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Preparation method of low-dimensional tantalum-based nano-array photo-electrode

A nano-array, photoelectrode technology, applied in electrodes, electrical components, electrolysis process, etc., to achieve the effect of high oxygen production quantum efficiency, good application prospects and economic benefits

Inactive Publication Date: 2013-10-16
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although different low-dimensional arrays of Ta-based oxynitride nanostructures can be obtained, it remains a challenge to synthesize ideal low-dimensional nano-arrays of Ta-based oxynitrides using low-cost and facile and feasible methods.

Method used

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  • Preparation method of low-dimensional tantalum-based nano-array photo-electrode
  • Preparation method of low-dimensional tantalum-based nano-array photo-electrode
  • Preparation method of low-dimensional tantalum-based nano-array photo-electrode

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Add 1cm×2cm tantalum foil to 0.05mol / L hydrofluoric acid, 2mol / L hydrogen peroxide and 8.0x10 -3 mol / L copper acetate mixed solution 16mL.

[0022] (2) Put the mixed solution and tantalum foil into a 30mL polytetrafluoroethylene-lined stainless steel autoclave, heat up to 200°C, react for 12 hours, and cool in the furnace after the reaction.

[0023] (3) The reaction product was washed several times with distilled water and alcohol and then dried at 60°C. XRD diffraction of the phase structure of the tantalum oxide photoelectrode is as follows: figure 1 shown. Put it into a muffle furnace and sinter at 700°C for 5h. The flow rate of ammonia gas in the atmosphere was controlled to 20mL / min, and the temperature of the water bottle was controlled to 30°C. After the reaction is completed, cool down with the furnace to obtain Cu 2 O / TaON photoelectrodes. The product was analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM).

[0024] (4) The pro...

Embodiment 2

[0027] (1) Add 1cm×2cm tantalum foil to 16mL of a mixed solution of 0.08mol / L hydrofluoric acid and 4mol / L hydrogen peroxide.

[0028] (2) Put the mixed solution and tantalum foil into a 30mL polytetrafluoroethylene-lined stainless steel autoclave, heat up to 240°C, react for 6 hours, and cool in the furnace after the reaction.

[0029] (3) The reaction product was washed several times with distilled water and alcohol, and then dried at 60°C. Put it into a muffle furnace and sinter at 700°C for 1h, 2h and 60h. The flow rate of ammonia gas in the atmosphere was controlled to 20mL / min, and the temperature of the water bottle was controlled to 30°C. After the reaction is completed, cool with the furnace to obtain γ-TaON array electrodes, β-TaON array electrodes, Ta 3 N 5 Array electrodes, XRD diffraction such as figure 1 .

Embodiment 3

[0031] (1) Add 1cm×2cm tantalum foil to 0.25mol / L hydrofluoric acid, 6mol / L hydrogen peroxide and 5.0x10 -3 mol / L copper acetate mixed solution 16mL.

[0032] (2) Put the mixed solution and tantalum foil into a 30mL polytetrafluoroethylene-lined stainless steel autoclave, heat up to 240°C, react for 6 hours, and cool in the furnace after the reaction.

[0033] (3) The reaction product was washed several times with distilled water and alcohol, and then dried at 60°C. Put it into a muffle furnace and sinter at 720°C for 2h. The flow rate of ammonia gas in the atmosphere was controlled to 10mL / min, and the temperature of the water bottle was controlled to 30°C. After the reaction is completed, it is obtained by cooling the furnace to obtain Co 3 o 4 / Co(II)Ta 3 N 5 photoelectrode.

[0034] (4) Subsequent photoelectric conversion performance test, such as Figure 3b shown.

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Abstract

The invention relates to a preparation method of a low-dimensional tantalum-based nano-array photo-electrode. The invention belongs to the field of solar energy, photo-catalyzing, and photochemical material. A metal tantalum foil is adopted as an initial raw material, and is mixed with hydrofluoric acid, hydrogen peroxide, cobaltate, cuprate, and the like; a constant-temperature reaction is carried out in an autoclave, such that a metal-oxide-loaded photo-electrode with the tantalum foil as a substrate and with a low-dimensional tantalum-based nano-array uniformly grown on the surface is obtained; the photo-electrode is washed by using ethanol and water, and is dried; the photo-electrode is further delivered into a heat treatment furnace, such that nitriding heat treatment is carried out; through the controlling over the ratio and flow rates of ammonia and water vapor, and through different periods of time, oxynitride and nitride array photo-electrodes with different nitrogen contents can be obtained; with a spin-coating method, graphene or nitrogen-doped graphene is uniformly covered on the surface of the nano-array. The photoelectric conversion efficiency of the tantalum-based composite nano-array photo-electrode is substantially improved. The visible-light-response tantalum-based composite nano-array photo-electrode provided by the invention has high Light-quantum conversion efficiency, and can be used in solar energy conversion and utilization.

Description

technical field [0001] The invention belongs to the preparation of nanometer material and its application in the field of new energy. It specifically relates to a preparation method of tantalum oxide, tantalum oxynitride and nitride and its heterogeneous composite nano-array photoelectrode material and the application of the material as an electrode in a photoelectrochemical cell (PEC) in splitting water by solar visible light. Background technique [0002] Obtaining energy directly from sunlight through photosynthesis is a very attractive and suitable solution to the energy crisis. People are trying to find suitable materials and systems that can use solar energy to produce chemical fuels. One of the feasible options is Construction of photochemical cells (PECs) using photoelectrodes as integrated devices. Metal oxides as photoelectrodes in photochemical cells (PECs) have been extensively studied for the conversion of solar energy to chemical fuels due to their good photos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C18/12C23C8/28C25B11/00H01M14/00
CPCY02P20/133
Inventor 侯军刚朱鸿民焦树强杨超王政
Owner UNIV OF SCI & TECH BEIJING
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