CN106082337A - VO2(M) nanometer line ordered array and preparation method thereof - Google Patents
VO2(M) nanometer line ordered array and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of VO2(M) nanometer line ordered array and preparation method thereof.Oldered array is VO2(M) nano wire becomes array along its line length direction ordered arrangement, wherein, forms VO2(M) VO of nanometer line ordered array2(M) linear diameter of nano wire be 200～600nm, line length be 10～50 μm；Method first uses hydro-thermal method to obtain VO2(A) nano wire, then by VO2(A) nano wire and water are ultrasonic after mixing, and obtain VO2(A) nanowire dispersion, afterwards, first by VO2(A) nanowire dispersion is added dropwise in chloroform, treats VO2(A) nano wire is after chloroform surface self-organization becomes oldered array, uses substrate to be picked up, obtains being covered with on it VO2(A) substrate of nanometer line ordered array, then VO will be covered with on it2(A) after the substrate of nanometer line ordered array is placed in vacuum or protective atmosphere annealing, separate substrate, prepare purpose product.It is extremely easy to widely commercial applications in fields such as photodetection, intelligent response, electro-catalysis, sensor and magnetic component.
Description
Technical field
The present invention relates to a kind of oldered array and preparation method, especially a kind of VO2(M) (M phase hypovanadic oxide) nano wire
Oldered array and preparation method thereof.
Background technology
Vanadium dioxide is the not special phase-change material of one, when the condition such as temperature or pressure changes, and can be from insulator phase or half
Conductor phase in version is to metal phase, and meanwhile, its resistivity, light refractive index, magnetic susceptibility, reflectivity etc. also have change.Titanium dioxide
Vanadium crystal has different phases, such as VO2(A)、VO2(B)、VO2(C)、VO2(D)、VO2And VO (M)2(R) etc., wherein, VO2(M)
Phase transition temperature is closest to room temperature (68 DEG C).At present, in terms of vanadium dioxide photodetection, the single vanadium dioxide of document report
Though nano wire has more excellent photodetection performance, but because its photocurrent values is less, and device cannot be prepared as and be difficult to
It is on the actual application.For solving this problem, people have made some good tries and effort, such as entitled " Orientated
Langmuir-Blodgett Assembly of VO2Nanowires ", Nano Lett., Vol.9, No.2,2009, (" LB method
NW-TFT vanadium dioxide nanowire ", " nanometer bulletin " the 2nd phase of volume 9 in 2009) article.The titanium dioxide mentioned in this article
Vanadium nano wire is the VO of line footpath 200～500nm2(B) nano wire；First by V during preparation2O5Join with cetyl trimethylammonium bromide
After making precursor solution, obtain VO by hydro-thermal method2(B) nano wire, then use stearic acid, hexamethylene and cetyl three respectively
Methyl bromide ammoniums etc. are to VO2(B), after the surface of nano wire is modified, use LB film machine to assemble it, obtain product.But
It is, either product, or its preparation method, all there is weak point, first, VO2(B) not having phase-change characteristic, it should
With prospect difficult with phase transition temperature close to the VO of room temperature2(M) mention in the same breath；Secondly, the length of nano wire is substantially all less than 5 μ
M, and its only in very little scope along certain orientation arrangement, the nano wire under overall 5 μm of scales be still present miscellaneous
The disorderly disordered state of distribution；Again, during preparing product, kinds of surface dressing agent and activating agent are employed, these residuals
The actual application of product will be had adverse effect on by the coating material on product and activating agent；Finally, preparation method
VO can not be obtained2(M) nanometer line ordered array, also has the defect that technique is loaded down with trivial details, cost is high.
Content of the invention
The technical problem to be solved in the present invention, for overcoming weak point of the prior art, provides a kind of nanometer line length relatively
Long and become array along its line length direction ordered arrangement VO2(M) nanometer line ordered array.
Another technical problem that the invention solves the problems that is for providing a kind of above-mentioned VO2(M) preparation of nanometer line ordered array
Method.
For solving the technical problem of the present invention, the technical scheme being used is: VO2(M) nanometer line ordered array is by VO2(M)
Composition, particularly,
Described VO2(M) pattern is nanometer line ordered array, and described nanometer line ordered array is that nano wire is along its line length side
Become array to ordered arrangement；
Described composition VO2(M) VO of nanometer line ordered array2(M) linear diameter of nano wire is that 200～600nm, line length are
10～50 μm.
