A spherical W 18 O 49 Method for producing a material

Abstract

This invention relates to a spherical W 18 O 49 The material was prepared by dissolving 100-500 mg of WCl6 in 100 ml of anhydrous ethanol, transferring the solution to the lining of a stirred reactor, and stirring at 100-400 rpm while purging with argon gas for 10-30 minutes. The reaction was maintained at 140-200℃ for 18-24 hours. After the reaction, the reactor was cooled to room temperature, and the resulting blue precipitate was repeatedly washed with anhydrous ethanol by centrifugation. Finally, it was vacuum dried in a vacuum drying oven at 60℃ for 24 hours to obtain spherical WCl6. 18 O 49 This invention solves the problem of uneven sample morphology synthesized by conventional hydrothermal methods, and synthesizes a new W... 18 O 49 Morphology. The prepared W 18 O 49 With uniform morphology and clean surface, it can be combined with other photocatalytic materials to achieve good photocatalytic performance, and can also be used to assemble two-dimensional and three-dimensional ordered arrays to prepare metamaterials.

Description

TECHNICAL FIELD

[0001] The present application relates to a spherical W 18 O 49 The preparation method of the material belongs to the technical field of materials. BACKGROUND

[0002] Since the photocatalytic performance of semiconductor TiO2 was first discovered in 1972, photocatalytic technology has developed rapidly. Photocatalytic technology can convert solar energy into new energy such as hydrogen energy under mild conditions without secondary pollution, and can also convert organic pollutants, CO2 and the like in the environment into environmentally friendly products, and therefore has been widely concerned.

[0003] The full solar spectrum includes ultraviolet, visible and infrared. Common photocatalysts can only absorb energy in the ultraviolet region due to their wide band gap, and cannot fully utilize solar energy, limiting their application in photocatalysis. W 18 O 49 Due to its unique structural characteristics and high carrier concentration, especially due to the strong near-infrared absorption induced by its own LSPR effect, it has attracted people's attention. W 18 O 49 The light absorption capacity of W is closely related to its morphology, and the strength of the light absorption capacity determines the photocatalytic activity. Therefore, the morphology of W 18 O 49 plays an important role in photocatalytic performance. Compared with one-dimensional and two-dimensional nanostructures, three-dimensional structures have the characteristics of strong light absorption capacity and multiple carrier migration paths. In addition, the acquisition of uniform spherical W 18 O 49 can effectively expand the application range of its LSPR effect, and make it play an important role in the field of super materials such as photonic crystals. The present application adopts a method of stirring hydrothermal synthesis in an argon environment to synthesize spherical W 18 O 49 material.

[0004] Currently, W 18 O 49 is usually synthesized by simple static hydrothermal method at a certain temperature. During the synthesis process, the morphology of the reaction product is not uniform due to the inability to accurately control the internal conditions of the reaction kettle such as atmosphere. SUMMARY

[0005] The present application solves the problem of non-uniform morphology of materials prepared by ordinary static hydrothermal method by controlling the atmosphere inside the reaction kettle, the stirring rate of the reactants and the like. And a new morphology of W 18 O 49 material is synthesized and prepared.

[0006] The present application proposes a spherical W 18 O49 The preparation method of the material is that 100-500 mg WCl6 is dissolved in 100 ml anhydrous ethanol, transferred to the inner liner of a stirring reaction kettle, stirred under the rotation speed of 100-400 / min, and argon is passed for 10-30 min. The reaction is kept at 140℃-200℃ for 18-24 h. After the reaction is completed, the reaction kettle is cooled to room temperature, and the obtained blue precipitate is repeatedly centrifuged and washed with anhydrous ethanol. Finally, vacuum drying is carried out at 60℃ in a vacuum drying box for 24 h, and finally spherical W 18 O 49 .

[0007] The present application has the beneficial effects compared with the prior art:

[0008] The present application solves the problem of uneven morphology of the sample synthesized by the ordinary hydrothermal method, and synthesizes a new W 18 O 49 The prepared W 18 O 49 The morphology is uniform, the surface is clean, and the WO4 can be compounded with other photocatalytic materials to achieve better photocatalytic performance. This spherical particle is especially suitable for assembling into a two-dimensional or three-dimensional ordered array, so as to prepare a metamaterial with rich optical properties. BRIEF DESCRIPTION OF DRAWINGS

[0009] Figure 1 The XRD patterns of WO4 synthesized at different temperatures. 18 O 49

[0010] Figure 2 The SEM image of WO4 synthesized at 1 μm and 200℃. 18 O 49

[0011] Figure 3 The SEM image of WO4 synthesized at 200 nm and 200℃. 18 O 49

[0012] Figure 4 The DRS patterns of WO4 synthesized at different temperatures. 18 O 49 DETAILED DESCRIPTION

[0013] ​​​​Example 1. 500 mg of WCl6was dissolved in 100 ml of absolute ethanol. It was then transferred to the inner liner of a stirred reaction kettle, the stirring rate was set to 400 rpm, and argon was bubbled through the stirred solution for 30 minutes. The stirring rate was then kept constant and the reaction was carried out at 160 °C for 24 hours. After the reaction was completed, the reaction kettle was allowed to cool to room temperature, and the resulting blue precipitate was repeatedly washed by centrifugation with absolute ethanol three times to remove the impurities in the product. Finally, it was vacuum dried in a vacuum drying oven at 60 °C for 24 h to obtain W 18 O 49 .

