CN113981486A - Pt cocatalyst modified photoanode material BiVO4Preparation method of (1) - Google Patents
Pt cocatalyst modified photoanode material BiVO4Preparation method of (1) Download PDFInfo
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- CN113981486A CN113981486A CN202111229963.5A CN202111229963A CN113981486A CN 113981486 A CN113981486 A CN 113981486A CN 202111229963 A CN202111229963 A CN 202111229963A CN 113981486 A CN113981486 A CN 113981486A
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- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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Abstract
The invention relates to the field of solar cell anode materials, and discloses a Pt promoter modified photo-anode material, wherein BiVO is formed on FTO through electrodeposition and calcination methods4A photoanode material, and Pt-BiVO is generated by taking the photoanode material as a substrate and adopting an electrodeposition method4A photoanode material. Due to the excellent performance of the Pt cocatalyst, the BiVO is greatly increased4The photo-anode material has a photo-current effect, so that the performance of hydrogen production by PEC photolysis water is improved. BiVO at a potential of 1.23V vs RHE4Has a photocurrent efficiency of 0.91mA/cm2Pt-BiVO modified by Pt catalyst4The highest photocurrent efficiency can reach 1.22mA/cm2And the photocurrent efficiency is improved by 25.4%.
Description
Technical Field
The invention relates to the field of solar cell anode materials, in particular to BiVO4The strength of the catalyst itself of the electrode.
Background
With the rapid increase of the degree of the current world industrialization and the rapid increase of the population, the demand for energy and the worry about environmental problems gradually develop into two mountains faced by the sustainable development of human beings, and in the past two centuries, most of the global energy consumption still comes from the traditional fossil energy, but the endless consumption of the fossil energy can bring great pressure to the life of people, the fossil fuel can be used up, and simultaneously, a large amount of greenhouse gas can be discharged to the air, so that the global warming is caused. Therefore, in order to reduce greenhouse gas emissions, it is currently the most suitable method to find clean renewable energy sources, and there are many renewable energy sources in nature, such as solar energy, wind energy, tidal energy and geothermal energy. Solar energy is considered as the most promising sustainable energy because of its considerable abundance among many clean energy sources, and the current global energy demand can be met by using as little as 0.04% of solar energy that reaches the earth's surface every year, i.e., about 50 tewatts.
However, it is difficult to directly utilize solar energy, for example, solar energy irradiated to the ground is intermittent and has a relatively low power density (about 1000W/m)2) Therefore, a large area of solar energy conversion equipment is required to improve its utilization. It is necessary to find a suitable way of storing solar energy and to improve its conversion efficiency.
Hydrogen energy is an ideal energy carrier, and combustion can generate a large amount of energy without releasing harmful greenhouse gases. Without any environmental problems. The hydrogen is widely applied in all aspects, and in the aspect of public transportation, the hydrogen energy is mature in technology and has the advantage of efficiency, and after the hydrogen energy is popularized in the future, urban pollution is greatly reduced. Besides the public transportation aspect, the battery using hydrogen fuel as energy can also be used as an emergency power supply to ensure global power supply. And the heat generated in the power generation process can be reused for providing heating. Hydrogen is therefore widely regarded as an ideal non-polluting secondary energy source.
Therefore, the conversion of solar energy into hydrogen energy is the most desirable way, and therefore, there is a strong need for a low-cost, industrially-scalable, sustainable hydrogen production system based on this idea.
Among the various hydrogen production technologies, hydrogen production by water splitting has attracted increasing attention due to the high abundance of water (covering the earth's surface by about 71%). H produced by water splitting2High purity and greatly reduced CO2And (4) discharging.
Photoelectrochemical (PEC) water splitting to produce hydrogen is considered one of the most promising approaches due to its low cost and simplicity of processing in a number of schemes for splitting water to produce hydrogen.
In order to better realize the hydrogen production by splitting the PEC water, a good-performance photo-anode material is needed, and the good photo-anode material can more efficiently realize the hydrogen production by splitting the PEC water. Wherein bismuth vanadate (BiVO)4) The material has the advantages of small band gap, proper band edge position, better theoretical water splitting efficiency and the like, and is one of the most potential photoanode materials for PEC water splitting. However, BiVO4BiVO (BiVO) is caused by short hole transmission distance and poor surface water oxidation kinetics4The base photoanode material research faces several constraints and challenges.
