Preparation method for WO3/CuWO4/NiFe LDH ternary composite photoelectrode film

A ternary composite, photoelectrode technology, applied in electrodes, electrolysis process, electrolysis components, etc., can solve problems such as poor stability, and achieve the effect of reducing energy barrier, slowing attenuation, and simple preparation process

Active Publication Date: 2019-06-21
TAIZHOU UNIV
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Problems solved by technology

[0004] The object of the present invention is to provide a WO 3 / CuWO 4 / NiFe LDH ternary composite photoelectrode thin film preparation method, the photoelectrode thin film prepared by the present invention is based on FTO conductive glass, prior to the hydrothermal growth of WO on the substrate 3 , after impregnating copper nitrate, the WO 3 High temperature calcination into CuWO 4 , and finally NiFe LDH was supported on the electrode surface by electrodeposition, and WO was successfully constructed. 3 / CuWO 4 / NiFe LDH ternary composite photoelectrode, the photoelectrode can realize effective water splitting and hydrogen production in the electrolyte solution with a pH of 9, and the electrode effectively solves the problem of WO 3 The problem of poor stability has broad application prospects in the field of photocatalytic water splitting

Method used

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  • Preparation method for WO3/CuWO4/NiFe LDH ternary composite photoelectrode film

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Embodiment 1

[0017] A kind of WO 3 / CuWO 4 / NiFe LDH ternary composite photoelectrode thin film preparation method, the specific steps are as follows:

[0018] Prepare 15ml of sodium tungstate solution with a concentration of 25mmol / L, and add 5ml of hydrochloric acid (3mol / L) dropwise; prepare 15ml of an aqueous ammonium oxalate solution with a concentration of 55mmol / L, slowly add it to the sodium tungstate solution, and stir for 30min; transfer the mixture To the lining of the hydrothermal reactor, the FTO glass is washed with water, ethanol and acetone, N 2 Flow down and blow dry, place the FTO with the conductive side facing down, and place it in the inner lining of the reaction kettle, and conduct a hydrothermal reaction at 140°C for 6 hours; take it out, wash it with water three times, dry it at 25°C, and place it in a muffle furnace for calcination at 500°C for 2 hours ; Dissolve copper nitrate in acetic acid solution with a concentration of 50 mmol / L, pipette 100 μL of the solut...

Embodiment 2

[0021] A kind of WO 3 / CuWO 4 / NiFe LDH ternary composite photoelectrode film preparation method, the experimental steps are the same as in Example 1, changing the copper nitrate concentration to 20mmol / L, pipetting 100 μL of this solution with a pipette, and adding it dropwise to WO 3 On the membrane electrode, repeat this operation 3 times; Configuration 50ml concentration is the ferric nitrate of 5mmol / L and concentration is the nickel nitrate solution of 2mmol / L, the WO 3 / CuWO 4 As a working electrode, deposit at -1.1V potential for 30s, take out the working electrode, wash with water, and dry in the air to obtain WO 3 / CuWO 4 / NiFeLDH ternary composite photoelectrode.

[0022] figure 2 for WO 3 and WO 3 / CuWO 4 / NiFe LDH thin-film electrode UV-Vis diffuse reflectance map for pure phase WO 3 , its band-edge absorption position appears at 450nm, and the calculated band gap is about 2.65eV. in WO 3 After the introduction of copper tungstate and NiFe LDH on the e...

Embodiment 3

[0024] A kind of WO 3 / CuWO 4 / NiFe LDH ternary composite photoelectrode film preparation method, the experimental steps are the same as in Example 1, changing the copper nitrate concentration to 60mmol / L, pipetting 100 μL of this solution with a pipette, and adding it dropwise to WO 3 On the membrane electrode, repeat this operation 2 times; Configuration 50ml concentration is the ferric nitrate of 3mmol / L and concentration is the nickel nitrate solution of 10mmol / L, the WO 3 / CuWO 4 As a working electrode, deposit at -1.2V potential for 30s, take out the working electrode, wash with water, and dry in the air to obtain WO 3 / CuWO 4 / NiFeLDH ternary composite photoelectrode.

[0025] image 3 for WO 3 、WO 3 / CuWO 4 and WO 3 / CuWO 4 / NiFe LDH three electrode scanning electron microscope images, it can be seen that the morphology of the three electrodes is plate-like, but after calcining with the addition of copper ions, the surface of the plate-like structure becomes ...

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Abstract

The invention relates to a preparation method for a WO3/CuWO4/NiFe LDH ternary composite photoelectrode film, and belongs to the technical field of photoelectrocatalysis. According to the composite photoelectrode, key problems of low WO3 stability, weak product selectivity and the like can be overcome; long-term stable operation in a photochemical water decomposition process is realized successfully; the composite photoelectrode has an extremely high application value. The preparation method for the ternary composite photoelectrode film mainly comprises the following steps: taking sodium tungstate and ammonium oxalate as raw materials; carrying out a hydrothermal reaction for 6 hours at 140 DEG C to synthesize a WO3 film electrode; adding an acetic acid solution of copper nitrate on the surface of the WO3 film electrode dropwise in an impregnating manner; performing high-temperature calcining at 500 DEG C, wherein part WO3 reacts with CuO to generate copper tungstate to obtain a WO3/CuWO4 film electrode; then, preparing an electrolyte solution of ferric nitrate and nickel nitrate, and loading a NiFe layered compound onto the surface of the WO3/CuWO4 film electrode according to an electrodepositing method to finally obtain the WO3/CuWO4/NiFe LDH ternary composite photoelectrode film.

Description

technical field [0001] The present invention relates to a WO 3 / CuWO 4 The preparation method of / NiFe LDH ternary composite photoelectrode film belongs to the field of photoelectric catalysis technology, and more specifically, the invention provides a kind of WO with visible light response 3 / Fe 2 o 3 / Mn 3 o 4 The invention discloses a method for preparing a ternary composite photoelectrode. The composite photoelectrode can effectively utilize solar energy to realize continuous and stable hydrogen evolution. Background technique [0002] Hydrogen energy is a clean and pollution-free energy source, and the development of efficient, clean and low-cost hydrogen production technology is the key to realize the utilization of hydrogen energy. Photoelectric catalytic water splitting technology simulates the photosynthesis of plants. Semiconductor materials absorb solar energy to generate photogenerated carriers. Photogenerated electrons reduce hydrogen ions to generate hydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/06C25B1/04
CPCY02E60/36
Inventor 熊贤强范利亚武承林
Owner TAIZHOU UNIV
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