a kind of wo 3 Preparation method and application of nanosheet array thin film

Abstract

The invention discloses a preparation technology of a visible-light response WO3 nanosheet array film electrode. The preparation technology comprises the following steps that Na2WO4.2H2O and ammonium oxalate are dissolved in deionized water to react with hydrochloric acid to obtain tungstic acid precipitates, and the tungstic acid precipitates react with H2O2 to obtain a clear peroxotungstic acid solution; an ethyl alcohol reducing agent is added into the peroxotungstic acid solution, fluorine-doped tin oxide (FTO) conducting glass serves as a substrate to be placed in the solution, under the water bath condition, the peroxotungstic acid is slowly reduced into tungstic acid, the tungstic acid is slowly separated out on an FTO film, and then a tungstic acid film is obtained; after being cleaned and dried, the tungstic acid film is calcined to obtain the WO3 nanosheet array film electrode. The preparation technology has the advantages of being simple, convenient, mild, efficient and suitable for large-scale preparation. The prepared WO3 nanosheet array film electrode has the good visible-light absorption property and good stability and is high in photoelectric efficiency, good in photoelectrocatalytic degradation effect on organic matter and capable of being applied to the fields of photoelectrocatalysis hydrogen production and organic matter degradation, and the better effect is achieved.

Description

technical field

[0001] The invention relates to a photoelectrocatalytic electrode material, in particular to a visible light-responsive WO 3 The invention relates to a preparation process of a nanosheet array thin film photoelectric catalysis electrode, which belongs to the field of nanometer materials. technical background

[0002] Solar photodegradation of organic matter and hydrogen production based on photocatalytic technology is a new technology with promising application prospects. In this technology, the performance of the photocatalytic electrode directly affects the effect of the photocatalytic system. Therefore, the preparation of photocatalytic electrode materials is a research hotspot in the field of photocatalysis.

[0003] At present, it is generally believed that the characteristics that an excellent photocatalytic electrode should have are: good visible light absorption performance, stable in aqueous solution, non-toxic, easy to prepare, and cheap. Among t...

Examples

Embodiment 1

[0035] 1) Add 0.4g Na 2 WO 4 2H 2 O and 0.15g of ammonium oxalate were dissolved in 30mL of deionized water, and 9mL of 37% hydrochloric acid was added to obtain a yellow tungstic acid precipitate. After stirring for 10 minutes, 8mL of 37% H 2 o 2 , the precipitate was dissolved and a clear peroxytungstic acid solution was obtained. After stirring for 10 minutes, 30 mL of ethanol was added and stirred for another 10 minutes. The fluorine-doped tin oxide (FTO) conductive glass was used as the substrate, and the FTO leaned against the wall with the face down. Water bath at 85°C for 200 minutes, and slowly precipitate tungstic acid on the FTO substrate to obtain a uniform tungstic acid film. The above tungstic acid film is rinsed with deionized water and dried at about 50°C for more than 1 hour;

[0036] 2) heat-treat the dry tungstic acid film obtained in step 1) at a temperature of 500°C for 2 hours, and obtain the WO after natural cooling 3 Nanosheet array thin film electr...

Embodiment 2

[0042] 1) Add 0.2g Na 2 WO 4 2H 2 O and 0.06g of ammonium oxalate were dissolved in 30mL of deionized water, and 5mL of 37% hydrochloric acid was added to obtain a yellow tungstic acid precipitate. After stirring for 10 minutes, 5mL of 37% H 2 o 2 , the precipitate was dissolved and a clear peroxytungstic acid solution was obtained. After stirring for 10 minutes, 30 mL of ethanol was added and stirred for another 10 minutes. The fluorine-doped tin oxide (FTO) conductive glass was used as the substrate, and the FTO leaned against the wall with the face down. Water bath at 95°C for 120 minutes, and slowly precipitate tungstic acid on the FTO substrate to obtain a uniform tungstic acid film. The above tungstic acid film is rinsed with deionized water and dried at about 50°C for more than 1 hour;

[0043] 2) The dried tungstic acid film obtained in step 1) was heat-treated at 400°C for 6h, and the WO was obtained after natural cooling. 3 Nanosheet array thin film electrodes. ...

