CN110965073B - WO containing defects3Preparation method of photoelectrode - Google Patents
WO containing defects3Preparation method of photoelectrode Download PDFInfo
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Abstract
The present invention provides a WO having a defect3Method for producing photoelectrode, WO3The electrodes are grown on the conductive surface of the conductive glass by a water bath method, and the WO is led by a lead3Electrodes are connected to the metal foil, and then WO is added3The electrode and the metal foil being immersed simultaneously in an electrolyte solution of a given concentration, WO3The color of the film gradually changes from yellow to blue, and defects are generated on the surface of the material. WO3The light absorption characteristics and color change of the film can be controlled by controlling the reaction time, the reduction potential of the metal foil, and the concentration of the solution. The preparation method has simple process and is beneficial to large-scale preparation and production. The material has great application prospect in the aspects of hydrogen production by photoelectric decomposition of water, chemical discoloration, solar cells and the like. Belongs to the technical field of photoelectrode improvement.
Description
Technical Field
The invention relates to a WO containing defects3A preparation method of a photoelectrode belongs to the technical field of photoelectrode improvement.
Background
With the rapid development of modern human society and the continuous increase of population, the shortage of energy becomes a central problem restricting the development of economy, so that new energy and energy-saving ways are searched in all countries in the world. Among a plurality of renewable clean energy sources, people pay attention to the utilization of solar energy, because the solar energy is inexhaustible, green and convenient natural energy. Solar energy can be classified into three types, i.e., photoelectric conversion, photothermal conversion, and photochemical conversion, depending on the manner of utilization of the solar energy. The technology of hydrogen production by water photolysis, which is one of the solar energy photochemical conversion technologies, is the leading edge of the research field of solar energy utilization technology at present. The principle of hydrogen production by photolysis of water is that under the irradiation of sunlight, a semiconductor can generate electrons and holes in a conduction band and a valence band respectively due to the photoelectric effect, and the generated electrons and holes can be used for reducing and oxidizing water to generate hydrogen and oxygen respectively. The hydrogen is used as a clean energy source, has the advantages of no toxicity, no odor, large mass energy density, high combustion heat value and the like, and is convenient to transport and an ideal energy carrier. The photocatalytic hydrogen production technology can convert wide solar energy into clean hydrogen energy, and provides an ideal solution for solving the problems of energy shortage and environmental deterioration.
The commonly used photocatalyst is TiO2、ZnO、CdS、WO3Etc., in which WO3The semiconductor is a typical indirect semiconductor with a narrow band gap, the forbidden band width Eg is 2.6-2.8 eV, and the semiconductor can absorb part of visible light in sunlight. In addition, tungsten oxide has high carrier mobility and stability in acid electrolytes and against corrosion by light, and the advantages make it a hot research point in the field of photoelectrochemical water decomposition. W of tungsten oxide6+The material has the advantages of easy valence change and structural diversity, great adjustability of surface properties and electronic structures, gradual change into a material which is very concerned in the field of defect engineering, and wide application in the fields of photoelectricity and photo-thermal catalysis. However, although tungsten oxide can absorb visible light, it can only absorb a small portion of visible light due to the deep 2p orbital of the oxygen atom, and is still insufficient for light absorption. And the hole mobility of tungsten oxide is low, which causes serious recombination of photon-generated carriers. In addition oxidationTungsten is an acidic semiconductor and cannot be stabilized in neutral or alkaline electrolytes. These disadvantages limit its further application.
Recent studies have shown that the introduction of a proper amount of defects in the oxide semiconductor can enhance the light absorption characteristics, charge separation efficiency, and catalytic reaction kinetics of the photocatalyst, thereby improving the photoelectric activity of the photoelectrode. However, the traditional defect introduction method often involves high-temperature inert atmosphere treatment, and not only the reaction conditions are harsh, but also the preparation process is complex and expensive. In order to overcome the defects in the traditional preparation method, the invention provides a method for introducing the defects of the semiconductor at normal temperature, and can realize the accurate regulation and control of the defect concentration and the light absorption characteristic of the photoelectrode.
