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Ultra-long one-dimensional dihalogen tungsten dioxide material and preparation method thereof

A technology of tungsten dioxide and tungsten halide, applied in chemical instruments and methods, inorganic chemistry, tungsten compounds, etc., can solve problems such as high temperature and small long diameter, and achieve the effect of stable supply and lower temperature

Pending Publication Date: 2022-05-13
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide an ultra-long one-dimensional dihalogen dioxide A tungsten material and a preparation method thereof, the method can prepare a one-dimensional dihalogenated tungsten dioxide material with millimeter-scale length, high crystallinity, and uniform element distribution, and the obtained one-dimensional material can be used to prepare one-dimensional WO 3 and one-dimensional metal tungsten, widely used in catalysis, high-performance electronic devices and other fields

Method used

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  • Ultra-long one-dimensional dihalogen tungsten dioxide material and preparation method thereof
  • Ultra-long one-dimensional dihalogen tungsten dioxide material and preparation method thereof
  • Ultra-long one-dimensional dihalogen tungsten dioxide material and preparation method thereof

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Embodiment 1

[0023](1) Cut a silicon wafer with a size of 1cm×1cm with a silicon wafer knife, ultrasonically clean it with acetone, ethanol, and deionized water for 5 minutes and dry it with an argon stream, and place it at a suitable position downstream of the tube furnace; weigh it in a glove box. Take 20mg of WCl 6 The powder is placed in the middle of the tube furnace tube; connect all parts of the CVD system to ensure good airtightness. Such as figure 1 Shown is a schematic diagram of the chemical vapor deposition device used in the experiment

[0024] (2) Turn on the vacuum pump to evacuate the system to vacuum; mix argon and air in the gas mixing system at a ratio of 2:3, and then pass it into the vacuum system with a total flow rate of 50 sccm; adjust the valve of the vacuum pump to make the system pressure It reaches 550Pa and remains stable.

[0025] (3) Start the tube furnace and heat it to 300°C at a heating rate of 10°C / s and keep it warm for 30 minutes. After the reaction ...

Embodiment 2

[0029] (1) Cut a silicon wafer with a size of 1cm×1cm with a silicon wafer knife, ultrasonically clean it with acetone, ethanol, and deionized water for 5 minutes and dry it with an argon stream, and place it at a suitable position downstream of the tube furnace; weigh it in a glove box. Take 50mg of WCl 6 The powder is placed in the middle of the tube furnace tube; connect all parts of the CVD system to ensure good airtightness. Such as figure 1 Shown is a schematic diagram of the chemical vapor deposition device used in the experiment

[0030] (2) Turn on the vacuum pump to evacuate the system to vacuum; mix argon and air at a ratio of 2:3 in the gas mixing system, and then pass it into the vacuum system with a total flow rate of 300 sccm; adjust the valve of the vacuum pump to make the system pressure It reaches 550Pa and remains stable.

[0031] (3) Start the tube furnace and heat it to 300°C at a heating rate of 10°C / s and keep it warm for 30 minutes. After the reactio...

Embodiment 3

[0033] (1) Cut a silicon wafer with a size of 1cm×1cm with a silicon wafer knife, ultrasonically clean it with acetone, ethanol, and deionized water for 5 minutes and dry it with an argon stream, and place it at a suitable position downstream of the tube furnace; weigh it in a glove box. Take 20mg of WCl 6 The powder is placed in the middle of the tube furnace tube; connect all parts of the CVD system to ensure good airtightness. Such as figure 1 Shown is a schematic diagram of the chemical vapor deposition device used in the experiment

[0034] (2) Turn on the vacuum pump and evacuate the system to a vacuum; Compressed air is passed into the vacuum system with a total flow of 50 sccm; the valve of the vacuum pump is adjusted to make the system pressure reach 10 5 Pa and remain stable.

[0035] (3) Start the tube furnace to heat up to 500°C at a heating rate of 10°C / s and keep it warm for 30 minutes. After the reaction is over, turn off the electric furnace, vacuum pump and...

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Abstract

The invention discloses an ultra-long one-dimensional dihalogen tungsten dioxide material and a preparation method thereof. A chemical vapor deposition method and a limited oxidation technology are utilized to control the morphology, crystallinity and oxidation degree of the one-dimensional dihalogenotungsten dioxide material by changing pressure, temperature, carrier gas components, flow and the like, so that the one-dimensional dihalogenotungsten dioxide material with the length of 0.4-5mm and the diameter of 0.2-5mu m is obtained. The method has the advantages of low raw material cost, low energy consumption, simple process, good parameter controllability, high yield, high product purity and easiness in realization of industrial large-scale production. According to the method, the one-dimensional tungsten dioxide dihalide material with millimeter-scale length, high crystallinity and uniform element distribution can be prepared, and the obtained material can be further prepared into ultra-long one-dimensional tungsten oxide and one-dimensional metal tungsten microwires through a subsequent oxidation-reduction process; the product can be widely used in the fields of catalysis, storage, gas sensitivity, electrochromism, photoelectric induction and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of low-dimensional functional materials, and in particular relates to an ultra-long one-dimensional dihalogenated tungsten dioxide material and a preparation method thereof. Background technique [0002] With the development of science and technology, transition metal oxides have aroused the research interests of many scientists due to their unique physical and chemical properties. Tungsten oxide is a wide bandgap n-type semiconductor material with a bandgap of 2.6-3.0eV. It has a wide range of applications in the fields of catalysis, sensor preparation and electrochromism. It is currently the most studied transition metal oxide. Tungsten oxide crystal 6 Octahedron is the basic structural unit, and can form monoclinic, triclinic, square, cubic and hexagonal crystal structures at different temperatures. Tungsten oxide has stable chemical properties and is insoluble in inorganic acids except h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00
CPCC01G41/00C01P2002/72C01P2004/03
Inventor 李芳菲刘道昕薛兵徐志强
Owner JILIN UNIV
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