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Process method for preparing vanadium dioxide nano-powder

A kind of technology of vanadium dioxide nanometer and process method, which is applied in the process field to achieve the effects of energy saving, uniform appearance and improved system dispersibility

Inactive Publication Date: 2021-01-01
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, these methods are difficult to obtain monodisperse, high-purity, and sufficiently small nano-powders with high yield and high efficiency.

Method used

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Experimental program
Comparison scheme
Effect test

specific Embodiment

[0034] In view of the problems existing in the prior art, the object of the present invention is to provide a method for preparing monodisperse, high-purity vanadium dioxide powder in high yield. Before the hydrothermal reaction, double ultrasonic spraying is used to prepare the precursor, which can combine the advantages of double ultrasonic atomization and hydrothermal method, which is beneficial to make the hydrothermal reaction easier, and the prepared vanadium dioxide powder particles Small, evenly distributed throughout, good crystallinity.

[0035] The specific operation steps are as follows:

[0036] 1. Preparation of precipitant solution: Dissolve the precipitant in deionized water, prepare a 0.2-1mol / L solution, and disperse it ultrasonically for 15-30 minutes; the precipitant can be one of the following: ammonia water; sodium hydroxide; carbonic acid One or more of ammonium bicarbonate; ammonium carbonate; sodium bicarbonate; sodium carbonate.

[0037] 2. Preparat...

Embodiment 1

[0042] Step 1, dissolving 0.2 mol sodium hydroxide in deionized water, ultrasonically dispersing for 15-30 minutes, and preparing 1000 ml of solution a with a concentration of 0.2 mol / L;

[0043] Step 2, dissolving vanadyl sulfate in deionized water, making 1000ml of a solution with a concentration of 0.1mol / l, adding 5g of PEG-6000, and ultrasonically dispersing for 15-30min to obtain solution b;

[0044] Step 3: Place solutions a and b in a 3MHz ultrasonic atomization device for atomization, and then pass the atomized reaction droplets into the reactor to mix and react. The reaction process continues with ultrasonic and mechanical stirring. After fully reacting, The suspension is obtained, and then the precipitate c is obtained by centrifugation, and the rotation speed is 10000rpm;

[0045] Step 4. Wash the precipitate c three times with deionized water and twice with absolute ethanol. During each washing and alcohol washing process, the precursor suspension is stirred evenl...

Embodiment 2

[0048] Step 1, dissolving 0.4 mol sodium hydroxide in deionized water, ultrasonically dispersing for 15-30 minutes, and preparing 1000 ml of solution a with a concentration of 0.4 mol / L;

[0049] Step 2, dissolving vanadyl sulfate in deionized water, making 1000 ml of a solution with a concentration of 0.2 mol / l, adding 10 g of PEG-2000, and ultrasonically dispersing for 15 to 30 minutes to obtain solution b;

[0050] Step 3: Place solutions a and b in a 3MHz ultrasonic atomization device for atomization, and then pass the atomized reaction droplets into the reactor for mixed reaction. The reaction process continues with ultrasonic and mechanical stirring. After fully reacting, The suspension was obtained, aged for 6 hours, and then the precipitate c was obtained by centrifugation at a speed of 10,000 rpm;

[0051] Step 4. Wash the precipitate c three times with deionized water and twice with absolute ethanol. During each washing and alcohol washing process, the precursor susp...

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Abstract

The invention discloses a process method, particularly discloses a process method for preparing vanadium dioxide nano-powder, and belongs to the technical field of metallurgical production process manufacturing. The process method for preparing the vanadium dioxide nano-powder is short in preparation time, high in preparation efficiency and capable of saving energy and preparing the vanadium dioxide nano-powder which is uniform in morphology and high in system dispersity. The process method comprises the following steps: respectively atomizing an alkaline precipitator and a surfactant-containing tetravalent vanadate solution into fog drops with the particle size of less than 10 microns by adopting an ultrasonic atomizer, then putting the two atomized liquid drops into a reactor in an ultrasonic water bath for contact, making reacting to generate a VO(OH)2 precipitate, collecting the precipitate VO(OH)2 obtained by the reaction by using ethanol, and performing washing to obtain a VO(OH)2 precursor; carrying out ultrasonic dispersion on the collected and washed VO(OH)2 precursor and deionized water to form a suspension; and finally, carrying out hydrothermal crystallization treatmenton the suspension to obtain the nano vanadium dioxide with uniform granularity and dispersed monomers.

Description

technical field [0001] The invention relates to a process method, in particular to a process method for preparing vanadium dioxide nanometer powder, which belongs to the technical field of metallurgical production process manufacturing. 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, among which VO 2 (M) is currently the most studied phase. 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 before the phase tran...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y30/00B82Y40/00
CPCC01G31/02B82Y30/00B82Y40/00C01P2004/64
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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