[0014] Example 2. 500 mg of WCl6was dissolved in 100 ml of absolute ethanol. It was then transferred to the inner liner of a stirred reaction kettle, the stirring rate was set to 400 rpm, and argon was bubbled through the stirred solution for 30 minutes. The stirring rate was then kept constant and the reaction was carried out at 180 °C for 24 hours. After the reaction was completed, the reaction kettle was allowed to cool to room temperature, and the resulting blue precipitate was repeatedly washed by centrifugation with absolute ethanol three times to remove the impurities in the product. Finally, it was vacuum dried in a vacuum drying oven at 60 °C for 24 h to obtain W 18 O 49 .

[0015] Example 3. 500 mg of WCl6was dissolved in 100 ml of absolute ethanol. It was then transferred to the inner liner of a stirred reaction kettle, the stirring rate was set to 400 rpm, and argon was bubbled through the stirred solution for 30 minutes. The stirring rate was then kept constant and the reaction was carried out at 200 °C for 24 hours. After the reaction was completed, the reaction kettle was allowed to cool to room temperature, and the resulting blue precipitate was repeatedly washed by centrifugation with absolute ethanol three times to remove the impurities in the product. Finally, it was vacuum dried in a vacuum drying oven at 60 °C for 24 h to obtain W 18 O 49 .

[0016] Example 4. 100 mg of WCl6was dissolved in 100 ml of absolute ethanol. It was then transferred to the inner liner of a stirred reaction kettle, the stirring rate was set to 400 rpm, and argon was bubbled through the stirred solution for 30 minutes. The stirring rate was then kept constant and the reaction was carried out at 160 °C for 24 hours. After the reaction was completed, the reaction kettle was allowed to cool to room temperature, and the resulting blue precipitate was repeatedly washed by centrifugation with absolute ethanol three times to remove the impurities in the product. Finally, it was vacuum dried in a vacuum drying oven at 60 °C for 24 h to obtain W 18 O 49 .

[0017] Example 5. 100 mg of WCl6 was dissolved in 100 ml of anhydrous ethanol. The solution was then transferred to a stirred reactor liner, and the stirring speed was adjusted to 400 rpm. Argon gas was passed through the reactor for 30 minutes with stirring. The stirring speed was then maintained, and the reaction was carried out at 140 °C for 24 hours. After the reaction, the reactor was cooled to room temperature, and the resulting blue precipitate was repeatedly washed three times with anhydrous ethanol by centrifugation to remove impurities. Finally, the precipitate was vacuum dried at 60 °C for 24 hours to obtain WCl6. 18 O 49 .

[0018] Example 6. 100 mg of WCl6 was dissolved in 100 ml of anhydrous ethanol. The solution was then transferred to a stirred reactor liner, and the stirring speed was adjusted to 400 rpm. Argon gas was passed through the reactor for 20 minutes with stirring. The stirring speed was then maintained, and the reaction was carried out at 200 °C for 18 hours. After the reaction, the reactor was cooled to room temperature, and the resulting blue precipitate was washed three times by centrifugation with anhydrous ethanol to remove impurities. Finally, the precipitate was dried under vacuum at 60 °C for 24 hours to obtain WCl6. 18 O 49 .

[0019] Example 7. 500 mg of WCl6 was dissolved in 100 ml of anhydrous ethanol. The solution was then transferred to a stirred reactor liner, and the stirring speed was adjusted to 200 rpm. Argon gas was passed through the reactor for 10 minutes while stirring. The stirring speed was then maintained, and the reaction was carried out at 200 °C for 24 hours. After the reaction, the reactor was cooled to room temperature, and the resulting blue precipitate was washed three times by centrifugation with anhydrous ethanol to remove impurities. Finally, the precipitate was dried under vacuum at 60 °C for 24 hours to obtain WCl6. 18 O 49 .

[0020] The following experiments were used to verify the effectiveness of the invention:

[0021] This invention provides a spherical W 18 O 49 The spherical W-shaped material prepared by the material preparation method 18 O 49 The materials were characterized by XRD. Figure 1 ), scanning electron microscope ( Figure 2 , Figure 3 ) and DRS characterization ( Figure 4 ). Spherical W-shaped samples prepared at different temperatures 18 O 49 The characteristic peak positions of the material and W 18 O 49 The material XRD standard card is consistent. Figure 2 and Figure 3 spherical W 18 O 49The material scanning electron microscope image, obviously visible formed uniform spherical W 18 O 49 Material. Figure 4 It is shown that due to LSPR spherical W 18 O 49 The material has long wavelength absorption.

Claims

1. A spherical W 18 O 49 Method for the production of a material, characterized in that: Dissolve 100-500 mg WCl6in 100 ml anhydrous ethanol, transfer into the inner liner of the stirred reaction kettle, and stir under argon at a rotation speed of 100-400 r / min for 10-30 min; keep the temperature at 140-200 °C and react for 18-24 h; after the reaction is completed, cool the reaction kettle to room temperature, and repeatedly centrifuge and wash the obtained blue precipitate with anhydrous ethanol; finally, vacuum dry at 60 °C for 24 h in a vacuum drying box to obtain spherical WO3 18 O 49 .

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