Based on the BiVO4The invention relates to a challenge faced by the research of a base photo-anode material, namely BiVO4The base photo-anode material is a main research object, and the BiVO with high-efficiency photo-catalytic activity is prepared by constructing a Pt cocatalyst layer on the surface4The photoelectrochemical property of the base photo-anode is improved.
Disclosure of Invention
The purpose of the invention is as follows: for BiVO4The invention utilizes the traditional electrodeposition and calcination method to grow BiVO on the surface of FTO4Base photo anode material, BiVO4A Pt promoter layer is constructed on the surface of the base photo-anode material by an electrodeposition method to further improve BiVO4Photocurrent efficiency of the base photoanode material. Is simultaneously high-efficiency BiVO4The design and development of the base photo-anode material provide important theoretical guidance and research thought
The technical scheme is as follows: scrubbing the guide surface of the FTO conductive glass for 20min by using wet cotton until water flow passes through the guide surface and can be covered with a layer of uniform water film, then scribing into 10mm multiplied by 30mm from the non-conductive surface, sequentially placing the scribed FTO glass on a glass cleaning frame, adding deionized water and glass cleaning liquid into a beaker in a ratio of 100: 3, carrying out ultrasonic treatment for 35min, carrying out ultrasonic treatment for 5min by using the deionized water, then taking out the glass cleaning frame, drying the beaker by blowing, putting the glass cleaning frame back to the beaker by adding acetone for ultrasonic treatment for 30min, then taking out the glass cleaning frame, washing the beaker by using the deionized water and then drying, putting the glass cleaning frame back to the beaker by adding absolute ethyl alcohol for ultrasonic treatment for 30min, and after cleaning, preserving the glass by using a clean ethyl alcohol solution for later use.
Growing BiVO on cleaned FTO glass by using electrodeposition and calcination methods4The specific configuration of the materials and the electrodeposition solution is as follows: 100mL of 0.4M KI solution is prepared and stirred for 15min until KI is completely dissolved. Then 1.94g Bi (NO) is added3)3·5H2Adding O into the above solution, stirring for 10min, and adding concentrated HNO dropwise3The pH of the solution was adjusted to 1.4, after which it was stirred for a further 15min until a clear solution was formed. Then 40mL of 0.23M p-benzoquinone ethanol solution is added into the clear solution dropwise, and the mixture is stirred vigorously for 20min to obtain an electrodeposition solution.
A three-electrode system is adopted, a BiOI film is deposited on cleaned FTO glass at room temperature under the condition of-0.1V vs. Ag/AgCl, and the deposition time is set to be 3 min. And after the deposition is finished, washing the substrate by using deionized water, and drying the substrate in air for later use. Then, 50. mu.L of a film containing 0.4M vanadyl acetylacetonate (VO (acac))2) And heating the DMSO solution at 450 ℃ for 2h at a heating rate of 2 ℃/min.
Then the FTO was cooled to room temperature, soaked in 1M NaOH solution and stirred slowly for 35min to remove excess V on the surface2O5Finally preparing BiVO4And (3) rinsing the photo-anode material with deionized water, placing the photo-anode material on a heating plate, setting the temperature to be 40 ℃, and drying the photo-anode material in the air for later use.
BiVO (BiVO) of the material prepared by the steps4Placing into a container containing 0.5mM H2PtCl6The electrochemical deposition is carried out in the aqueous electrolyte solution, and a three-electrode system is also adopted for preparing the Pt promoter layer. The water bath temperature is 60 ℃, the deposition voltage is respectively-0.35V vs. Ag/AgCl, -0.4V vs. Ag/AgCl, -0.45V vs. Ag/AgCl, -0.5V vs. Ag/AgCl, -0.55V vs. Ag/AgCl, the deposition is carried out under different deposition voltages, and the deposition time is 120 s.
Has the advantages that:
1. the Pt modified BiVO provided by the invention4Electrode is compared with BiVO4And the electrode has higher strength.
2. The Pt modified BiVO provided by the invention4Electrode is compared with BiVO4The electrode has higher photocurrent efficiency which is relatively improved by 15 to 26 percent.
Drawings
FIG. 1 shows Pt-BiVO prepared in example 14And BiVO4The J-V curve of the counter electrode was Pt.
