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

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

Active Publication Date: 2021-01-12
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, such a scheme is preferred in step a: 1. In step a, the purity of the tetravalent vanadium salt is ≥ 99.0%; 2. In step a, the molar concentration of the precursor solution is 0.01 to 1 mol / L; 3. In step a, ultrasonically disperse for 15 to 30 min; 4. In step a, the auxiliary salt is: sodium nitrate, potassium nitrate, sodium acetate, potassium chloride, lithium chloride, potassium chloride or its total 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 the auxiliary salt to the vanadium salt: 2:1 to 10:1 . Through the above-mentioned more precise control, the quality of the preparation can be effectively improved, so as to obtain better products.

[0019] Similarly, in order to obtain a better preparation effect, such a scheme is preferred in step b: 1. In step b, the ultrasonic frequency of the ultrasonic nebulizer is 1.7-3MHz, and...

Embodiment 1

[0022] a. Configure 1000ml of 0.2mol / L vanadyl dichloride solution, add 1mol sodium acetate at the same time, and sonicate for 1h to obtain a blue and transparent precursor solution;

[0023] b. Place the precursor solution prepared in step a in an ultrasonic nebulizer with an ultrasonic frequency of 3 MHz to atomize to generate mist droplets, and pass the small droplets through a vertical tube furnace with a heating temperature of 550 ° C by 5 L / min nitrogen gas, Collected by 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 40-50nm .

Embodiment 2

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

[0026] b. The precursor solution prepared in step a is placed in an ultrasonic nebulizer with an ultrasonic frequency of 3 MHz and atomized to produce droplets, and the small droplets are passed through a vertical tube furnace with a heating temperature of 600 ° C by 5 L / min nitrogen gas, and passed through Collected by 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 50-70nm.

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Abstract

The invention relates to the field of preparation methods of inorganic functional materials, in particular to a method for preparing M-phase vanadium dioxide nano-powder by a salt-assisted ultrasonicpyrolysis method, and the preparing method is simple in synthesis process and short in flow and can be used for efficiently preparing monodisperse and high-purity nano-vanadium dioxide powder. The preparation method comprises the following steps: a, preparing a precursor solution: dissolving auxiliary salt and tetravalent vanadate in deionized water to prepare a precursor solution of a vanadium source, and carrying out ultrasonic dispersion treatment; and b, preparing M-phase vanadium dioxide nano-powder: putting the precursor solution prepared in the step a into an ultrasonic atomizer, conducting atomizing to generate fog drops, collecting the fog drops carried by carrier gas through a vertical tube furnace and a high-voltage electrostatic collector, then putting the collected powder intodeionized water, and performing ultrasonic treatment and filtration, and conducting drying in vacuum to obtain the M-phase vanadium dioxide nano-powder. The preparation method is particularly suitable for the preparation process of the M-phase vanadium dioxide nano-powder.

Description

technical field [0001] The invention relates to the field of preparation methods of inorganic functional materials, in particular to a method for preparing M-phase vanadium dioxide nanopowder by a salt-assisted ultrasonic pyrolysis method. Background technique [0002] Vanadium dioxide (VO 2 ) is currently the most reported and most 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 isotropes. where VO 2 (M) The M-phase vanadium dioxide is currently 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 crystal structure, resistivity, optical properties, etc. Thanks to VO 2 Unique phase transition properties and excellent performance have been applied in smart glass, optical storage,...

Claims

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Application Information

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Patent Type & Authority Applications(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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