For solving another technical problem of the present invention, another technical scheme being used is: above-mentioned VO2(M) nanometer
The preparation method of line oldered array includes hydro-thermal method, and particularly key step is as follows:
Step 1, first uses hydro-thermal method to obtain VO2(A) nano wire, then by VO2(A) nano wire and water are 1 according to weight ratio:
After the ratio mixing of 800～1200, ultrasonic at least 10min, obtain VO2(A) nanowire dispersion；
Step 2, first according to VO2(A) the weight ratio of nanowire dispersion and chloroform is 1: the ratio of >=0.8, by VO2(A) receive
Rice noodles dispersant liquid drop adds in chloroform, treats VO2(A) nano wire is after chloroform surface self-organization becomes oldered array, and use substrate will
It picks up, and obtains being covered with on it VO2(A) substrate of nanometer line ordered array, then VO will be covered with on it2(A) nanometer line ordered array
Substrate be placed in vacuum or protective atmosphere, after at least 60min that anneals at 480～550 DEG C, separate substrate, prepare VO2
(M) nanometer line ordered array.
As VO2(M) improvement further of the preparation method of nanometer line ordered array:
Preferably, hydro-thermal method obtains VO2(A) process of nano wire is, first by vanadium pentoxide powder, oxalic acid and water according to
Weight stirs at least 1h after mixing than the ratio for 0.2～0.4:0.4～0.6:50, obtains precursor solution, then by precursor
Solution is placed in air-tight state, after reacting at least 50h, carries out solid-liquid to chilled reactant liquor successively and divides at 200～240 DEG C
From, washing and be dried process.
Preferably, by VO2(A) for along chamber wall dropping when nanowire dispersion is added dropwise in chloroform.
Preferably, substrate is conductor, or semiconductor, or insulator.
Preferably, protective atmosphere is nitrogen atmosphere, or argon gas atmosphere, or helium atmosphere, or neon atmosphere.
Preferably, separating substrate is physical separation.
Preferably, separation of solid and liquid is processed as centrifugation, and its rotating speed is 8000～12000r/min, time is 5～
15min。
Preferably, carrying out washing treatment for use deionized water and the solid to isolated for the ethanol carry out 2～3 times alternately
Cleaning, separating solid during cleaning is centrifugation.
Preferably, it is dried the solid being processed as after cleaning and be placed at 40～80 DEG C baking 10～14h.
Provide the benefit that relative to prior art:
One, uses ESEM, X-ray diffractometer and semi-conductor test instrument to carry out table prepared purpose product respectively
Levying, from its result, purpose product is by VO2(M) forming, its pattern is nanometer line ordered array；Wherein, nano thread ordered battle array
Being classified as nano wire and becoming array along its line length direction ordered arrangement, the linear diameter of nano wire therein is that 200～600nm, line length are
10～50 μm.This by VO2(M) the purpose product that set of nanowires is dressed up, both due to VO2(M) phase transition temperature is closest to room
Temperature, again because the line footpath of its nano wire is nano-scale, due also to line length >=10 μm of nano wire, more because nano wire is along its line length side
Having become array to ordered arrangement, particularly its phase transition temperature is closest to room temperature, so that its performance is improved.Test shows mesh
The photocurrent values of product be greatly improved.
Its two, preparation method is simple, science, efficiently.Not only prepare nanometer line length longer and along its line length direction height
Ordered arrangement becomes the purpose product VO of array2(M) nanometer line ordered array；Also make it both will not be subject in actual applications
Coating material and the interference of activating agent, unrestricted as desired can prepare large-area purpose product again；More there is work
Skill is easy, the feature of low cost；And then make purpose product be extremely easy to widely commercial applications in photodetection, intelligent response,
The fields such as electro-catalysis, sensor and magnetic component.
Brief description
Fig. 1 is to the VO using hydro-thermal method to obtain2(A) nano wire and VO2(A) nanometer line ordered array uses respectively and sweeps
Retouch Electronic Speculum (SEM) and one of result that X-ray diffraction (XRD) instrument characterizes.Wherein, Fig. 1 a is for using hydro-thermal method to obtain
VO2(A) SEM image of nano wire；Fig. 1 b is VO2(A) SEM image of nanometer line ordered array；Fig. 1 c is Fig. 1 a and shown in Fig. 1 b
The XRD spectra of nanometer line ordered array, it shows that nanometer line ordered array is VO2(A) nanometer line ordered array.
Fig. 2 is that the purpose product preparing preparation method uses ESEM and X-ray diffractometer to characterize respectively
One of result.Wherein, the SEM image of product for the purpose of Fig. 2 a, the XRD spectra of product for the purpose of Fig. 2 b；Be can be seen that by it, purpose
Product is VO2(M) nanometer line ordered array.