Disclosure of Invention
The present invention provides a WO having a defect3Method for preparing photoelectrode, WO of the type3The photoelectrode has smaller impedance and enhanced visible and infrared light absorption capability, and can effectively improve WO3The photoelectrochemistry water decomposition efficiency of the electrode is low, the cost is low, the preparation method is simple, and the environment is protected.
To achieve the above object, it is proposed to use such a WO containing defects3The preparation method of the photoelectrode comprises the following specific steps:
(1)WO3preparing a photoelectrode: adding a certain amount of HCl solution into sodium tungstate solution to obtain yellow tungstic acid suspension, and then adding a certain amount of ammonium oxalate to obtain transparent clear solution. Putting the cleaned FTO conductive glass with the conductive surface facing downwards into the solution, and reacting in a water bath at a certain temperature for a certain time to obtain bright yellow H2WO4And an electrode. H to be prepared2WO4Annealing the electrode in a muffle furnace for a period of time to obtain a pale yellow WO3An electrode;
(2) defect WO3Preparing a photoelectrode: the WO prepared in (1) is3Connecting the electrodes to the metal foil with wires, and connecting the electrodes to the metal foil with the wires3The electrode and the metal foil are immersed into an electrolyte solution with a certain concentration for reaction for a certain time, WO3The color of the electrode gradually changes from light yellow to light yellowDeep blue, washing the photoelectrode with deionized water and ethanol respectively and drying to obtain WO containing defects3And a photoelectrode.
In the step (1), the molar ratio of sodium tungstate to hydrochloric acid to ammonium oxalate is 1: (5-20): (1-10), the water bath temperature is 50-80 ℃, the water bath time is 4-12 hours, the annealing temperature is 400-.
In the method, the electrolyte solution is an acidic solution, and is one or a mixed solution of hydrochloric acid, sulfuric acid and nitric acid, the concentration of the electrolyte is 0.1-6mol/L, the metal sheet used in the acidic solution is Fe, Zn, Cu, Ni or Al, the purity of the metal foil is more than 99%, and the reaction time is 2 seconds-5 minutes.
In the method, the electrolyte solution is alkaline solution, is one or a mixed solution of KOH, NaOH and LiOH, the concentration of the electrolyte solution is 0.1-6mol/L, the metal foil used in the alkaline solution is Al foil, the purity is more than 99%, and the reaction time is 2 seconds-5 minutes.
WO3The principle of color change is that the metal foil and electrolyte solution generate oxidation-reduction reaction to generate electrons, and the electrons are transferred to WO3On the electrode and the WO3Partially reduced while being described in WO3Generation of oxygen vacancies, defects WO in semiconductors3Photoelectrodes exhibit light absorption in the visible and infrared regions. Oxygen vacancy can increase WO3Conductivity of electrodes and extension of WO3Thereby enhancing WO3Photoelectrochemical water splitting efficiency of the photoelectrode.
Compared with the prior art, the invention has the following advantages:
1) WO prepared3The photoelectrode consists of a nanosheet array, a nanopore structure exists on the surface of the nanosheet after high-temperature annealing, so that light absorption and electrolyte diffusion are facilitated, and WO3The introduction of defects into the semiconductor can expand the absorption in the visible and infrared regions and increase WO3The conductivity of the material promotes the separation of photogenerated electrons and holes, so that higher photoelectric conversion efficiency can be obtained;
2) preparation of WO by water bath method3Photoelectrode, reaction temperatureLow cost, simple process, simple equipment and low cost;
3) in WO3The method for introducing defects into the electrode does not need the traditional high-temperature reduction treatment, and has the advantages of low reaction temperature, simple technical process, simple equipment, quick and safe reaction and low cost;
4)WO3the light absorption peak caused by the color and the defect of can be adjusted by chemical reaction, by controlling the reaction time, adopting different metal foils, adopting solutions with different concentrations and other reaction conditions, the WO can be accurately regulated and controlled3The degree of color change and the defect concentration of the prepared WO can be flexibly regulated and controlled according to requirements3Performance of the photoelectrode.
