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
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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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