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Preparation method of tungsten bronze profile

A technology of tungsten bronze and hydrogen tungsten bronze, applied in the field of preparation of tungsten bronze type materials, can solve the problems of limited amount of single synthesis, high energy consumption of mechanical ball milling, and restriction of wide application, etc., achieving simple equipment and long synthesis cycle. , the effect of easy operation

Active Publication Date: 2019-03-12
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are some preparation methods for the preparation of hydrogen tungsten bronze, but the amount of single synthesis is limited, and the reaction conditions are harsh. For example, the hydrothermal synthesis method takes a long time, requires high temperature and high pressure conditions during the reaction process, consumes a lot of energy and has poor repeatability.
The mechanical ball milling method consumes a lot of energy and has disadvantages such as uneven composition
Therefore, there is still a lack of a cheap, reliable and stable industrial synthesis method for the synthesis of pure hydrogen tungsten bronze, which has become a bottleneck restricting its wide application

Method used

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  • Preparation method of tungsten bronze profile
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  • Preparation method of tungsten bronze profile

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] This embodiment provides a tungsten bronze material, the preparation method is as follows:

[0037] 100nm WO 3 The powder and liquid metal (Ga 75.5%, In 24.5%) and hydrochloric acid, the pH value is 0.3, are mixed according to the mass ratio of 1:5:5, the temperature of the mixed solution is selected as 20 ℃, and put into a polyethylene centrifuge tube Vibration and mixing, the choice of vibration mixing is to vibrate on a disc vibrator for 2 minutes. The prepared mixture first separates the liquid metal from the mixed solution, and the separated liquid metal is placed in 1mol / L hydrochloric acid for recycling. The separated powder is mixed with hydrochloric acid. The mixed solution was centrifuged with a centrifuge, and the powder obtained after centrifugation was washed with alcohol, deionized water, and alcohol in sequence. After cleaning, the hydrogen tungsten bronze was placed in a vacuum drying oven and dried at 20°C for 30 minutes. See attached for vibration pre...

Embodiment 2

[0039] This embodiment provides a tungsten bronze material, the preparation method is as follows:

[0040] 50nmWO 3 The powder and liquid metal (Ga 75.5%, In 24.5%) and hydrochloric acid, the pH value is 0, are mixed according to the mass ratio of 2:5:2, the temperature of the mixed solution is selected as 40 ° C, and put into a polyethylene centrifuge tube Vibration and mixing, the choice of vibration mixing is to vibrate on a disc vibrator for 1min. The prepared mixture first separates the liquid metal from the mixed solution, and the separated liquid metal is placed in 1mol / L hydrochloric acid for recycling. The separated powder is mixed with hydrochloric acid. The mixed solution was centrifuged with a centrifuge, and the powder obtained after centrifugation was washed with alcohol, deionized water, and alcohol in sequence. After cleaning, the hydrogen tungsten bronze powder was placed in a vacuum drying oven and dried at 40°C for 20 minutes. The SEM image of the prepared ...

Embodiment 3

[0042] This embodiment provides a tungsten bronze material, the preparation method is as follows:

[0043] 50nmWO 3 The powder is mixed with Ga 67%, In 20.5%, Sn 12.5% ​​and hydrochloric acid, the pH value is 0, according to the mass ratio of 1:5:10, the temperature of the mixed solution is selected as 60 ° C, and put into a polyethylene centrifuge tube Medium vibration mixing, vibration mixing is selected as vibration on a disc vibrator for 5 minutes, the prepared mixture is first separated from the liquid metal and the mixed solution, the separated liquid metal is placed in 1mol / L hydrochloric acid for recycling, and the separated powder is mixed with hydrochloric acid The mixed solution was centrifuged with a centrifuge, and the powder obtained after centrifugation was washed with alcohol, deionized water, and alcohol in sequence, and the hydrogen tungsten bronze powder of the cleaned thickness was placed in a vacuum drying oven and dried at 60°C for 5 minutes. The macrosc...

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Abstract

The invention provides a preparation method of a tungsten bronze profile. The preparation method comprises the following steps of S1, mixing MO3-n powder and gallium-based liquid metal, adding acid with a pH value smaller than or equal to 5, and performing reaction at a room temperature to obtain a mixed solution; and S2, collecting powder in the mixed solution, performing washing to remove acid radical ions in the powder, and performing vacuum drying to obtain the tungsten bronze profile, wherein in MO3-n, M is W or Mo, and n is smaller than or equal to 0.28. In the preparation method, a preparation environment is the room temperature, a reducer is the liquid metal, and a hydrogen ion source is acid, so that synthesis of the tungsten bronze profile can be realized without any atmosphere and high temperature, and use of vacuum or sealing capacity is thoroughly avoided.

Description

technical field [0001] The invention relates to the technical field of preparation of oxide materials, and more specifically, to a preparation method of tungsten bronze-type materials. Background technique [0002] Tungsten bronze or molybdenum bronze materials have a bronze-like color and brightness, so compounds with similar structures are called tungsten bronze materials. Hydrogen tungsten bronze (H x WO 3 ) and hydrogen molybdenum bronze (H x MoO 3 ) material is a typical tungsten hydride copper oxide semiconductor material, through WO 3 or MoO 3 The unique tunnel structure of the crystal is doped with hydrogen ions, and the prepared hydrogen tungsten bronze is a hydrogen ion-doped metal oxide with high stability and dark blue metallic luster, showing the properties of metal conductors or semiconductors. Its color and performance can be adjusted by different parameters. It has attracted widespread attention for its good energy storage, photocatalysis, photo / gas / el...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00
CPCC01G41/00
Inventor 崔云涛刘静
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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