Drawings
FIG. 1 shows WO prepared by a water bath method3Scanning electron microscope photographs of the photoelectrode;
FIG. 2 is WO3The UV-visible absorption spectra of photoelectrode and Fe foil after different reaction times (2s, 5s, 10s, 60s) with the reaction time being prolonged, WO3Gradually blue-shifting an absorption peak caused by a defect energy level of the electrode;
FIG. 3 is WO3Ultraviolet-visible absorption spectrum of photoelectrode and different metal foils (Ni, Cu, Fe, Zn and Al) after reaction in 3mol/L HCl solution;
FIG. 4 is WO3Ultraviolet-visible absorption spectra before and after the electrode and the Al metal foil react in 1mol/L NaOH solution;
FIG. 5 shows WO3Photoelectrochemical properties of the photoelectrode after different times of reaction with the Fe foil. And (3) testing conditions are as follows: simulated sunlight (AM1.5G,100 mW/cm)2) 0.5mol/L of H2SO4The solution is used as electrolyte, the Pt wire is used as a counter electrode, and the Ag/AgCl is used as a reference electrode;
FIG. 6 shows WO before and after reduction treatment3W4 f high resolution XPS spectra of the electrodes.
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 6, 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
(1)WO3The preparation process of the photoelectrode is as follows: 3.3g of sodium tungstate is weighed and dissolved in 1000mL of deionized water, and the mixture is stirred for 10 minutes to obtain a transparent clear solution. 40mL of a 5mol/L HCl solution was added to the solution, and the mixture was stirred for 10 minutes to obtain a yellow tungstic acid suspension, and then 2.48g of ammonium oxalate was added to obtain a transparent clear solution. Putting the cleaned FTO conductive glass into the solution with the conductive surface facing downwards, and reacting in a water bath at 60 ℃ for 8 hours to obtain bright yellow H2WO4And an electrode. H to be prepared2WO4The electrode was placed in a muffle furnace and annealed at 500 ℃ for 2 hours to give a pale yellow WO3And an electrode.
(2) Defect WO3The preparation process of the photoelectrode is as follows: the WO prepared in (1) is3The electrodes are connected with Fe foil by wires, and WO3The electrode and the Fe foil are immersed into 3mol/L HCl solution for reaction for 10 seconds, WO3Gradually changing the color of the electrode from light yellow to dark blue, washing the photoelectrode with deionized water and ethanol respectively, and drying to obtain the WO containing defects3And a photoelectrode.
Example 2
(1)WO3The preparation process of the photoelectrode is as follows: 8.25g of sodium tungstate is weighed and dissolved in 1000mL of deionized water, and the solution is stirred for 10 minutes to obtain a transparent clear solution. 100mL of a 5mol/L HCl solution was added to the solution, and the mixture was stirred for 10 minutes to obtain a yellow tungstic acid suspension, and then 6.2g of ammonium oxalate was added to obtain a transparent clear solution. Putting the cleaned FTO conductive glass into the solution with the conductive surface facing downwards, and reacting in water bath at 60 ℃ for 8 hours to obtain bright yellow H2WO4And an electrode. H to be prepared2WO4The electrode was placed in a muffle furnace and annealed at 500 ℃ for 2 hours to give a pale yellow WO3And an electrode.
(2) Defect WO3The preparation process of the photoelectrode is as follows: the WO prepared in (1) is3The electrodes are connected with Fe foil by wires, and WO3The electrode and the Fe foil are immersed into 3mol/L HCl solution for reaction for 10 seconds, WO3The color of the electrode gradually changes from light yellow to light yellowDeep blue, washing the photoelectrode with deionized water and ethanol respectively and drying to obtain the WO containing defects3And a photoelectrode.
Example 3
(1)WO3The preparation process of the photoelectrode is as follows: 16.5g of sodium tungstate is weighed and dissolved in 1000mL of deionized water, and the solution is stirred for 10 minutes to obtain a transparent clear solution. 250mL of HCl solution with the concentration of 5mol/L is added into the solution, the solution is stirred for 10 minutes to obtain a yellow tungstic acid suspension, and then 12.4g of ammonium oxalate is added to obtain a transparent clear solution. Putting the cleaned FTO conductive glass into the solution with the conductive surface facing downwards, and reacting in water bath at 60 ℃ for 8 hours to obtain bright yellow H2WO4And an electrode. H to be prepared2WO4The electrode was placed in a muffle furnace and annealed at 500 ℃ for 2 hours to give a pale yellow WO3And an electrode.
