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A kind of tungsten oxide monolayer nanosheet and its preparation method and application

A tungsten oxide monolayer and nanosheet technology, applied in tungsten oxide/tungsten hydroxide, nanotechnology, electrolytic components, etc., to achieve the effects of easy implementation, low energy consumption, and simple synthesis process

Active Publication Date: 2021-03-30
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the thickness of the obtained tungsten trioxide nanosheets of this method is 5-40nm, because the thickness of single-layer nanosheets is about 1nm, so the resulting product is not single-layer tungsten trioxide nanosheets

Method used

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  • A kind of tungsten oxide monolayer nanosheet and its preparation method and application
  • A kind of tungsten oxide monolayer nanosheet and its preparation method and application
  • A kind of tungsten oxide monolayer nanosheet and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0053] A kind of WO 3 ·H 2 O. WO 3 A method for preparing a single-layer nanosheet, comprising the steps of:

[0054] Preparation of metatungstate anion intercalation LDHs complex by ion exchange method:

[0055] Take 10.2g Mg(NO 3 ) 2 ·6H 2 O and 7.6g Al(NO 3 ) 3 9H 2 O was dissolved in 200ml deionized water to obtain solution A. Take 6.4g NaOH and dissolve in 100ml deionized water to obtain solution B. Solutions A and B were simultaneously added dropwise to 50 ml of degassed deionized water C under stirring conditions, and the pH was controlled to be 10.0 under nitrogen protection. After stirring at room temperature for 30 min, it was aged in an oven at 80° C. under nitrogen protection for 12 h. After filtration, washing, and vacuum drying at 60°C for 12 hours, NO 3 - Intercalated LDHs. Weigh 5.0g of prepared LDHs and 5.0g of ammonium metatungstate into 100ml of degassed deionized water, N 2 Under protection, stir at 40°C for 24h. After filtration, washing an...

Embodiment 2

[0065] A kind of WO 3 ·H 2 O. WO 3 A method for preparing a single-layer nanosheet, comprising the steps of:

[0066] Metatungstate anion-intercalated LDHs composites were prepared by structural reconstruction method.

[0067] Take 100ml deionized water, 6.8g Mg(NO 3 ) 2 ·6H 2 O, 5.0g Al(NO 3 ) 3 9H 2 O and 8g of urea were added to a three-necked flask, stirred at room temperature for 0.5h to dissolve the solid, and refluxed in an oil bath at 90°C for 24h. After filtering, washing, and drying at 60°C for 12 hours, CO 3 2― Intercalated LDHs. The prepared LDHs were calcined in a muffle furnace at 400 °C for 2 h to obtain MMO templates. Weigh 5.0g of MMO and 5.0g of ammonium metatungstate, put them into 100ml of degassed deionized water, and stir for 24h under the protection of nitrogen, with the temperature kept at 40°C. Then the dispersion was filtered, washed, and dried at 60°C for 12 hours to obtain the metatungstate anion-intercalated LDHs complex.

[0068] 5 g...

Embodiment 3

[0071] A kind of WO 3 ·H 2 O. WO 3 A method for preparing a single-layer nanosheet, comprising the steps of:

[0072] The preparation of the metatungstate anion intercalation LDHs complex is as described in Example 1;

[0073] 5 g of AMT anion intercalation LDH composite powder was placed in a tube furnace, heated to 300 °C for 1 h in an air atmosphere, and calcined at a heating rate of 5 °C / min. After natural cooling to room temperature, WO 3 / MMO complex. Take 2g WO 3 / MMO complex was added to 100ml 0.5mol / L sulfuric acid, stirred at room temperature for 12h, then filtered, washed with water, and freeze-dried for 10h to obtain WO 3 ·H 2 O monolayer nanosheets.

[0074] The above obtained WO 3 ·H 2 O monolayer nanosheets placed in a tube furnace, N 2 Under protection, the temperature was raised to 280°C for 1h and the heating rate was 2°C / min to obtain WO 3 monolayer nanosheets.

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Abstract

The invention provides a tungsten oxide single-layer nanosheet as well as a preparation method and application thereof. The method comprises the steps: preparing a tungstate or metatungstate anion intercalation LDHs compound; calcining the tungstate radical or metatungstate radical anion intercalation LDHs compound for 1 to 4 h at the temperature of 200 to 600 DEG C to obtain a WO3 / MMO compound; and then adding into acid, stirring for 10-15 h at room temperature, filtering, washing and drying to obtain the WO3.H2O single-layer nanosheet; and further calcining the obtained WO3.H2O single-layernanosheet at a low temperature of 300-450 DEG C for 0.5-2 h to obtain the WO3 single-layer nanosheet. The preparation method is simple to operate, environment-friendly and easy to industrialize; the proportion of a single layer in the obtained tungsten oxide nanosheet is high, and the technical problem of large-scale preparation of the tungsten oxide single-layer nanosheet is solved; the preparedtungsten oxide nanosheet has good electro-catalytic hydrogen evolution performance.

Description

technical field [0001] The invention relates to a tungsten oxide single-layer nanosheet and a preparation method and application thereof, belonging to the field of nanomaterial preparation. Background technique [0002] Transition metal oxides have great application potential in the fields of photocatalysts, electrocatalysts, energy storage materials, and degradation of pollutants. Ultrathin materials have attracted extensive attention due to their high specific surface area and unique properties, but their macrofabrication remains challenging. [0003] Tungsten oxide (WO 3 ) or hydrated tungsten oxide (WO 3 ·xH 2 O) as a typical transition metal oxide can be widely used in photocatalysis, sensing, energy conversion, and pollutant degradation. The existing preparation methods of tungsten oxide ultrathin nanosheets include ultrasonic liquid phase exfoliation method, hydrothermal method and electrochemical deposition method, but the above methods are difficult to realize t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/02B82Y40/00C25B11/077C25B1/04
CPCB82Y40/00C01G41/02C01P2002/72C01P2004/03C01P2004/04C01P2004/20C01P2006/12C01P2006/14C01P2006/16C01P2006/82C25B1/04C25B11/077Y02E60/36
Inventor 侯万国王德良李海平杜娜
Owner SHANDONG UNIV