Method for preparing m-phase vanadium dioxide nano-powder by salt-assisted ultrasonic pyrolysis

A technology of vanadium dioxide nanometer and pyrolysis method, which is applied in the field of preparation of inorganic functional materials, can solve the problems of unfavorable large-scale production and high cost, and achieve the effect of low cost, easy operation, continuous and rapid production

Active Publication Date: 2022-07-29
CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above method has strict requirements on the experimental atmosphere and high cost, which is not conducive to large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0018] In order to obtain a better preparation effect, the following scheme is preferred in step a: 1. In step a, the purity of the tetravalent vanadium salt is greater than or equal to 99.0%; 2. In step a, the molar concentration of the precursor solution is 0.01-1 mol 3. In step a, ultrasonic dispersion is performed for 15-30 min; 4. In step a, the auxiliary salt is: sodium nitrate, potassium nitrate, sodium acetate, potassium chloride, lithium chloride, potassium chloride or a combination thereof molten mixture; 5. In step a, the vanadium salt is: vanadyl sulfate, vanadyl oxalate or vanadyl dichloride; 6. In step a, the molar ratio of auxiliary salt to vanadium salt: 2:1~10:1 . Through the above-mentioned more precise control, the quality of preparation can be effectively improved, thereby obtaining better products.

[0019] Similarly, in order to obtain a better preparation effect, the following scheme is preferred in step b: 1. In step b, the ultrasonic frequency of the ...

Embodiment 1

[0022] a. Prepare 1000ml of 0.2mol / L vanadium oxychloride solution, add 1mol of sodium acetate at the same time, and ultrasonicate for 1h to obtain a blue and transparent precursor solution;

[0023] b. The precursor solution prepared in step a is placed in an ultrasonic atomizer with an ultrasonic frequency of 3MHz to be atomized to generate droplets, and the droplets are passed through a vertical tube furnace with a heating temperature of 550°C by 5L / min nitrogen gas, Collected through a high-voltage electrostatic collector, reacted for 1 hour, placed the collected powder in deionized water, ultrasonicated for 1 hour, filtered, and vacuum-dried at 80 °C to obtain blue-black M-phase vanadium dioxide nano-powder with a particle size of 40-50 nm. .

Embodiment 2

[0025] a. Configure 1000ml of 0.2mol / L vanadium oxychloride solution, add 1mol potassium chloride / lithium chloride (molar ratio 0.59 / 0.41) at the same time, and ultrasonicate for 1h to obtain a blue and transparent precursor solution;

[0026] b. The precursor solution prepared in step a is placed in an ultrasonic atomizer with an ultrasonic frequency of 3MHz for atomization to generate droplets, and the droplets are passed through a vertical tube furnace with a heating temperature of 600°C by 5L / min nitrogen gas, Collected with a high-voltage electrostatic collector, reacted for 1 hour, placed the collected powder in deionized water, ultrasonicated for 1 hour, filtered, and vacuum-dried at 80°C to obtain blue-black M-phase vanadium dioxide nanopowder with a particle size of 50-70 nm.

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Abstract

The invention relates to the field of preparation methods for inorganic functional materials, in particular to a salt-assisted ultrasonic pyrolysis method for preparing M-phase dioxide with a simple synthesis process and a short process, which can efficiently prepare monodisperse, high-purity nanometer vanadium dioxide powders The method for vanadium nano-powder includes the following steps: a. Preparing a precursor solution: dissolving auxiliary salt and tetravalent vanadium salt in deionized water, configuring into a precursor solution of vanadium source, and ultrasonically dispersing; b. preparing M Phase vanadium dioxide nano-powder: put the precursor solution prepared in step a in an ultrasonic atomizer and atomize to generate droplets, which are carried by the carrier gas through a vertical tube furnace and through a high-voltage electrostatic collector Collect, then put the collected powder in deionized water, carry out ultrasonic treatment and filtration, and obtain M-phase vanadium dioxide nano-powder after vacuum drying. The invention is especially suitable for the preparation process for preparing M-phase vanadium dioxide nano-powder.

Description

technical field [0001] The invention relates to the field of preparation methods for inorganic functional materials, in particular to a method for preparing M-phase vanadium dioxide nano-powder by a salt-assisted ultrasonic pyrolysis method. Background technique [0002] Vanadium dioxide (VO 2 ) is currently the most reported and widely used vanadium oxide, with VO 2 (A), VO 2 (B), VO 2 (C), VO 2 (D), VO 2 (M), VO 2 (R), VO 2 (T) and VO 2 (P) and other allotropes. where VO 2 (M) is the M-phase vanadium dioxide is the most studied phase. Since Morin F.J. first discovered that it has a semiconductor-metal phase transition in 1959, it has been confirmed that light, heat, electricity, stress, etc. can induce VO 2 (M) A phase transition occurs, accompanied by dramatic changes in properties such as crystal structure, resistivity, and optics. Due to VO 2 The unique phase change properties and excellent performance have been used in smart glass, optical storage, laser ra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/02B82Y40/00B01J19/10
CPCC01G31/02B82Y40/00B01J19/10C01P2004/64C01P2004/62
Inventor 辛亚男彭穗刘波李道玉
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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