Fig. 3 is to one of result that prepared purpose product use semi-conductor test instrument characterizes.Its result confirms
The photocurrent values of purpose product is greatly improved relative to single nano-wire.
Detailed description of the invention
Below in conjunction with the accompanying drawings the preferred embodiment of the present invention is described in further detail.
First buy from market or prepare voluntarily:
VO2(A) nano wire；Chloroform；As the conductor of substrate, semiconductor and insulator；As protective atmosphere nitrogen,
Argon gas, helium and neon.Wherein,
Hydro-thermal method obtains VO2(A) process of nano wire is, first by vanadium pentoxide powder, oxalic acid and water according to weight ratio
Stir at least 1h after the ratio mixing being 0.2～0.4:0.4～0.6:50, obtain precursor solution, then precursor solution is put
In air-tight state, after reacting at least 50h at 200～240 DEG C, carry out separation of solid and liquid, washing successively to chilled reactant liquor
With the process being dried；Separation of solid and liquid therein is processed as centrifugation, and its rotating speed is 8000～12000r/min, time is 5～
15min, the alternately cleaning that carrying out washing treatment carries out 2～3 times for using deionized water and the solid to isolated for the ethanol, clean
When separate solid be centrifugation, be dried be processed as will clean after solid be placed at 40～80 DEG C baking 10～14h.
Then,
Embodiment 1
Concretely comprising the following steps of preparation:
Step 1, first uses hydro-thermal method to obtain VO2(A) nano wire.Again by VO2(A) nano wire and water are 1 according to weight ratio:
After the ratio mixing of 800, ultrasonic 20min, obtain VO2(A) nanowire dispersion.
Step 2, first according to VO2(A) weight of nanowire dispersion and chloroform is than the ratio for 1:0.8, by VO2(A) nanometer
Line dispersion liquid is added dropwise in chloroform along chamber wall, treats VO2(A) nano wire is after chloroform surface self-organization becomes oldered array, uses
Substrate is picked up, and obtains being covered with on it VO2(A) substrate of nanometer line ordered array；Wherein, substrate is insulator.Again by it
On be covered with VO2(A) substrate of nanometer line ordered array is placed in protective atmosphere (or vacuum), and anneal at 480 DEG C 100min
After, physical separation substrate；Wherein, protective atmosphere is nitrogen atmosphere.Prepare and be similar to shown in Fig. 2 a, and such as Fig. 2 b and Fig. 3
In the VO shown in curve2(M) nanometer line ordered array.
Embodiment 2
Concretely comprising the following steps of preparation:
Step 1, first uses hydro-thermal method to obtain VO2(A) nano wire.Again by VO2(A) nano wire and water are 1 according to weight ratio:
After the ratio mixing of 900, ultrasonic 18min, obtain VO2(A) nanowire dispersion.
Step 2, first according to VO2(A) weight of nanowire dispersion and chloroform is than the ratio for 1:3, by VO2(A) nano wire
Dispersion liquid is added dropwise in chloroform along chamber wall, treats VO2(A) nano wire is after chloroform surface self-organization becomes oldered array, uses lining
The end, is picked up, and obtains being covered with on it VO2(A) substrate of nanometer line ordered array；Wherein, substrate is insulator.Again by it
It is covered with VO2(A) substrate of nanometer line ordered array is placed in protective atmosphere (or vacuum), after the 90min that anneals at 498 DEG C,
Physical separation substrate；Wherein, protective atmosphere is nitrogen atmosphere.Prepare and be similar to shown in Fig. 2 a, and as in Fig. 2 b and Fig. 3
VO shown in curve2(M) nanometer line ordered array.
Embodiment 3
Concretely comprising the following steps of preparation:
Step 1, first uses hydro-thermal method to obtain VO2(A) nano wire.Again by VO2(A) nano wire and water are 1 according to weight ratio:
After the ratio mixing of 1000, ultrasonic 15min, obtain VO2(A) nanowire dispersion.
Step 2, first according to VO2(A) weight of nanowire dispersion and chloroform is than the ratio for 1:6, by VO2(A) nano wire
Dispersion liquid is added dropwise in chloroform along chamber wall, treats VO2(A) nano wire is after chloroform surface self-organization becomes oldered array, uses lining
The end, is picked up, and obtains being covered with on it VO2(A) substrate of nanometer line ordered array；Wherein, substrate is insulator.Again by it
It is covered with VO2(A) substrate of nanometer line ordered array is placed in protective atmosphere (or vacuum), after the 80min that anneals at 515 DEG C,
Physical separation substrate；Wherein, protective atmosphere is nitrogen atmosphere.Prepare as shown in Figure 2 a, and such as the curve in Fig. 2 b and Fig. 3
Shown VO2(M) nanometer line ordered array.
