Preparation method of monodispersed M-phase vanadium dioxide nanoparticles

A vanadium dioxide nano, vanadium dioxide technology, applied in the field of nanoparticle preparation, can solve the problems of difficulty in reducing production costs, increasing preparation complexity, large amount of oxalic acid, etc., to achieve good phase transition characteristics, excellent infrared control performance, The effect of simplifying the preparation process

Inactive Publication Date: 2014-10-01
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this preparation method has obtained granular M-phase vanadium dioxide, there are also shortcomings. First, the amount of oxalic acid is too large, which is easy to affect the environment; secondly, the intermediate product-solid vanadyl oxalate precursor During bulk annealing, temperature gradient control is required, which increases the complexity of preparation and makes it difficult to reduce production costs

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Embodiment 1

[0019] The concrete steps of preparation are:

[0020] In step 1, vanadium pentoxide, oxalic acid dihydrate and water are mixed in a molar ratio of 1:1:500; wherein, the water is deionized water to obtain a mixed liquid. Then add a surfactant to the mixed solution and stir for 2 hours, wherein the added amount of the surfactant is 4% of the volume of the mixed solution, and the surfactant is polyethylene glycol to obtain a precursor solution.

[0021] In step 2, first place the precursor solution in an airtight state, and react at a temperature of 200°C for 5 days to obtain a reaction solution. Then the reaction solution is subjected to solid-liquid separation and washing in sequence; wherein, the solid-liquid separation is centrifugation, and the speed of centrifugation is 10000r / min, and the washing process is obtained after centrifugation with deionized water and ethanol respectively. The solid matter is washed 3 times, and the approximate figure 1 as shown in a, and as ...

Embodiment 2

[0024] The concrete steps of preparation are:

[0025] In step 1, vanadium pentoxide, oxalic acid dihydrate and water are mixed in a molar ratio of 1.4:1:580; wherein, the water is deionized water to obtain a mixed solution. Then add a surfactant to the mixed solution and stir for 2.5 hours, wherein the added amount of the surfactant is 4.5% of the volume of the mixed solution, and the surfactant is polyethylene glycol to obtain a precursor solution.

[0026] Step 2, first place the precursor solution in a closed state, and react at a temperature of 215° C. for 4 days to obtain a reaction solution. Then the reaction solution is subjected to solid-liquid separation and washing in sequence; wherein, the solid-liquid separation is centrifugation, and the speed of centrifugation is 11000r / min, and the washing process is obtained after centrifugation with deionized water and ethanol respectively. The solid matter is washed 3 times, and the approximate figure 1 as shown in a, and ...

Embodiment 3

[0029] The concrete steps of preparation are:

[0030]In step 1, vanadium pentoxide, oxalic acid dihydrate and water are mixed in a molar ratio of 1.8:1:650; wherein, the water is deionized water to obtain a mixed solution. Then add a surfactant to the mixed liquid and then stir for 3 hours, wherein the added amount of the surfactant is 5% of the volume of the mixed liquid, and the surfactant is polyethylene glycol to obtain a precursor solution.

[0031] Step 2, first place the precursor solution in a closed state, and react at a temperature of 230° C. for 3 days to obtain a reaction solution. Then the reaction solution is subjected to solid-liquid separation and washing in sequence; wherein, the solid-liquid separation is centrifugation, and the speed of centrifugation is 12000r / min, and the washing process is obtained after centrifugation with deionized water and ethanol respectively. The solid matter is cleaned 3 times to obtain such as figure 1 as shown in a, and as fi...

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Abstract

The invention discloses a preparation method of monodispersed M-phase vanadium dioxide nanoparticles. The preparation method comprises the following steps: mixing vanadium pentoxide, oxalate dihydrate and water according to a molar ratio of (1-2.5) : 1 : (500-800) to obtain mixed liquid, adding 4%-6% of a surfactant based on the volume of the mixed liquid into the mixed liquid, and stirring for at least 2 hours to obtain a precursor solution; reacting the precursor solution in a sealed state at 200-260 DEG C for at least 1 day to obtain reaction liquid; performing solid-liquid separation and washing on the reaction liquid in sequence to obtain orthogonal vanadium dioxide powder; annealing the orthogonal vanadium dioxide powder in a nitrogen atmosphere at 300-600 DEG C for 0.5 hour to obtain the monodispersed M-phase vanadium dioxide nanoparticles with particle sizes of 60nm-80nm. The preparation method has the advantages of environmental protection and no temperature gradient control during annealing, and can be widely used for preparing the M-phase vanadium dioxide nanoparticles with very good dispersity.

Description

technical field [0001] The invention relates to a method for preparing nanoparticles, in particular to a method for preparing monodisperse M-phase vanadium dioxide nanoparticles. Background technique [0002] M phase vanadium dioxide (VO 2 (M)) The single crystal has the characteristic of transition from a monoclinic semiconductor phase to a tetragonal metal phase at 341k. Near the phase transition, the optical and electrical properties of the material will change abruptly. In the infrared band, the monoclinic phase has higher transmission properties, while the tetragonal phase has higher reflection properties. will VO 2 (M) As an infrared control material, using VO before and after Mott phase transition 2 The sudden change in electricity and optics has great potential application value in optoelectronic devices, infrared detection, smart windows, storage devices and other fields. For this reason, people have made various efforts in order to obtain M-phase vanadium dioxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02B82Y30/00
Inventor 李登兵李明潘静张云霞李广海
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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