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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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000002070 nanowire Substances 0.000 claims abstract description 149
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000758 substrate Substances 0.000 claims abstract description 45
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 239000012298 atmosphere Substances 0.000 claims abstract description 21
- 230000001681 protective effect Effects 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 15
- 239000012212 insulator Substances 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 239000004065 semiconductor Substances 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004020 conductor Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052754 neon Inorganic materials 0.000 claims description 4
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000003491 array Methods 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000012855 volatile organic compound Substances 0.000 claims 15
- 230000004044 response Effects 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 59
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012782 phase change material Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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 invention relates to an ordered array and a preparation method thereof, in particular to a VO2(M) (M phase vanadium dioxide) nanowire ordered array and a preparation method thereof.
Background
Vanadium dioxide is a mott phase change material, and when conditions such as temperature or pressure are changed, it is transformed from an insulator phase or a semiconductor phase to a metal phase, and at the same time, its resistivity, optical refractive index, magnetic susceptibility, reflectivity, etc. are also changed. The vanadium dioxide crystals having different phases, e.g. VO2(A)、VO2(B)、VO2(C)、VO2(D)、VO2(M) and VO2(R) and the like, wherein VO2The phase transition temperature of (M) is closest to room temperature (68 ℃). At present, in the aspect of vanadium dioxide photoelectric detection, although a single vanadium dioxide nanowire reported in documents has excellent photoelectric detection performance, the single vanadium dioxide nanowire has a small photocurrent value and cannot be prepared into a device, so that the single vanadium dioxide nanowire is difficult to be practically applied. To solve this problem, some beneficial attempts and efforts have been made, such as the title "OrientatedLangmuir-Blodgett Assembly of VO2An article by Nanowires ", Nano lett, vol.9, No.2,2009 (" LB statutory directional assembly of vanadium dioxide Nanowires "," Nano promissory "2009, volume 9, phase 2). The vanadium dioxide nano-wire mentioned in the paper is VO with wire diameter of 200-500 nm2(B) A nanowire; when in preparation, V is firstly2O5Preparing precursor solution with hexadecyl trimethyl ammonium bromide, and obtaining VO by a hydrothermal method2(B) Nanowires, and then using stearic acid, cyclohexane, hexadecyl trimethyl ammonium bromide and the like to the VO respectively2(B) And (3) after the surface of the nanowire is modified, assembling the nanowire by using an LB film machine to obtain a product. However, both the product and the process for its preparation have disadvantages, first of all VO2(B) VO without phase transition characteristic and with application prospect difficult to approach room temperature with phase transition temperature2(M) phase-contrast theory; secondly, the length of the nanowire is basically not more than 5 μm, the nanowire is arranged along a certain direction in a very small range, and the nanowire still presents a disordered and distributed disordered state under the scale of 5 μm on the whole; thirdly, various surface modifiers and active agents are used in the process of preparing the product, and the surface modifiers and active agents remained on the product have adverse effects on the practical application of the product; finally, the preparation methodVO can not be obtained by the method2The (M) nanowire ordered array also has the defects of complex process and high cost.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide the VO with longer nano-wires and orderly arranged in an array along the length direction of the nano-wires2(M) an ordered array of nanowires.
Another technical problem to be solved by the present invention is to provide a VO as described above2(M) a method for preparing the ordered nanowire array.
In order to solve the technical problem of the invention, the adopted technical scheme is as follows: VO (vacuum vapor volume)2(M) ordered arrays of nanowires consisting of VO2(M) a composition, in particular,
the VO2(M) the shape of the nanowire array is a nanowire ordered array, and the nanowire ordered array is formed by orderly arranging nanowires along the length direction of the nanowires;
the composition VO2VO of (M) nanowire ordered array2The (M) nanowire has a wire diameter of 200 to 600nm and a wire length of 10 to 50 μ M.