FIG. 2 shows Pt-BiVO prepared in example 24And BiVO4The J-V curve of the counter electrode was Pt.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
scrubbing the guide surface of the FTO conductive glass for 20min by using wet cotton until water flow passes through the guide surface and can be covered with a layer of uniform water film, then scribing into 10mm multiplied by 30mm from the non-conductive surface, sequentially placing the scribed FTO glass on a glass cleaning frame, adding deionized water and glass cleaning liquid into a beaker in a ratio of 100: 3, carrying out ultrasonic treatment for 35min, carrying out ultrasonic treatment for 5min by using the deionized water, then taking out the glass cleaning frame, drying the beaker by blowing, putting the glass cleaning frame back to the beaker by adding acetone for ultrasonic treatment for 30min, then taking out the glass cleaning frame, washing the beaker by using the deionized water and then drying, putting the glass cleaning frame back to the beaker by adding absolute ethyl alcohol for ultrasonic treatment for 30min, and after cleaning, preserving the glass by using a clean ethyl alcohol solution for later use.
Growing BiVO on cleaned FTO glass by using electrodeposition and calcination methods4The specific configuration of the materials and the electrodeposition solution is as follows: 100mL of 0.4M KI solution is prepared and stirred for 15min until KI is completely dissolved. Then 1.94g Bi (NO) is added3)3·5H2Adding O into the above solution, stirring for 10min, and drippingEnriched HNO3The pH of the solution was adjusted to 1.4, after which it was stirred for a further 15min until a clear solution was formed. Then 40mL of 0.23M p-benzoquinone ethanol solution is added into the clear solution dropwise, and the mixture is stirred vigorously for 20min to obtain an electrodeposition solution.
A three-electrode system is adopted, a BiOI film is deposited on cleaned FTO glass at room temperature under the condition of-0.1V vs. Ag/AgCl, and the deposition time is set to be 3 min. And after the deposition is finished, washing the substrate by using deionized water, and drying the substrate in air for later use. Then, 50. mu.L of a film containing 0.4M vanadyl acetylacetonate (VO (acac))2) And heating the DMSO solution at 450 ℃ for 2h at a heating rate of 2 ℃/min.
Then the FTO was cooled to room temperature, soaked in 1M NaOH solution and stirred slowly for 35min to remove excess V on the surface2O5Finally preparing BiVO4And (3) rinsing the photo-anode material with deionized water, placing the photo-anode material on a heating plate, setting the temperature to be 40 ℃, and drying the photo-anode material in the air for later use.
BiVO (BiVO) of the material prepared by the steps4Placing into a container containing 0.5mM H2PtCl6The electrochemical deposition is carried out in the aqueous electrolyte solution, and a three-electrode system is also adopted for preparing the Pt promoter layer. The water bath temperature was 60 ℃, the deposition voltage was-0.4V vs. ag/AgCl and the deposition time was 120 s.
The test light source was a xenon lamp (PLS-SXE300/300UV) equipped with an AM1.5G filter, and the optical power density was adjusted to 100mV cm using an optical power meter-2. During the test, FTO is used as a working electrode, Pt is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, a 0.5M sodium sulfate aqueous solution (pH 7) is used as an electrolyte, and 10mV s is used-1The scanning speed of the electrode is in a potential interval of-0.41-0.79V vs. Ag/AgCl for linear scanning voltammetry test (LSV).
FIG. 1 shows the preparation of Pt-BiVO4And BiVO4The J-V curve of Pt as the counter electrode is shown schematically. BiVO at a potential of 1.23V vs RHE4Has a photocurrent efficiency of 0.98mA/cm2Pt-BiVO modified by Pt catalyst4Has a photocurrent efficiency of 1.19mA/cm2Improvement in photocurrent efficiency17.6％。
Example 2:
scrubbing the guide surface of the FTO conductive glass for 20min by using wet cotton until water flow passes through the guide surface and can be covered with a layer of uniform water film, then scribing into 10mm multiplied by 30mm from the non-conductive surface, sequentially placing the scribed FTO glass on a glass cleaning frame, adding deionized water and glass cleaning liquid into a beaker in a ratio of 100: 3, carrying out ultrasonic treatment for 35min, carrying out ultrasonic treatment for 5min by using the deionized water, then taking out the glass cleaning frame, drying the beaker by blowing, putting the glass cleaning frame back to the beaker by adding acetone for ultrasonic treatment for 30min, then taking out the glass cleaning frame, washing the beaker by using the deionized water and then drying, putting the glass cleaning frame back to the beaker by adding absolute ethyl alcohol for ultrasonic treatment for 30min, and after cleaning, preserving the glass by using a clean ethyl alcohol solution for later use.
