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Hydrothermal synthesis method of monoclinic phase vanadium dioxide nano-powder

A vanadium dioxide nano, hydrothermal synthesis technology, applied in the field of photocatalytic materials, can solve the problems of complex preparation process, difficult control, unfavorable synthesis product repeatability and mass production, and achieve high chemical activity and large specific surface area Effect

Inactive Publication Date: 2020-02-07
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the size of these nanomaterials is still relatively large, all on the scale of 100 nm or even microns; and various raw materials such as vanadium sources, reducing agents, and complexing agents need to be added during the synthesis process, because the morphology of nanomaterials is very sensitive to synthesis conditions , the more variables, the more difficult it is to control, the more complicated the preparation process is, which is not conducive to the repeatability and mass production of synthetic products

Method used

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Embodiment 1

[0031] At room temperature, 2.2 g of ammonium dioxalate dioxovanadate complex was dissolved in 50 mL of deionized water and transferred to a reaction kettle for hydrothermal crystallization. The heating rate in the reactor was 5°C min -1 (that is, increase by 5°C per minute), keep at a constant temperature of 180°C for 20 hours, then naturally cool to room temperature and take it out; after washing with alcohol, dry it in an environment of 60±1°C to obtain monoclinic vanadium dioxide nanopowder body.

[0032] figure 1 It is the VO of embodiment one hydrothermal synthesis 2 The XRD pattern of nanoparticles (that is, monoclinic vanadium dioxide nanopowder) shows that it has a monoclinic C2 / m(12) structure. figure 2 It is the VO of embodiment one hydrothermal synthesis 2 TEM photo of nanoparticles, VO can be seen from the small black dots in the picture 2 The shape of the nanoparticle is about 1-2 nanometers in diameter.

Embodiment 2

[0034] At room temperature, 2.2 g of ammonium dioxalate dioxovanadate complex was dissolved in 30 mL of deionized water, transferred to a reaction kettle for hydrothermal crystallization. Heating rate is 5°C min -1 , kept at 180°C for 20 h, then cooled naturally to room temperature and taken out. After alcohol washing, dry at 60±1°C to obtain monoclinic phase vanadium dioxide nanopowder.

[0035] image 3 It is the VO of embodiment two hydrothermal synthesis 2 TEM photo of nanoparticles, VO can be seen from the small black dots in the picture 2 The shape of the nanoparticle is still about 1-2 nanometers in diameter. It shows that changing the concentration of the raw material solution within a certain range has little effect on the shape and size of the synthesized nanoparticles, which is beneficial to the repeated preparation and mass production of the product.

Embodiment 3

[0037] Take 2.2 g of ammonium dioxalate dioxovanadate complex and dissolve it in 50 mL of deionized water, transfer it to a reaction kettle for hydrothermal crystallization. Heating rate is 5°C min -1 , kept at 200°C for 20 h, then cooled naturally to room temperature and taken out. After alcohol washing, dry at 60±1°C to obtain monoclinic phase vanadium dioxide nanopowder.

[0038] Figure 4 It is the VO of embodiment three hydrothermal synthesis 2 TEM photo of nanoparticles, VO can be seen from the small black dots in the picture 2 The shape of the nanoparticle is still about 1-2 nanometers in diameter. It shows that changing the hydrothermal temperature within a certain range has little effect on the morphology and size of the synthesized nanoparticles, which is beneficial to the repeated preparation and mass production of products.

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Abstract

The invention discloses a hydrothermal synthesis method of monoclinic phase vanadium dioxide nano-powder. The hydrothermal synthesis method is characterized in that X is a real number; the method comprises the following steps: dissolving: dissolving X g of an ammonium dioxo vanadate complex in 13.64 X-22.73 X mL of deionized water at normal temperature; 2, carrying out hydrothermal crystallization: transferring the solution obtained in the first step into a reaction kettle, and carrying out hydrothermal crystallization; heating in the reaction kettle at a heating rate of 5 DEG C / min, keeping the temperature for 20 hours at a constant temperature of 180-200 DEG C, and then naturally cooling to room temperature; and 3, alcohol washing and drying: taking out a product obtained in the second step from the reaction kettle, washing with alcohol, and drying in an environment of 60 + / -1 DEG C to obtain the monoclinic phase vanadium dioxide nano-powder. According to the method, the synthesis process can be more easily controlled, the monoclinic phase vanadium dioxide nano-powder can be repeatedly produced on a large scale, and the final product has higher chemical activity, catalytic activity and adsorption activity.

Description

technical field [0001] The invention relates to an inorganic chemical synthesis technology, in particular to a hydrothermal synthesis method of a monoclinic phase vanadium dioxide nanopowder, and the vanadium dioxide nanopowder can be applied to the fields of photocatalytic materials and the like. Background technique [0002] VO 2 It is a typical thermochromic material. Due to its unique properties, it has a very rich application value in the fields of smart windows, photoelectric switches, optical storage devices, thermistors, and infrared radiation detection. VO 2 The powder can be directly pressed into a device, or it can be formed into a film alone or together with an organic medium, which is more convenient for application. [0003] In recent years, the research on vanadium dioxide powder has become a hot spot. VO 2 It is a blue-black solid, and its energy band structure makes it have strong absorption in the visible light band, which can be used for photocatalytic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G31/02C01P2004/64
Inventor 申万岭李新
Owner HENAN UNIVERSITY OF TECHNOLOGY
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