In order to solve another technical problem of the present invention, another technical solution is adopted: VO described above2The preparation method of the (M) nanowire ordered array comprises a hydrothermal method, and particularly comprises the following main steps:
step 1, firstly obtaining VO by using a hydrothermal method2(A) Nanowire and VO2(A) The weight ratio of the nano wire to the water is 1: mixing the materials in a ratio of 800-1200, and performing ultrasonic treatment for at least 10min to obtain VO2(A) A nanowire dispersion;
step 2, firstly according to VO2(A) The weight ratio of the nanowire dispersion liquid to the chloroform is 1: at a ratio of not less than 0.8, adding VO2(A) Adding the nano-wire dispersed liquid drop into chloroform until VO2(A) Self-assembly of nanowires into order on chloroform surfaceAfter the array, the substrate was used to pick it up to obtain VO coated thereon2(A) A substrate of the ordered array of nanowires, and VO is coated on the substrate2(A) Placing the substrate of the nanowire ordered array in vacuum or protective atmosphere, annealing at 480-550 ℃ for at least 60min, and separating the substrate to obtain VO2(M) an ordered array of nanowires.
As VO2(M) further improvement of the preparation method of the ordered array of nanowires:
preferably, VO is obtained by hydrothermal method2(A) The process of the nanowire comprises the steps of mixing vanadium pentoxide powder, oxalic acid and water according to the weight ratio of 0.2-0.4: 0.4-0.6: 50, stirring for at least 1h to obtain a precursor solution, placing the precursor solution in a closed state, reacting for at least 50h at 200-240 ℃, and then sequentially carrying out solid-liquid separation, washing and drying on the cooled reaction liquid.
Preferably, VO is mixed2(A) The nanowire dispersion liquid is dripped along the wall of the container when being added into chloroform.
Preferably, the substrate is a conductor, or a semiconductor, or an insulator.
Preferably, the protective atmosphere is a nitrogen atmosphere, or an argon atmosphere, or a helium atmosphere, or a neon atmosphere.
Preferably, the separation substrate is physically separated.
Preferably, the solid-liquid separation treatment is centrifugal separation, the rotating speed of the centrifugal separation is 8000-12000 r/min, and the time is 5-15 min.
Preferably, the washing treatment is to alternately wash the separated solid matters for 2-3 times by using deionized water and ethanol, and the solid matters are separated in the washing process by centrifugal separation.
Preferably, the drying treatment is to bake the cleaned solid object at 40-80 ℃ for 10-14 h.
Compared with the prior art, the beneficial effects are that:
firstly, the prepared target product is characterized by using a scanning electron microscope, an X-ray diffractometer and a semiconductor tester respectively, and the result shows that the target product is VO2(M) the shape of the nano-wire ordered array; the nanowire ordered array is formed by orderly arranging nanowires along the length direction of the nanowires, wherein the diameter of the nanowires is 200-600 nm, and the length of the nanowires is 10-50 mu m. This is composed of VO2(M) target product assembled by nanowires, i.e. due to VO2The phase transition temperature of the (M) is closest to the room temperature, the nano-wires have the wire diameter of nano size, the wire length of the nano-wires is more than or equal to 10 mu M, and the nano-wires are orderly arranged into an array along the wire length direction, particularly the phase transition temperature is closest to the room temperature, so the performance of the nano-wires is improved. Tests show that the photocurrent value of the target product is greatly improved.
Secondly, the preparation method is simple, scientific and efficient. Not only the target product-VO with longer nano-wire length and highly orderly arranged into an array along the wire length direction is prepared2(M) an ordered array of nanowires; the preparation method also can prepare large-area target products without being interfered by a surface modifier and an active agent in practical application and without limitation according to requirements; the method has the characteristics of simple and convenient process and low cost; further, the target product is easy to be widely applied to the fields of photoelectric detection, intelligent response, electrocatalysis, sensors, magnetic devices and the like in a commercial mode.