Growing BiVO on cleaned FTO glass by using electrodeposition and calcination methods4The specific configuration of the materials and the electrodeposition solution is as follows: 100mL of 0.4M KI solution is prepared and stirred for 15min until KI is completely dissolved. Then 1.94g Bi (NO) is added3)3·5H2Adding O into the above solution, stirring for 10min, and adding concentrated HNO dropwise3The pH of the solution was adjusted to 1.4, after which it was stirred for a further 15min until a clear solution was formed. Then 40mL of 0.23M p-benzoquinone ethanol solution is added into the clear solution dropwise, and the mixture is stirred vigorously for 20min to obtain an electrodeposition solution.
A three-electrode system is adopted, a BiOI film is deposited on cleaned FTO glass at room temperature under the condition of-0.1V vs. Ag/AgCl, and the deposition time is set to be 3 min. And after the deposition is finished, washing the substrate by using deionized water, and drying the substrate in air for later use. Then, 50. mu.L of a film containing 0.4M vanadyl acetylacetonate (VO (acac))2) And heating the DMSO solution at 450 ℃ for 2h at a heating rate of 2 ℃/min.
Then the FTO was cooled to room temperature, soaked in 1M NaOH solution and stirred slowly for 35min to remove excess V on the surface2O5Finally preparing BiVO4And (3) rinsing the photo-anode material with deionized water, placing the photo-anode material on a heating plate, setting the temperature to be 40 ℃, and drying the photo-anode material in the air for later use.
BiVO (BiVO) of the material prepared by the steps4Placing into a container containing 0.5mM H2PtCl6The electrochemical deposition is carried out in the aqueous electrolyte solution, and a three-electrode system is also adopted for preparing the Pt promoter layer. The water bath temperature was 60 ℃, the deposition voltage was-0.35V vs. Ag/AgCl, and the deposition time was 120 s.
The test light source was a xenon lamp (PLS-SXE300/300UV) equipped with an AM1.5G filter, and the optical power density was adjusted to 100mV cm using an optical power meter-2. During the test, FTO is used as a working electrode, Pt is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, a 0.5M sodium sulfate aqueous solution (pH 7) is used as an electrolyte, and 10mV s is used-1The scanning speed of the electrode is in a potential interval of-0.41-0.79V vs. Ag/AgCl for linear scanning voltammetry test (LSV).
FIG. 1 shows the preparation of Pt-BiVO4And BiVO4The J-V curve of Pt as the counter electrode is shown schematically. BiVO at a potential of 1.23V vs RHE4Has a photocurrent efficiency of 0.91mA/cm2Pt-BiVO modified by Pt catalyst4Has a photocurrent efficiency of 1.22mA/cm2And the photocurrent efficiency is improved by 25.4%.
Claims (7)
1. Pt cocatalyst modified photoanode material BiVO4The preparation method is characterized by comprising the following steps: BiVO modified by Pt cocatalyst4The photo-anode material has higher photo-current efficiency.
2. The BiVO of claim 1 produced by growing BiOI on FTO by electrodeposition, adding a DMSO solution of vanadyl acetylacetonate, and calcining4A photoanode material, characterized by: the voltage at which the electrodeposition produces the BiOI can be controlled, and the thickness of the BiOI can be controlled.
3. The method for preparing BiVO modified by Pt promoter according to claim 14A photoanode material, characterized by: the concentration of KI electrolyte is 0.4M, and the concentration of Bi (NO)3)3·5H2The O concentration was 0.04M.
4. The method for preparing BiVO modified by Pt promoter according to claim 14A photoanode material, characterized by: the surface of the generated photo-anode material is of a porous structure.
5. BiVO modified by Pt promoter prepared according to claim 14A photoanode material, characterized by: and the traditional BiVO4Compared with the photo-anode material, the material has better photolytic water splitting effect.
6. BiVO modified by Pt promoter prepared according to claim 14A photoanode material, characterized by: and the traditional BiVO4The material is more stable than the photoanode material.
7. BiVO modified by Pt promoter prepared according to claim 14A photoanode material, characterized by: the concentration of vanadyl acetylacetonate in DMSO was 0.4M.
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| CN115207367A (en) * | 2022-07-11 | 2022-10-18 | 燕山大学 | Air electrode, preparation method and application thereof, and photo-assisted charging zinc-air battery |
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| CN115207367A (en) * | 2022-07-11 | 2022-10-18 | 燕山大学 | Air electrode, preparation method and application thereof, and photo-assisted charging zinc-air battery |
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