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Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame

A VO2, monoclinic phase technology, applied in vanadium oxide and other directions, can solve the problems of too high reaction temperature, harsh requirements, complicated equipment, etc., and achieve the effect of simple reaction process and equipment, easy industrialization, and excellent performance.

Active Publication Date: 2013-12-25
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, there are two main methods for preparing vanadium dioxide powder as a smart window material: one is vapor deposition of VO2 under the protection of hydrogen or inert atmosphere. 2 (M), but this method requires harsh conditions, complex equipment, high cost and difficult to control the valence state of vanadium in it, and it is difficult to obtain pure phase VO 2 (M)
The other is to use V at high temperature 2 o 5 and V 2 o 3 Quantitative reaction or decomposition of complex precursors to prepare, but the reaction temperature is too high, generally above 700-800 ° C, the reaction measurement is difficult to control, and the product is very impure

Method used

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  • Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame
  • Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame
  • Method for preparing monoclinic-phase VO2 (vanadium dioxide) by utilizing lean flame

Examples

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preparation example Construction

[0021] h 2 V 3 o 8 The preparation method: add 53mg VO(acac) to a polytetrafluoroethylene kettle with a volume of 55ml 2 and 50ml of distilled water, then keep the reaction kettle in a high-temperature furnace at 90°C for 30 minutes, then take out the reaction kettle and stir to allow it to cool naturally, then add 0.2ml of HCl with a concentration of 1M, and continue stirring for ten minutes to obtain a yellow-green solution. Then put the reaction kettle into a metal shell, place it in a high-temperature furnace at 200°C for 12 hours, and after natural cooling, centrifuge the obtained precipitate, wash it with distilled water and absolute ethanol three times, and then keep it in a vacuum oven at 60°C for 6 hours , to obtain a dry gray-green flake sample, which is H 2 V 3 o 8 .

[0022] VOCs 2 o 4 The preparation method: add 4mmol V to a volumetric flask with a volume of 100ml 2 o 5 , 9 mmol H 2 C 2 o 4 and 20ml of distilled water, then reflux in an oil bath at 70...

Embodiment 1

[0029] After adding 50ml of absolute ethanol to a 100ml glass beaker with a built-in glass stake of 4.5cm in height, 80mg of V 2 o 5 , NH 4 VO 3 、H 2 V 3 o 8 、VOSO 4 、VO(acac) 2 、VOC 2 o 4 、VO 2 (A), VO2 (B), VO 2 (paramontroseite), V 2 o 3 , VOOH and V(OH) 2 NH 2 spread the powder on a common glass sheet, place the glass sheet on a glass stake, ignite the absolute ethanol in an air atmosphere, so that the above-mentioned vanadium-containing compound is always in the rich flame of the ethanol, and Without contact with the air, after burning for 45 minutes, cover the alcohol flame with a watch glass, collect the sample on the glass piece after cooling, wash and dry to get VO 2 (M) Powder.

[0030] figure 1 The resulting product VO was prepared for this Example 1 2 (M) XRD pattern, figure 2 The resulting product VO was prepared for this example 2 (M) DSC characterization. From the above detection results, it can be seen that the structure of the obtained pr...

Embodiment 2

[0032] After adding 2ml of absolute ethanol to a 100ml beaker with a connecting device, then put a wire shelf with a height of 3.5cm into the beaker, and put 80mg of V 2 o 5 Powder and NH 4 VO 3 Spread the powder on an ordinary glass sheet, put the glass sheet on the wire shelf in the beaker, ignite the absolute ethanol in the air atmosphere, so that the above-mentioned vanadium-containing compound is always in the rich flame of the ethanol without contact with the air, after burning for 1 hour, cover the alcohol flame with a watch glass, collect the sample on the glass slide after cooling, wash and dry to get VO 2 (M) Powder.

[0033] image 3 Prepare the XRD collection of illustrative plates and the DSC characterization of the product obtained for this embodiment, as can be seen from the above detection results, the product structure obtained is correct, is VO 2 (M), and the purity is 99%.

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Abstract

The invention discloses a method for preparing a monoclinic-phase VO2 (vanadium dioxide) and doped powder of monoclinic-phase VO2 by utilizing lean flame, and the method comprises the following steps of: placing a vanadium-containing compound or the vanadium-containing compound doped with a metal element in the lean flame of an organic solvent to carry out a reaction, and cooling to obtain the monoclinic-phase VO2 after the reaction is completed. According to the method, the solid-phase powder of a vanadium-containing raw material is directly arranged in the flame of an organic solvent such as ethanol and the like to react; the reaction process and equipment are quite simple; and the method is a simple and efficient method which can be industrialized easily for preparing VO2 (M) (metal) which is an intelligent window material. The VO2 (M) and the doped powder of VO2 (M), which are prepared by the method, have excellent performances, and are quite important intelligent window materials.

Description

technical field [0001] The invention belongs to the technical field of flame method preparation, and relates to a method for preparing monoclinic VO by using a rich combustion flame. 2 Methods. Background technique [0002] Among various smart window materials, VO with metal-insulator phase transition characteristics 2 (M) has been receiving extensive attention from both academia and industry due to the optimum phase transition temperature. [0003] VO 2 (M)(Monoclinic VO 2 ) is an infrared-transmissive monoclinic insulating phase at low temperature. With the increase of ambient temperature, when the 2 (M) transforms into an infrared-blocking tetragonal metallic phase (rutile phase), during which VO 2 The conductivity of (M) also occurs 10 5 change of magnitude. These properties make VO 2 (M) has broad application prospects in the fields of photoelectric conversion devices and solar smart windows. At the same time, if in VO 2 (M) is mixed with a proper amount of W,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/02
Inventor 谢毅白亮飞宋磊
Owner UNIV OF SCI & TECH OF CHINA