Drawings
FIG. 1 shows the VO obtained by hydrothermal method2(A) Nanowire and VO2(A) The ordered array of nanowires was characterized using one of a Scanning Electron Microscope (SEM) and an X-ray diffraction (XRD) instrument, respectively. Wherein FIG. 1a shows VO obtained by hydrothermal method2(A) SEM images of nanowires; FIG. 1b is VO2(A) SEM images of the ordered array of nanowires; FIG. 1c is an XRD spectrum of the ordered array of nanowires shown in FIGS. 1a and 1b, which shows that the ordered array of nanowires is VO2(A) An ordered array of nanowires.
FIG. 2 shows one of the results of the characterization of the objective product obtained by the preparation method using a scanning electron microscope and an X-ray diffractometer, respectively. Wherein, fig. 2a is an SEM image of the target product, and fig. 2b is an XRD spectrogram of the target product; it can be seen that the desired product is VO2(M) an ordered array of nanowires.
FIG. 3 is one of the results of characterization of the obtained objective product using a semiconductor tester. The result proves that the photocurrent value of the target product is greatly improved relative to that of a single nanowire.
Detailed Description
Preferred embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
First commercially available or manufactured on its own:
VO2(A) a nanowire; chloroform; conductors, semiconductors, and insulators as substrates; nitrogen, argon, helium and neon as protective atmosphere. Wherein,
hydrothermal method to obtain VO2(A) Mixing vanadium pentoxide powder, oxalic acid and water according to the weight ratio of 0.2-0.4: 0.4-0.6: 50, stirring for at least 1h to obtain a precursor solution, placing the precursor solution in a closed state, reacting for at least 50h at 200-240 ℃, and then sequentially carrying out solid-liquid separation, washing and drying on the cooled reaction solution; the solid-liquid separation treatment is centrifugal separation, the rotating speed is 8000-12000 r/min, the time is 5-15 min, the washing treatment is to use deionized water and ethanol to alternately clean the separated solid matters for 2-3 times, the solid matters are separated during cleaning, the drying treatment is to place the cleaned solid matters at 40-80 ℃ for drying for 10-14 h.
Then, the process of the present invention is carried out,
example 1
The preparation method comprises the following specific steps:
step 1, firstly obtaining VO by using a hydrothermal method2(A) A nanowire. Then make VO2(A) The weight ratio of the nano wire to the water is 1: mixing at the ratio of 800, and performing ultrasonic treatment for 20min to obtain VO2(A) A nanowire dispersion.
Step 2, firstly according to VO2(A) The weight ratio of the nanowire dispersion liquid to the chloroform is 1: 0.8 of the ratio, mixing VO2(A) Dripping the nano-wire dispersion liquid into chloroform along the wall of the container until VO2(A) The nanowires are self-assembled into an ordered array on the chloroform surface, and then fished up by using a substrate to obtain VO coated on the nanowires2(A) A substrate of an ordered array of nanowires; wherein the substrate is an insulator. Then coating VO thereon2(A) Placing the substrate of the nanowire ordered array in a protective atmosphere (or vacuum), annealing at 480 ℃ for 100min, and physically separating the substrate; wherein the protective atmosphere is a nitrogen atmosphere. VO was prepared as shown approximately in FIG. 2a, and as shown by the curves in FIGS. 2b and 32(M) an ordered array of nanowires.
Example 2
The preparation method comprises the following specific steps:
step 1, firstly obtaining VO by using a hydrothermal method2(A) A nanowire. Then make VO2(A) The weight ratio of the nano wire to the water is 1: 900, and performing ultrasonic treatment for 18min to obtain VO2(A) A nanowire dispersion.
Step 2, firstly according to VO2(A) The weight ratio of the nanowire dispersion liquid to the chloroform is 1: 3 ratio of VO2(A) Dripping the nano-wire dispersion liquid into chloroform along the wall of the container until VO2(A) The nanowires are self-assembled into an ordered array on the chloroform surface, and then fished up by using a substrate to obtain VO coated on the nanowires2(A) A substrate of an ordered array of nanowires; wherein the substrate is an insulator. Then coating VO thereon2(A)The substrate of the nanowire ordered array is placed in protective atmosphere (or vacuum), and after annealing is carried out for 90min at 498 ℃, the substrate is physically separated; wherein the protective atmosphere is a nitrogen atmosphere. VO was prepared as shown approximately in FIG. 2a, and as shown by the curves in FIGS. 2b and 32(M) an ordered array of nanowires.
