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A method for preparing monoclinic phase vanadium dioxide powder by ball milling reduction

A technology of vanadium dioxide and monoclinic phase, applied in vanadium oxide, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problems of poor environmental protection, high energy consumption, long reaction time and other unfavorable problems, and achieve The effect of low price, wide range of sources, and easy product separation

Active Publication Date: 2021-12-31
蒋绪川
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to provide a method for preparing monoclinic vanadium dioxide powder by ball milling reduction, which overcomes the VO2 powder existing in the prior art. 2 (M) The long reaction time of the powder preparation method is not conducive to industrial production, the reaction is poor in environmental protection, and the energy consumption is large.

Method used

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  • A method for preparing monoclinic phase vanadium dioxide powder by ball milling reduction
  • A method for preparing monoclinic phase vanadium dioxide powder by ball milling reduction
  • A method for preparing monoclinic phase vanadium dioxide powder by ball milling reduction

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Embodiment 1

[0044] A method for preparing monoclinic vanadium dioxide powder by ball milling reduction, comprising the following steps:

[0045] (1) Mix 8.675 g of vanadium pentoxide, 0.569 g of glucose and 2.356 g of amyl acetate to obtain a mixed batch.

[0046] (2) Grinding: Add the mixed ingredients into a ball mill jar, add 88 g of stainless steel grinding balls, and grind for 2 hours at a rotational speed of 1000 r / min.

[0047] (3) Retrieving material: Use a key to scrape the grinding material in the ball mill tank.

[0048] (4) Washing: transfer the grinding material to a 50ml beaker, add 30ml deionized water, stir magnetically for 5min, transfer to a centrifuge at a speed of 3000r / min, centrifuge for 10min, wash twice with deionized water and once with ethanol.

[0049] (5) Drying: put the above-mentioned washing materials in a constant temperature oven and bake at 60°C for 10 hours to remove residual ethanol, and grind with a mortar to obtain a powder.

[0050] The prepared po...

Embodiment 2

[0052] A method for preparing monoclinic vanadium dioxide powder by ball milling reduction, comprising the following steps:

[0053] (1) Ingredients: use vanadium pentoxide, activated carbon, and oleic acid as raw materials, wherein, 8.235g of vanadium pentoxide, 1.232g of activated carbon, and 2.324g of oleic acid.

[0054] (2) Grinding: Add the mixed ingredients into a ball mill jar, add 89 g of stainless steel grinding balls, and grind for 2 hours at a rotational speed of 1000 r / min.

[0055] (3) Retrieving material: Use a key to scrape the grinding material in the ball mill tank.

[0056] (4) Washing: transfer the grinding material to a 50ml beaker, add 30ml of ethanol, magnetically stir for 5min, transfer to a centrifuge at a speed of 3000r / min, centrifuge for 10min, and wash with ethanol three times.

[0057] (5) Drying: put the above-mentioned washing materials in a constant temperature oven and bake at 60° C. for 10 h, remove absolute ethanol, and grind with a mortar ...

Embodiment 3

[0060] A method for preparing monoclinic vanadium dioxide powder by ball milling reduction, comprising the following steps:

[0061] (1) Ingredients: Mix 9.564g of vanadium pentoxide, 0.789g of fructose, and 1.213g of butyric acid to obtain a mixed ingredient.

[0062] (2) Grinding: Add the mixed ingredients into a ball mill jar, add 100 g of cemented carbide grinding balls, and grind for 1 hour at a rotational speed of 1000 r / min.

[0063] (3) Retrieving material: Use a key to scrape the grinding material in the ball mill tank.

[0064] (4) Washing: transfer the grinding material to a 100ml beaker, add 50ml deionized water, stir magnetically for 5min, transfer to a centrifuge at a speed of 3000r / min, centrifuge for 10min, wash twice with deionized water and once with ethanol.

[0065] (5) Drying: Put the above-mentioned washing materials in a constant temperature oven and bake at 60°C for 10 hours to remove residual ethanol and grind them with a mortar to obtain a powder. Th...

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Abstract

The invention provides a method for preparing monoclinic vanadium dioxide powder by ball milling reduction, which belongs to the field of vanadium dioxide powder preparation. The method comprises the following steps: 1) mixing a vanadium source, a reducing agent and a grinding aid to obtain a mixed ingredient; 2) adding the mixed ingredient to a ball milling device, and adding grinding balls for grinding; 3) grinding the material in step 2) Take out, wash and dry to obtain monoclinic phase vanadium dioxide powder. Ball milling method of the present invention prepares VO 2 (M), causing a redox reaction between the vanadium source and the reducing agent under mechanochemical action. During the continuous ball milling process, the grinding balls produce shearing and squeezing forces on the materials, which can continuously reduce the particle size of the materials.

Description

technical field [0001] The invention belongs to the field of vanadium dioxide powder preparation, and in particular relates to a method for preparing monoclinic phase vanadium dioxide powder by ball milling reduction. Background technique [0002] Vanadium dioxide (VO 2 ) is a polymorphic transition metal oxide, in which the monoclinic phase VO 2 (M) An insulator-metal phase transition occurs at about 68°C, accompanied by sudden changes in physical properties such as resistivity and infrared transmittance, making this material applicable to memory storage, smart switches, microbolometers, laser protection and other fields. [0003] Currently, one-step preparation of VO 2 (M) The method of powder mainly includes combustion method, hydrothermal method and so on. Chinese patent CN108975401A discloses a one-step hydrothermal preparation of VO 2 (M) Powder method. In this patent, oxalic acid and vanadium sources are added to deionized water, stirred at a constant temperature ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/02B82Y30/00B82Y40/00
CPCC01G31/02B82Y30/00B82Y40/00C01P2002/72C01P2002/88C01P2002/85C01P2004/03C01P2004/04C01P2004/64C01P2004/62C01P2006/80
Inventor 蒋绪川王驰元徐慧妍聂永王程
Owner 蒋绪川