Embodiment 3

[0046] 1) Add 0.6g Na 2 WO 4 2H 2 O and 0.2g of ammonium oxalate were dissolved in 30mL of deionized water, and 15mL of 37% hydrochloric acid was added to obtain a yellow tungstic acid precipitate. After stirring for 10 minutes, 10mL of 37% H 2 o 2 , the precipitate was dissolved and a clear peroxytungstic acid solution was obtained. After stirring for 10 minutes, 30 mL of ethanol was added and stirred for another 10 minutes. The fluorine-doped tin oxide (FTO) conductive glass was used as the substrate, and the FTO leaned against the wall with the face down. Water bath at 75°C for 220 minutes, and slowly precipitate tungstic acid on the FTO substrate to obtain a uniform tungstic acid film. The above tungstic acid film is rinsed with deionized water and dried at about 50°C for more than 1 hour;

[0047] 2) heat-treat the dried tungstic acid film obtained in step 1) at a temperature of 550°C for 1 hour, and obtain the WO after natural cooling 3 Nanosheet array thin film elec...

technical field

[0001] The invention relates to a photoelectrocatalytic electrode material, in particular to a visible light-responsive WO 3 The invention relates to a preparation process of a nanosheet array thin film photoelectric catalysis electrode, which belongs to the field of nanometer materials. technical background

[0002] Solar photodegradation of organic matter and hydrogen production based on photocatalytic technology is a new technology with promising application prospects. In this technology, the performance of the photocatalytic electrode directly affects the effect of the photocatalytic system. Therefore, the preparation of photocatalytic electrode materials is a research hotspot in the field of photocatalysis.

[0003] At present, it is generally believed that the characteristics that an excellent photocatalytic electrode should have are: good visible light absorption performance, stable in aqueous solution, non-toxic, easy to prepare, and cheap. Among t...

Examples

Embodiment 1

[0035] 1) Add 0.4g Na 2 WO 4 2H 2 O and 0.15g of ammonium oxalate were dissolved in 30mL of deionized water, and 9mL of 37% hydrochloric acid was added to obtain a yellow tungstic acid precipitate. After stirring for 10 minutes, 8mL of 37% H 2 o 2 , the precipitate was dissolved and a clear peroxytungstic acid solution was obtained. After stirring for 10 minutes, 30 mL of ethanol was added and stirred for another 10 minutes. The fluorine-doped tin oxide (FTO) conductive glass was used as the substrate, and the FTO leaned against the wall with the face down. Water bath at 85°C for 200 minutes, and slowly precipitate tungstic acid on the FTO substrate to obtain a uniform tungstic acid film. The above tungstic acid film is rinsed with deionized water and dried at about 50°C for more than 1 hour;

[0036] 2) heat-treat the dry tungstic acid film obtained in step 1) at a temperature of 500°C for 2 hours, and obtain the WO after natural cooling 3 Nanosheet array thin film electr...

Embodiment 2

[0042] 1) Add 0.2g Na 2 WO 4 2H 2 O and 0.06g of ammonium oxalate were dissolved in 30mL of deionized water, and 5mL of 37% hydrochloric acid was added to obtain a yellow tungstic acid precipitate. After stirring for 10 minutes, 5mL of 37% H 2 o 2 , the precipitate was dissolved and a clear peroxytungstic acid solution was obtained. After stirring for 10 minutes, 30 mL of ethanol was added and stirred for another 10 minutes. The fluorine-doped tin oxide (FTO) conductive glass was used as the substrate, and the FTO leaned against the wall with the face down. Water bath at 95°C for 120 minutes, and slowly precipitate tungstic acid on the FTO substrate to obtain a uniform tungstic acid film. The above tungstic acid film is rinsed with deionized water and dried at about 50°C for more than 1 hour;

[0043] 2) The dried tungstic acid film obtained in step 1) was heat-treated at 400°C for 6h, and the WO was obtained after natural cooling. 3 Nanosheet array thin film electrodes. ...

Embodiment 3

[0046] 1) Add 0.6g Na 2 WO 4 2H 2 O and 0.2g of ammonium oxalate were dissolved in 30mL of deionized water, and 15mL of 37% hydrochloric acid was added to obtain a yellow tungstic acid precipitate. After stirring for 10 minutes, 10mL of 37% H 2 o 2 , the precipitate was dissolved and a clear peroxytungstic acid solution was obtained. After stirring for 10 minutes, 30 mL of ethanol was added and stirred for another 10 minutes. The fluorine-doped tin oxide (FTO) conductive glass was used as the substrate, and the FTO leaned against the wall with the face down. Water bath at 75°C for 220 minutes, and slowly precipitate tungstic acid on the FTO substrate to obtain a uniform tungstic acid film. The above tungstic acid film is rinsed with deionized water and dried at about 50°C for more than 1 hour;

[0047] 2) heat-treat the dried tungstic acid film obtained in step 1) at a temperature of 550°C for 1 hour, and obtain the WO after natural cooling 3 Nanosheet array thin film elec...

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