructure 2Phase change material.
The VO of the pencil nanostructure that present embodiment prepares 2Phase change material, its X-ray diffractogram is as shown in Figure 1.Detect through sem, its SEM figure is as shown in Figure 2, and high power SEM figure is as shown in Figure 3, and high power TEM figure is as shown in Figure 4, and the TEM figure of the single nano-wire in the pencil nanostructure is as shown in Figure 5.
Figure 422497DEST_PATH_IMAGE004

Claims (3)

1. VO with pencil nanostructure 2Phase change material is characterized in that, its length is 18-25 μ m, and diameter is 3-5 μ m, and wherein, the nanometer bundle crystal is the VO of 10-30nm by diameter 2The nano wire tactic polymerization is formed.
2. the VO that has the pencil nanostructure according to claim 1 2Phase change material is characterized in that, said VO 2Nanometer bundle crystal even thickness, length is consistent, is monoclinic structure, is in the semi-conductor attitude, and its structure space crowd is P21/C, a=5.7529, b=4.5263, c=5.3825, β=122.68 °.
3. the VO that has the pencil nanostructure according to claim 1 2The preparation technology of phase change material is characterized in that, comprises that step is following:
A, configuration reaction soln: .5g is soluble in water with the oxalic acid crystal 2, adds propyl carbinol 8mL, adds vanadium pentoxide powder 1.5g again, is stirred to dissolving fully;
B, pour above-mentioned solution into autoclave,, under 260 ℃ of temperature, keep reaction 48 hours, naturally after the cooling, filter, cleaning obtains black powder shape material putting into air dry oven behind the autoclave good seal;
C, under nitrogen atmosphere, resultant black powder shape material under 550 ℃ of temperature, was calcined 60 minutes, promptly make said VO with pencil nanostructure 2Phase change material.
CN 201010507800 2010-10-15 2010-10-15 Vanadium dioxide (VO2) phase change material with beam-shaped nanostructure and preparation method thereof Expired - Fee Related CN101955752B (en)

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CN102583536A (en) * 2012-02-02 2012-07-18 南通大学 Vanadium pentoxide (V2O5) material with large specific surface area and preparation method thereof
US20160257823A1 (en) 2015-03-06 2016-09-08 Konica Minolta Laboratory U.S.A., Inc. Stable thermochromic polymer films with vanadium dioxide nanowires
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

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CN1522965A (en) * 2003-09-12 2004-08-25 武汉理工大学 Vanadium dioxide nanometer rod and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1522965A (en) * 2003-09-12 2004-08-25 武汉理工大学 Vanadium dioxide nanometer rod and preparation method thereof

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