Method for directly preparing M-phase vanadium dioxide nano-powder through ultrasonic spray pyrolysis

A vanadium dioxide nanometer and ultrasonic spray pyrolysis technology, applied in vanadium oxide, nanotechnology and other directions, 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: 2021-01-05
CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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Problems solved by technology

However, the above method has strict requirements on the experimental at

Method used

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Experimental program
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Effect test

Embodiment 1

[0021] a. Configure 1000ml of 0.2mol / L vanadyl dichloride solution to obtain a blue and transparent precursor solution;

[0022] b. Place the precursor solution prepared in step a in an ultrasonic nebulizer with an ultrasonic frequency of 3MHz to atomize to generate mist droplets, and pass the small droplets through a vertical tube furnace with a heating temperature of 700°C by 5L / 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 60-100nm .

Embodiment 2

[0024] a. Configure 0.5mol / L vanadyl dichloride solution for 1000m to obtain a blue and transparent precursor solution;

[0025] 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 80-110 nm.

Embodiment 3

[0027] a. Configure 1000ml of 0.5mol / L vanadyl dichloride solution to obtain a blue and transparent precursor solution;

[0028] 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 700 ° C by 2 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 30-150nm. The median particle size is 70nm.

[0029] The invention directly prepares the M-phase vanadium dioxide nanometer powder based on the ultrasonic spray pyrolysis method, and can prepare the nanometer powder with uniform appearance, narrow distribution and good dispersibility. Compared ...

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Abstract

The invention relates to the field of preparation of vanadium dioxide powder, in particular to a method for directly preparing M-phase vanadium dioxide nano-powder through ultrasonic spray pyrolysis,which is simple in synthesis process, short in flow and capable of directly preparing monodisperse and high-purity nano vanadium dioxide powder with high yield. The method comprises the following steps: a, dissolving vanadyl sulfate in deionized water, preparing a vanadyl sulfate solution of a vanadium source, carrying out ultrasonic dispersion, adding equimolar barium chloride into the vanadyl sulfate solution, fully reacting, and filtering out the generated barium sulfate precipitate to obtain a vanadyl dichloride precursor solution, and b, putting the precursor solution prepared in the stepa into an ultrasonic atomizer, atomizing to generate fog drops, carrying the small liquid drops through carrier gas to pass through a vertical tube furnace, collecting through a high-voltage electrostatic collector, then putting the collected powder into deionized water, and performing ultrasonic treatment, filtration and vacuum drying to obtain the M-phase vanadium dioxide nano-powder. The method is particularly suitable for preparing the M-phase vanadium dioxide nano-powder.

Description

technical field [0001] The invention relates to the field of vanadium dioxide powder preparation, in particular to a method for directly preparing M-phase vanadium dioxide nanometer powder by ultrasonic spray pyrolysis. 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) That is, the M-phase vanadium dioxide is the most studied phase at present, and 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. When the phase transition occurs, its crystal structure changes from monoclinic phase to tetragonal rutile phase, and the resistivity undergoes a sudden change of more than 3 orders of magnitude, changing from a semiconductor b...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y40/00
CPCC01G31/02B82Y40/00C01P2004/64
Inventor 辛亚男彭穗刘波姚洁
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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