Example 3
The preparation method comprises the following specific steps:
step 1, firstly obtaining VO by using a hydrothermal method2(A) A nanowire. Then make VO2(A) The weight ratio of the nano wire to the water is 1: mixing at the ratio of 1000, and performing ultrasonic treatment for 15min to obtain VO2(A) A nanowire dispersion.
Step 2, firstly according to VO2(A) The weight ratio of the nanowire dispersion liquid to the chloroform is 1: 6 ratio of VO2(A) Dripping the nano-wire dispersion liquid into chloroform along the wall of the container until VO2(A) The nanowires are self-assembled into an ordered array on the chloroform surface, and then fished up by using a substrate to obtain VO coated on the nanowires2(A) A substrate of an ordered array of nanowires; wherein the substrate is an insulator. Then coating VO thereon2(A) Putting the substrate of the nanowire ordered array in a protective atmosphere (or vacuum), annealing at 515 ℃ for 80min, and physically separating the substrate; wherein the protective atmosphere is a nitrogen atmosphere. VO was prepared as shown in FIG. 2a, and as shown by the curves in FIGS. 2b and 32(M) an ordered array of nanowires.
Example 4
The preparation method comprises the following specific steps:
step 1, firstly obtaining VO by using a hydrothermal method2(A) A nanowire. Then make VO2(A) The weight ratio of the nano wire to the water is 1: 1100, and carrying out ultrasonic treatment for 13min to obtain VO2(A) A nanowire dispersion.
Step 2, firstly according to VO2(A) The weight ratio of the nanowire dispersion liquid to the chloroform is 1: 8 ratio of VO2(A) Dripping the nano-wire dispersion liquid into chloroform along the wall of the container until VO2(A) The nanowires are self-assembled into an ordered array on the chloroform surface, and then fished up by using a substrate to obtain VO coated on the nanowires2(A) A substrate of an ordered array of nanowires; wherein the substrate is an insulator. Then coating VO thereon2(A) Placing the substrate of the nanowire ordered array in a protective atmosphere (or vacuum), annealing at 533 ℃ for 70min, and then physically separating the substrate; wherein the protective atmosphere is a nitrogen atmosphere. VO was prepared as shown approximately in FIG. 2a, and as shown by the curves in FIGS. 2b and 32(M) an ordered array of nanowires.
Example 5
The preparation method comprises the following specific steps:
step 1, firstly obtaining VO by using a hydrothermal method2(A) A nanowire. Then make VO2(A) The weight ratio of the nano wire to the water is 1: 1200, and performing ultrasonic treatment for 10min to obtain VO2(A) A nanowire dispersion.
Step 2, firstly according to VO2(A) The weight ratio of the nanowire dispersion liquid to the chloroform is 1: 10 ratio of VO to2(A) Dripping the nano-wire dispersion liquid into chloroform along the wall of the container until VO2(A) The nanowires are self-assembled into an ordered array on the chloroform surface, and then fished up by using a substrate to obtain VO coated on the nanowires2(A) A substrate of an ordered array of nanowires; wherein the substrate is an insulator. Then coating VO thereon2(A) Putting the substrate of the nanowire ordered array in a protective atmosphere (or vacuum), annealing at 550 ℃ for 60min, and physically separating the substrate; wherein the protective atmosphere is a nitrogen atmosphere. VO was prepared as shown approximately in FIG. 2a, and as shown by the curves in FIGS. 2b and 32(M) an ordered array of nanowires.
Then respectively selecting conductor or semiconductor or insulator as substrate, nitrogen gas or argon gas or helium gas or neon gas as protective atmosphere, and dryingVO as shown in or similar to FIG. 2a, and VO shown in FIG. 2b and FIG. 3 were prepared in the same manner as in examples 1 to 52(M) an ordered array of nanowires.
