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Preparation method of WO3 nano-sheet array

A nanosheet array and substrate material technology, applied in the field of photocatalysis and photoelectrochemical materials, can solve the problems of low crystallinity, complicated operation process, and low purity

Active Publication Date: 2017-09-01
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commonly used thermal evaporation method, chemical vapor deposition method, sputtering method, etc. are faced with the need to create a high temperature or vacuum environment, which is easy to cause environmental pollution and complicated operation processes, and the prepared nano-WO 3 It is also possible that the crystallinity is low and the purity is not high, which will affect the nano WO 3 various performance

Method used

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  • Preparation method of WO3 nano-sheet array
  • Preparation method of WO3 nano-sheet array
  • Preparation method of WO3 nano-sheet array

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1) Dissolve 0.4 g of oxalic acid in 40 mL of absolute ethanol, and weigh 0.2 g of tungsten hexachloride in a vacuum glove box. After mixing evenly, add it into a polytetrafluoroethylene reaction kettle with a volume of 60mL, then put the cleaned FTO into the polytetrafluoroethylene reaction kettle obliquely, react at 180°C for 6 hours, cool the reaction kettle with tap water for 30 minutes, and wash it with distilled water The surface of the FTO was vacuum-dried at 60°C for use.

[0015] (2) Put the electrode material synthesized in step (1) into a muffle furnace, raise the temperature to 500°C at a heating rate of 5°C / min, anneal for 120min, take it out after it drops to room temperature, and obtain the FTO surface with WO 3 Photoelectrodes of nanosheet arrays.

[0016] With the prepared WO 3 The nanosheet array photoelectrode was used as the working electrode (with an area of ​​1 cm 2 ), the auxiliary electrode is a platinum electrode, the saturated calomel electr...

Embodiment 2

[0018] (1) Dissolve 0.4 g of oxalic acid in 40 mL of absolute ethanol, and weigh 0.2 g of tungsten hexachloride in a vacuum glove box. After mixing evenly, add it to a polytetrafluoroethylene reaction kettle with a volume of 60mL, then put the cleaned carbon cloth into the polytetrafluoroethylene reaction kettle, react at 120°C for 6h, cool with tap water for 30min, and clean the surface of the carbon cloth with distilled water , vacuum-dried at 60°C and set aside.

[0019] (2) Put the electrode material synthesized in step (1) into a muffle furnace, raise the temperature to 400°C at a heating rate of 5°C / min, anneal for 120min, take it out after it drops to room temperature, and obtain carbon cloth substrate surface with WO 3 Photoelectrodes of nanosheet arrays.

[0020] WO 3 Nanosheet array carbon cloth as the working electrode (with an area of ​​1 cm 2 ), the auxiliary electrode is a platinum electrode, the saturated calomel electrode (SCE) is used as a reference electr...

Embodiment 3

[0022] 1) Dissolve 0.8g of oxalic acid in 40mL of absolute ethanol, and weigh 0.2g of tungsten hexachloride in a vacuum glove box. After mixing evenly, add it to a polytetrafluoroethylene reaction kettle with a volume of 60mL, then put the cleaned silicon chip into the polytetrafluoroethylene reaction kettle obliquely, react at 180°C for 6h, cool with tap water for 30min, and wash the silicon wafer with distilled water. The surface of the sheet was vacuum-dried at 60°C for use.

[0023] (2) Put the electrode material synthesized in step (1) into a muffle furnace, raise the temperature to 600°C at a heating rate of 5°C / min, anneal for 120min, take it out after it drops to room temperature, and obtain a substrate with WO 3 Photoelectrodes of nanosheet arrays.

[0024] WO 3 Nanosheet array carbon cloth as the working electrode (with an area of ​​1 cm 2 ), the auxiliary electrode is a platinum electrode, the saturated calomel electrode (SCE) is used as a reference electrode, 0....

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Abstract

The invention discloses a preparation method of a WO3 nano-sheet array. The preparation method comprises the following steps: firstly, growing WO3-x.H2O nano-sheet array thin films with oxygen defects on surfaces of FTO (Fluorine-doped Tin Oxide), carbon cloth and a silicon wafer through an oxalic acid, ethanol and tungsten hexachloride solvent-thermal method; calcining in a muffle furnace at certain temperature to obtain the WO3 nano-sheet array with a relatively good crystallization property. WO3 prepared on a substrate represents a regular and vertically aligned nano-sheet array, so that the specific surface area of the WO3 nano-sheet array is greatly improved; the light current of a WO3 nano-sheet reaches 0.8mA / cm<2> in 0.5ml / L of Na2SO4 electrolyte under 0.7 sunlight light intensity and bias voltage of 1.2V. The method disclosed by the invention is simple and convenient to operate and easy to control; a WO3 nano-sheet array thin film prepared by the method has a large specific surface area and high photoelectric chemical activity and stability.

Description

technical field [0001] The technical field of the invention is the technical field of photocatalysis and photoelectrochemical materials, in particular to WO 3 Catalyst development and preparation methods. Background technique [0002] Tungsten trioxide is a multifunctional inorganic metal oxide semiconductor material. The material has excellent physical and chemical properties, such as photocatalysis, photochromism, electrochromism, field emission and other properties, so it is widely used in the fields of photocatalysts, electrochromic smart windows and photoelectrochemical instruments. Nano WO 3 The preparation method can be summarized as solid-phase method, gas-phase method and liquid-phase method, and each preparation method all has certain advantages and disadvantages. The commonly used thermal evaporation method, chemical vapor deposition method, sputtering method, etc. are faced with the need to create a high temperature or vacuum environment, which is easy to caus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C17/34D06M11/48C01G41/02B82Y40/00H01L31/0224
CPCC01G41/02C01P2002/72C01P2004/03C01P2006/40C03C17/3417C03C2217/219C03C2217/241C03C2217/42C03C2217/71C03C2218/111C03C2218/32D06M11/48H01L31/022425
Inventor 刘勇平杨之书吕慧丹耿鹏林剑飞张梦莹米喜红
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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