(2) Defect WO3The preparation process of the photoelectrode is as follows: the WO prepared in (1) is3The electrodes are connected with Fe foil by wires, and WO3The electrode and the Fe foil are immersed into 3mol/L HCl solution for reaction for 10 seconds, WO3Gradually changing the color of the electrode from light yellow to dark blue, washing the photoelectrode with deionized water and ethanol respectively, and drying to obtain the WO containing defects3And a photoelectrode.
Example 4
(1)WO3The preparation process of the photoelectrode is as follows: 8.25g of sodium tungstate is weighed and dissolved in 1000mL of deionized water, and the solution is stirred for 10 minutes to obtain a transparent clear solution. 100mL of a 5mol/L HCl solution was added to the solution, and the mixture was stirred for 10 minutes to obtain a yellow tungstic acid suspension, and then 6.2g of ammonium oxalate was added to obtain a transparent clear solution. Putting the cleaned FTO conductive glass into the solution with the conductive surface facing downwards, and reacting in water bath at the temperature of 80 ℃ for 8 hours to obtain bright yellow H2WO4And an electrode. H to be prepared2WO4The electrode was placed in a muffle furnace and annealed at 500 ℃ for 2 hours to give a pale yellow WO3And an electrode.
(2) Defect WO3The preparation process of the photoelectrode is as follows: the WO prepared in (1) is3The electrodes are connected with Fe foil by wires, and WO3Electrode and FeThe foil is simultaneously immersed in a 3mol/L HCl solution for 10 seconds, WO3Gradually changing the color of the electrode from light yellow to dark blue, washing the photoelectrode with deionized water and ethanol respectively, and drying to obtain the WO containing defects3And a photoelectrode.
Example 5
The water bath time in step (1) of example 2 was changed to 4 hours, and the other reaction conditions were not changed.
Example 6
The water bath time in step (1) of example 2 was changed to 12 hours, and the other reaction conditions were not changed.
Example 7
The Fe foil used in the reaction of step (2) was replaced with Zn foil, and the other reaction conditions were the same as in example 2.
Example 8
The Fe foil used in the reaction of step (2) was replaced with Cu foil, and the other reaction conditions were the same as in example 2.
Example 9
The Fe foil used in the reaction of step (2) was replaced with Ni foil, and the other reaction conditions were the same as in example 2.
Example 10
The Fe foil used in the reaction of step (2) was replaced with Al foil, and the other reaction conditions were the same as in example 2.
Example 11
Replacing HCl solution used in the reaction in the step (2) with HNO3Solution, other reaction conditions were the same as in example 2.
Example 12
Changing the HCl solution used in the reaction of the step (2) into H2SO4Solution, other reaction conditions were the same as in example 2.
Example 13
The concentration of the HCl solution used in the reaction of step (2) was changed to 0.1mol/L, and the other reaction conditions were the same as in example 2.
Example 14
The concentration of the HCl solution used in the reaction of step (2) was changed to 0.5mol/L, and the other reaction conditions were the same as in example 2.
Example 15
The concentration of the HCl solution used in the reaction of step (2) was changed to 1mol/L, and the other reaction conditions were the same as in example 2.
Example 16
The concentration of the HCl solution used in the reaction of step (2) was changed to 6mol/L, and the other reaction conditions were the same as in example 2.
Example 17
The reaction time in the reaction of step (2) was changed to 2 seconds, and the other reaction conditions were the same as in example 2.
Example 18
The reaction time in the reaction of step (2) was changed to 5 seconds, and the other reaction conditions were the same as in example 2.
Example 19
The reaction time in the reaction of step (2) was changed to 30 seconds, and the other reaction conditions were the same as in example 2.
Example 20
The reaction time in the reaction of step (2) was changed to 60 seconds, and the other reaction conditions were the same as in example 2.