It is obvious that those skilled in the art can apply the VO of the present invention2Various changes and modifications may be made in the (M) ordered array of nanowires and methods of making the same without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (10)
1. VO (volatile organic compound)2(M) ordered arrays of nanowires, from VO2(M) composition characterized by:
the VO2(M) the shape of the nanowire array is a nanowire ordered array, and the nanowire ordered array is formed by orderly arranging nanowires along the length direction of the nanowires;
the composition VO2VO of (M) nanowire ordered array2The (M) nanowire has a wire diameter of 200 to 600nm and a wire length of 10 to 50 μ M.
2. VO according to claim 12The (M) preparation method of the ordered nanowire array comprises a hydrothermal method and is characterized by mainly comprising the following steps:
step 1, firstly obtaining VO by using a hydrothermal method2(A) Nanowire and VO2(A) The weight ratio of the nano wire to the water is 1: mixing the materials in a ratio of 800-1200, and performing ultrasonic treatment for at least 10min to obtain VO2(A) A nanowire dispersion;
step 2, firstly according to VO2(A) The weight ratio of the nanowire dispersion liquid to the chloroform is 1: at a ratio of not less than 0.8, adding VO2(A) Adding the nano-wire dispersed liquid drop into chloroform until VO2(A) The nanowires are self-assembled into an ordered array on the chloroform surface, and then fished up by using a substrate to obtain VO coated on the nanowires2(A) A substrate of the ordered array of nanowires, and VO is coated on the substrate2(A) Placing the substrate of the nanowire ordered array in vacuum or protective atmosphere, annealing at 480-550 ℃ for at least 60min, and separating the substrate to obtain VO2(M) an ordered array of nanowires.
3. VO according to claim 22The preparation process of ordered (M) nanometer line array features the hydrothermal process of obtaining VO2(A) The process of the nanowire comprises the steps of mixing vanadium pentoxide powder, oxalic acid and water according to the weight ratio of 0.2-0.4: 0.4-0.6: 50, stirring for at least 1h to obtain a precursor solution, placing the precursor solution in a closed state, reacting for at least 50h at 200-240 ℃, and then sequentially carrying out solid-liquid separation, washing and drying on the cooled reaction liquid.
4. VO according to claim 22The preparation process of ordered nanometer (M) line array features that VO is first prepared2(A) The nanowire dispersion liquid is dripped along the wall of the container when being added into chloroform.
5. VO according to claim 22The preparation method of (M) nanowire ordered array is characterized by that its substrate is a conductor, or a semiconductor or an insulator.
6. VO according to claim 22The preparation method of (M) the nanowire ordered array is characterized in that the protective atmosphere is nitrogen atmosphere, argon atmosphere, helium atmosphere or neon atmosphere.
7. VO according to claim 22The preparation process of ordered nanometer line array features the physical separation of the substrate.
8. VO according to claim 32The preparation method of the (M) nanowire ordered array is characterized in that solid-liquid separation treatment is centrifugal separation, the rotating speed is 8000-12000 r/min, and the time is 5-15 min.
9. VO according to claim 32The preparation method of the (M) nanowire ordered array is characterized in that washing treatment is that deionized water and ethanol are used for alternately cleaning separated solids for 2-3 times, and the solid separation during cleaning is centrifugal separation.
10. VO according to claim 32The preparation method of the (M) nanowire ordered array is characterized in that the drying treatment is to bake the cleaned solid object at 40-80 ℃ for 10-14 h.
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Cited By (6)
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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 |
| CN117923545A (en) * | 2024-01-26 | 2024-04-26 | 西北大学 | Ordered arrangement method of vanadium pentoxide nanobelts or vanadium pentoxide hydrate nanobelts |
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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 |
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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 (7)
| 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 |
| CN117923545A (en) * | 2024-01-26 | 2024-04-26 | 西北大学 | Ordered arrangement method of vanadium pentoxide nanobelts or vanadium pentoxide hydrate nanobelts |
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