CN111058057A - Porous WO3Preparation method of photoelectrode - Google Patents

Porous WO3Preparation method of photoelectrode Download PDF

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Publication number
CN111058057A
CN111058057A CN201911214382.7A CN201911214382A CN111058057A CN 111058057 A CN111058057 A CN 111058057A CN 201911214382 A CN201911214382 A CN 201911214382A CN 111058057 A CN111058057 A CN 111058057A
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CN
China
Prior art keywords
photoelectrode
sheet
tungsten foil
preparation
drying
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Pending
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CN201911214382.7A
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Chinese (zh)
Inventor
张学亮
蒋迪
刘仪柯
罗大军
李杨
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Guizhou Institute of Technology
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Guizhou Institute of Technology
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Priority to CN201911214382.7A priority Critical patent/CN111058057A/en
Publication of CN111058057A publication Critical patent/CN111058057A/en
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
    • C25B11/031—Porous electrodes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/50—Processes
    • C25B1/55—Photoelectrolysis
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/133—Renewable energy sources, e.g. sunlight

Abstract

The present invention provides a porous WO3The preparation method of the photoelectrode comprises the steps of cutting a W sheet into squares, sequentially cleaning the W sheet with NaOH solution, acetone and ethanol, blow-drying the W sheet with nitrogen, preparing aqueous alkali with the concentration of 0.1-5 mol/L, immersing cleaned tungsten foil into the aqueous alkali, taking out the tungsten foil for blow-drying, placing the tungsten foil into a muffle furnace, heating to 550-750 ℃ at the heating rate of 12 ℃/min, preserving heat for more than 0.5h, and cooling along with the furnace. WO of this type3The photoelectrode has enhanced visible and infrared light absorption capability and can effectively improve WO3The photoelectrochemistry water decomposition efficiency of the electrode has the advantages of low cost, simple preparation method and environmental protection. Belongs to the technical field of photoelectrode improvement.

Description

Porous WO3Preparation method of photoelectrode
Technical Field
The invention relates to a porous WO3A preparation method of a photoelectrode belongs to the technical field of photoelectrode improvement.
Background
The large-scale use of fossil fuels not only leads to the exhaustion of natural resources, but also causes serious damage to earth climate and human environment, so that a new high-efficiency and environment-friendly renewable energy conversion and storage technology is necessary to be developed, and the photoelectrocatalysis decomposition of water to produce hydrogen can convert and store widely available solar energy into clean and economic hydrogen energy, so that the method is one of ideal ways for solving the problems of energy crisis and environmental pollution.
A commonly used photoanode material is TiO2、BiVO4、α-Fe2O3、WO3Etc., wherein, WO3Is an indirect band gap n-type semiconductor, the energy band structure of which is in contact with TiO2Similarly, but with a narrower forbidden band (2.5-2.9 eV), more visible light can be absorbed, and in addition, WO3Initial potential ratio BiVO of electrode4(～0.8VRHE) And α -Fe2O3(～0.9VRHE) More negative, WO3Has good light corrosion resistance, can stably exist in an acidic solution under the condition of illumination, WO3Has a very positive valence band position (+ 3.1V)NHE) The photogenerated holes have strong oxidizing capability, and not only can decompose water to generate oxygen, but also can oxidize and decompose a plurality of common organic pollutants.
In order to improve the PEC water decomposition activity of a single semiconductor photoanode, researchers have developed various improving means in recent years, including morphology and crystal plane regulation, element doping, cocatalyst loading, heterojunction construction and the like. However, limited by WO3The larger forbidden band width can absorb visible light, but can only absorb visible light with the wavelength less than 450nm, and the light absorption efficiency is still low, so that the adjustment and control of WO are necessary3To extend its light absorption, thereby increasing WO3Photoelectrolytic water activity of the photoelectrode.
Disclosure of Invention
The present invention provides a porous WO3Method for preparing photoelectrode, WO of the type3The photoelectrode has enhanced visible and infrared light absorption capability and can effectively improve WO3The photoelectrochemistry water decomposition efficiency of the electrode has the advantages of low cost, simple preparation method and environmental protection.
To achieve the above object, it is intended to use such a porous WO3The preparation method of the photoelectrode comprises the following steps:
cutting the W sheet into squares, sequentially cleaning the W sheet with NaOH solution, acetone and ethanol, blow-drying the W sheet with nitrogen, preparing 0.1-5 mol/L aqueous alkali, immersing the cleaned tungsten foil into the aqueous alkali, taking out the tungsten foil for blow-drying, putting the tungsten foil into a muffle furnace, heating to 550-750 ℃ at a heating rate of 12 ℃/min, preserving the heat for more than 0.5h, and cooling along with the furnace.
In the method, the alkali solution is one or a mixed solution of LiOH, NaOH, KOH and RbOH.
Compared with the prior art, the invention has the following advantages:
1) preparation of WO by high-temperature molten salt method3The photoelectrode has simple process, simple equipment and low cost.
2) WO prepared3The photoelectric electrode is composed of porous nano particles, and is beneficial to absorption of light and diffusion of electrolyte. In WO3The introduction of defects into the semiconductor can expand the absorption in the visible and infrared regions and increase WO3The conductivity of the organic compound promotes the separation of photogenerated electrons and holes, so that higher photoelectric conversion efficiency can be obtained.
3)WO3The forbidden band of the semiconductor can be accurately regulated and controlled by the type and concentration of the alkali solution and the annealing temperature and time.
Drawings
FIG. 1 shows the preparation of WO by alkali molten salt method3Scanning photos of the photoelectrode;
FIG. 2 shows the preparation of WO by alkali molten salt method at different temperatures3XRD pattern of photoelectrode;
FIG. 3 shows the preparation of WO by alkali molten salt method at different temperatures3Ultraviolet-visible absorption spectrum of the photoelectrode;
FIG. 4 shows the preparation of WO by alkali molten salt method at different temperatures3Photoelectrochemical properties of photoelectrode.
Detailed Description
To make the objects, technical solutions and advantages of the present invention clearer, the present invention will be described in further detail with reference to fig. 1 to 4, and it should be understood that the specific embodiments described herein are only for explaining the present invention and are not intended to limit the present invention.
Example 1
WO3The preparation process of the photoelectrode is as follows:
cutting the W sheet into 2cm by 2cm, sequentially washing with 1M NaOH solution, acetone and ethanol, and blow-drying with nitrogen. 5.6g of KOH was weighed into 100mL of deionized water and stirred for 10 minutes to give a clear and clear solution. And (4) immersing the cleaned tungsten foil into the KOH solution, taking out and drying. Putting the W sheet into a muffle furnace, heating to 650 ℃ at a heating rate of 12 ℃/min, keeping the temperature for 2h, and then cooling along with the furnace. Obtaining bright yellow WO3And an electrode.
Example 2
The KOH in example 1 was changed to LiOH, and the other reaction conditions were not changed.
Example 3
The KOH in example 1 was changed to NaOH, and the other reaction conditions were not changed.
Example 4
The KOH in example 1 was changed to RbOH, and other reaction conditions were not changed
Example 5
5.6g in example 1 was changed to 0.56g, and the other reaction conditions were not changed.
Example 6
5.6g in example 1 was changed to 2.8g, and the other reaction conditions were not changed.
Example 7
The amount of 5.6g in example 1 was changed to 28g, and the other reaction conditions were not changed.
Example 8
The annealing temperature in example 1 was changed from 650 ℃ to 550 ℃.
Example 9
The annealing temperature in example 1 was changed from 650 ℃ to 600 ℃.
Example 10
The annealing temperature in example 1 was changed from 650 ℃ to 700 ℃.
Example 11
The annealing temperature in example 1 was changed from 650 ℃ to 750 ℃.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (2)