Embodiment 4
Concretely comprising the following steps of preparation:
Step 1, first uses hydro-thermal method to obtain VO2(A) nano wire.Again by VO2(A) nano wire and water are 1 according to weight ratio:
After the ratio mixing of 1100, ultrasonic 13min, obtain VO2(A) nanowire dispersion.
Step 2, first according to VO2(A) weight of nanowire dispersion and chloroform is than the ratio for 1:8, by VO2(A) nano wire
Dispersion liquid is added dropwise in chloroform along chamber wall, treats VO2(A) nano wire is after chloroform surface self-organization becomes oldered array, uses lining
The end, is picked up, and obtains being covered with on it VO2(A) substrate of nanometer line ordered array；Wherein, substrate is insulator.Again by it
It is covered with VO2(A) substrate of nanometer line ordered array is placed in protective atmosphere (or vacuum), after the 70min that anneals at 533 DEG C,
Physical separation substrate；Wherein, protective atmosphere is nitrogen atmosphere.Prepare and be similar to shown in Fig. 2 a, and as in Fig. 2 b and Fig. 3
VO shown in curve2(M) nanometer line ordered array.
Embodiment 5
Concretely comprising the following steps of preparation:
Step 1, first uses hydro-thermal method to obtain VO2(A) nano wire.Again by VO2(A) nano wire and water are 1 according to weight ratio:
After the ratio mixing of 1200, ultrasonic 10min, obtain VO2(A) nanowire dispersion.
Step 2, first according to VO2(A) weight of nanowire dispersion and chloroform is than the ratio for 1:10, by VO2(A) nanometer
Line dispersion liquid is added dropwise in chloroform along chamber wall, treats VO2(A) nano wire is after chloroform surface self-organization becomes oldered array, uses
Substrate is picked up, and obtains being covered with on it VO2(A) substrate of nanometer line ordered array；Wherein, substrate is insulator.Again by it
On be covered with VO2(A) substrate of nanometer line ordered array is placed in protective atmosphere (or vacuum), and anneal at 550 DEG C 60min
After, physical separation substrate；Wherein, protective atmosphere is nitrogen atmosphere.Prepare and be similar to shown in Fig. 2 a, and such as Fig. 2 b and Fig. 3
In the VO shown in curve2(M) nanometer line ordered array.
Select respectively again as the conductor of substrate or semiconductor or insulator, as the nitrogen of protective atmosphere or argon gas or
Helium or neon, repeat above-described embodiment 1～5, prepared equally as or be similar to shown in Fig. 2 a, and as in Fig. 2 b and Fig. 3
The VO shown in curve2(M) nanometer line ordered array.
Obviously, those skilled in the art can be to the VO of the present invention2(M) nanometer line ordered array and preparation method thereof enters
Row is various to be changed with modification without departing from the spirit and scope of the present invention.So, if these of the present invention are changed and modification
Within the scope of belonging to the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these changes and modification exists
In.
Claims (10)
1. a VO2(M) nanometer line ordered array, by VO2(M) form, it is characterised in that:
Described VO2(M) pattern is nanometer line ordered array, and described nanometer line ordered array is that nano wire has along its line length direction
Sequence is arranged in array；
Described composition VO2(M) VO of nanometer line ordered array2(M) linear diameter of nano wire be 200～600nm, line length be 10～
50μm。
2. VO described in a claim 12(M) preparation method of nanometer line ordered array, including hydro-thermal method, it is characterised in that main
Want step as follows:
Step 1, first uses hydro-thermal method to obtain VO2(A) nano wire, then by VO2(A) nano wire and water according to weight than for 1:800～
After the ratio mixing of 1200, ultrasonic at least 10min, obtain VO2(A) nanowire dispersion；
Step 2, first according to VO2(A) the weight ratio of nanowire dispersion and chloroform is 1: the ratio of >=0.8, by VO2(A) nano wire
Dispersant liquid drop adds in chloroform, treats VO2(A) nano wire is after chloroform surface self-organization becomes oldered array, uses substrate to be dragged for
Rise, obtain being covered with on it VO2(A) substrate of nanometer line ordered array, then VO will be covered with on it2(A) lining of nanometer line ordered array
The end, is placed in vacuum or protective atmosphere, after at least 60min that anneals, separates substrate, prepare VO at 480～550 DEG C2(M) receive
Rice noodles oldered array.