Example 21
The reaction time in the reaction of step (2) was changed to 5 minutes, and the other reaction conditions were the same as in example 2.
Example 22
1)WO3The preparation process of the photoelectrode is as follows: 8.25g of sodium tungstate is weighed and dissolved in 1000mL of deionized water, and the solution is stirred for 10 minutes to obtain a transparent clear solution. 100mL of a 5mol/L HCl solution was added to the solution, and the mixture was stirred for 10 minutes to obtain a yellow tungstic acid suspension, and then 6.2g of ammonium oxalate was added to obtain a transparent clear solution. Putting the cleaned FTO conductive glass into the solution with the conductive surface facing downwards, and reacting in water bath at 60 ℃ for 12 hours to obtain bright yellow H2WO4And an electrode. H to be prepared2WO4The electrode was placed in a muffle furnace and annealed at 500 ℃ for 2 hours to give a pale yellow WO3And an electrode.
(2) Defect WO3The preparation process of the photoelectrode is as follows: the WO prepared in (1) is3The electrodes are connected with Al foil by wires, and WO is added3The electrode and the Al foil are immersed into a 3mol/L NaOH solution at the same time for reaction for 10 seconds, WO3Color of the electrodeGradually changing from light yellow to dark blue, washing the photoelectrode with deionized water and ethanol respectively, and drying to obtain the WO containing defects3And a photoelectrode.
Example 23
The electrolyte solution of step (2) in example 22 was changed to a KOH solution, and other reaction conditions were not changed.
Example 24
The electrolyte solution of step (2) in example 22 was changed to a LiOH solution, and other reaction conditions were not changed.
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 (4)
1. WO containing defects3The preparation method of the photoelectrode is characterized by comprising the following specific steps:
(1)WO3preparing a photoelectrode: adding a certain amount of HCl solution into sodium tungstate solution to obtain yellow tungstic acid turbid liquid, then adding a certain amount of ammonium oxalate to obtain transparent clear solution, putting the cleaned FTO conductive glass into the solution with the conductive surface facing downwards, and reacting for a certain time in water bath at a certain temperature to obtain bright yellow H2WO4Electrode, H to be prepared2WO4Annealing the electrode in a muffle furnace for a period of time to obtain a pale yellow WO3An electrode;
(2) defect WO3Preparing a photoelectrode: the WO prepared in (1) is3Connecting the electrodes to the metal foil with wires, and connecting the electrodes to the metal foil with the wires3The electrode and the metal foil are immersed into an electrolyte solution with a certain concentration for reaction for a certain time, WO3Gradually changing the color of the electrode from light yellow to dark blue, washing the photoelectrode with deionized water and ethanol respectively, and drying to obtain the WO containing defects3And a photoelectrode.
2. WO containing defects according to claim 13Method for producing photoelectrodeCharacterized in that: in the step (1), the molar ratio of sodium tungstate to hydrochloric acid to ammonium oxalate is 1: (5-20): (1-10), the water bath temperature is 50-80 ℃, the water bath time is 4-12 hours, the annealing temperature is 400-.
3. WO containing defects according to claim 13The preparation method of the photoelectrode is characterized in that: the electrolyte solution is acidic solution, and is one or mixed solution of hydrochloric acid, sulfuric acid, and nitric acid, the concentration of the electrolyte solution is 0.1-6mol/L, the metal sheet is Fe, Zn, Cu, Ni or Al, and the purity of the metal foil is>99 percent and reaction time of 2 seconds to 5 minutes.
4. WO containing defects according to claim 13The preparation method of the photoelectrode is characterized in that: the electrolyte solution is alkaline solution, and is one or mixture of KOH, NaOH and LiOH, the concentration of the electrolyte solution is 0.1-6mol/L, the metal foil used in the alkaline solution is Al foil, and the purity of the metal foil is high>99 percent and reaction time of 2 seconds to 5 minutes.
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| WO3/Ag复合薄膜的制备及其电致变色性能;苗壮等;《光子学报》;20191031;第48卷(第10期);1031001 * |
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