1. Porous WO3The preparation method of the photoelectrode is characterized by comprising the following specific steps:
cutting the W sheet into squares, sequentially cleaning the W sheet with NaOH solution, acetone and ethanol, blow-drying the W sheet with nitrogen, preparing 0.1-5 mol/L aqueous alkali, immersing the cleaned tungsten foil into the aqueous alkali, taking out the tungsten foil for blow-drying, putting the tungsten foil into a muffle furnace, heating to 550-750 ℃ at a heating rate of 12 ℃/min, preserving the heat for more than 0.5h, and cooling along with the furnace.
2. A porous WO according to claim 23The preparation method of the photoelectrode is characterized in that: the alkali solution is one or a mixed solution of LiOH, NaOH, KOH and RbOH.
CN201911214382.7A 2019-12-02 2019-12-02 Porous WO3Preparation method of photoelectrode Pending CN111058057A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060051264A1 (en) * 2004-09-07 2006-03-09 Son Geon S System for removing soot of combustion exhaust gas
CN101318702A (en) * 2007-06-08 2008-12-10 郑州大学 Tungstic trioxide nano-slice and preparation method thereof
CN102674463A (en) * 2012-05-21 2012-09-19 上海交通大学 Tungsten-base tungsten trioxide nano film, and preparation method and application thereof
US20180166223A1 (en) * 2016-12-08 2018-06-14 University Of Central Florida Research Foundation, Inc. Nanowire supercapacitors and method of manufacture
CN108447692A (en) * 2018-02-09 2018-08-24 深圳源广安智能科技有限公司 A kind of improved light anode and dye-sensitized solar cells
CN110158110A (en) * 2019-06-05 2019-08-23 宁波工程学院 A kind of self-supporting WO3The preparation method and application of light anode

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060051264A1 (en) * 2004-09-07 2006-03-09 Son Geon S System for removing soot of combustion exhaust gas
CN101318702A (en) * 2007-06-08 2008-12-10 郑州大学 Tungstic trioxide nano-slice and preparation method thereof
CN102674463A (en) * 2012-05-21 2012-09-19 上海交通大学 Tungsten-base tungsten trioxide nano film, and preparation method and application thereof
US20180166223A1 (en) * 2016-12-08 2018-06-14 University Of Central Florida Research Foundation, Inc. Nanowire supercapacitors and method of manufacture
CN108447692A (en) * 2018-02-09 2018-08-24 深圳源广安智能科技有限公司 A kind of improved light anode and dye-sensitized solar cells
CN110158110A (en) * 2019-06-05 2019-08-23 宁波工程学院 A kind of self-supporting WO3The preparation method and application of light anode

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
NAOAKI KUMAGAI ET AL.,: "Kinetic and Structural Studies of the Electrochemical Insertion of Lithium into Hexagonal-type x(A20 WO3 (A = Na+, K+, NH4+)", 《J. ELECTROCHEM. SOC.》 *

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