3. VO according to claim 22(M) preparation method of nanometer line ordered array, is characterized in that hydro-thermal method obtains VO2
(A) process of nano wire is, is first 0.2～0.4:0.4～0.6:50 by vanadium pentoxide powder, oxalic acid and water according to weight ratio
Ratio mixing after stir at least 1h, obtain precursor solution, then precursor solution be placed in air-tight state, in 200～240 DEG C
Under react at least 50h after, chilled reactant liquor is carried out successively separation of solid and liquid, washing and be dried process.
4. VO according to claim 22(M) preparation method of nanometer line ordered array, is characterized in that VO2(A) nano wire
For along chamber wall dropping when dispersant liquid drop adds in chloroform.
5. VO according to claim 22(M) preparation method of nanometer line ordered array, is characterized in that substrate is conductor, or
Semiconductor, or insulator.
6. VO according to claim 22(M) preparation method of nanometer line ordered array, is characterized in that protective atmosphere is nitrogen
Gas atmosphere, or argon gas atmosphere, or helium atmosphere, or neon atmosphere.
7. VO according to claim 22(M) preparation method of nanometer line ordered array, is characterized in that separating substrate is physics
Separate.
8. VO according to claim 32(M) preparation method of nanometer line ordered array, is characterized in that separation of solid and liquid is processed as
Centrifugation, its rotating speed be 8000～12000r/min, time be 5～15min.
9. VO according to claim 32(M) preparation method of nanometer line ordered array, is characterized in that carrying out washing treatment is use
Deionized water and the solid to isolated for the ethanol carry out the alternately cleaning of 2～3 times, separate solid for centrifugal point during cleaning
From.
10. VO according to claim 32(M) preparation method of nanometer line ordered array, it is characterized in that be dried be processed as by
Solid after cleaning is placed at 40～80 DEG C baking 10～14h.
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| CN106809877A (en) * | 2017-03-20 | 2017-06-09 | 武汉理工大学 | A kind of preparation method of D phase hypovanadic oxides |
| CN108890820A (en) * | 2018-08-13 | 2018-11-27 | 东北林业大学 | A kind of preparation method of the wooden energy storage material of light temperature double-response |
| CN109748320A (en) * | 2019-03-20 | 2019-05-14 | 广州大学 | A kind of monoclinic phase vanadium dioxide nano wire film and its preparation method and application |
| CN110306260A (en) * | 2019-06-18 | 2019-10-08 | 东华大学 | A kind of macroscopic inorganic semiconductor nano fiber and its preparation method and application |
| CN111392685A (en) * | 2020-03-05 | 2020-07-10 | 华中科技大学 | Two-dimensional self-assembled M1/M2-VO2Homojunction nanosheet and preparation method thereof |
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| CN103663556A (en) * | 2013-12-11 | 2014-03-26 | 哈尔滨工业大学深圳研究生院 | A-phase vanadium dioxide nanowire preparation method |
| CN104152897A (en) * | 2014-08-15 | 2014-11-19 | 国家纳米科学中心 | Method for manufacturing SERS substrate monolayer film and SERS substrate monolayer film |
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| CN101955752A (en) * | 2010-10-15 | 2011-01-26 | 华东师范大学 | Vanadium dioxide (VO2) phase change material with beam-shaped nanostructure and preparation method thereof |
| CN103663556A (en) * | 2013-12-11 | 2014-03-26 | 哈尔滨工业大学深圳研究生院 | A-phase vanadium dioxide nanowire preparation method |
| CN104152897A (en) * | 2014-08-15 | 2014-11-19 | 国家纳米科学中心 | Method for manufacturing SERS substrate monolayer film and SERS substrate monolayer film |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106809877A (en) * | 2017-03-20 | 2017-06-09 | 武汉理工大学 | A kind of preparation method of D phase hypovanadic oxides |
| CN108890820A (en) * | 2018-08-13 | 2018-11-27 | 东北林业大学 | A kind of preparation method of the wooden energy storage material of light temperature double-response |
| CN109748320A (en) * | 2019-03-20 | 2019-05-14 | 广州大学 | A kind of monoclinic phase vanadium dioxide nano wire film and its preparation method and application |
| CN109748320B (en) * | 2019-03-20 | 2021-05-11 | 广州大学 | Monoclinic-phase vanadium dioxide nanowire film and preparation method and application thereof |
| CN110306260A (en) * | 2019-06-18 | 2019-10-08 | 东华大学 | A kind of macroscopic inorganic semiconductor nano fiber and its preparation method and application |
| CN111392685A (en) * | 2020-03-05 | 2020-07-10 | 华中科技大学 | Two-dimensional self-assembled M1/M2-VO2Homojunction nanosheet and preparation method thereof |
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