CN113044887A - Cobaltosic oxide porous microsphere, preparation method thereof and application thereof in photo-assisted supercapacitor - Google Patents
Cobaltosic oxide porous microsphere, preparation method thereof and application thereof in photo-assisted supercapacitor Download PDFInfo
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- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000004005 microsphere Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005286 illumination Methods 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 239000003990 capacitor Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 5
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000004408 titanium dioxide Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000007772 electrode material Substances 0.000 claims description 4
- 239000008151 electrolyte solution Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
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- 238000006479 redox reaction Methods 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/00—Particle morphology
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- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- 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
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Abstract
The invention relates to a photo-assisted super capacitor and a preparation method thereof. Belongs to the technical field of energy materials. The technical scheme is as follows: synthesis of Co by a one-step hydrothermal Process3O4Calcining the precursor at 500 ℃ for 4 hours to obtain Co3O4Porous microspheres. Co synthesized by the above3O4Is a working electrode, a saturated Ag/AgCl electrode is a reference electrode, a Pt net is a counter electrode, and TiO is used2For the photo-assisted electrode, Co was tested in 6M KOH3O4Electrochemical properties of the porous microspheres before and after illumination. After the photo-assisted supercapacitor prepared by the method is illuminated, the specific capacitance value can reach 352F/g, and is increased by 11% compared with that of the photo-assisted supercapacitor without illumination (317F/g).
Description
Technical Field
The invention belongs to the technical field of energy materials, and particularly relates to cobaltosic oxide porous microspheres, a preparation method thereof and application thereof in a photo-assisted supercapacitor.
Background
With the increasing concern over energy and environmental issues, there is an urgent need to improve the conversion and storage of electrochemical energy. The super capacitor has long cycle life, high charge-discharge efficiency, high power density and low cost, and is widely applied to the field of energy storage and conversion, such as laser equipment, a smart grid system, a hybrid electric vehicle, portable electronic equipment and the like. Solar energy is considered as the most promising energy source due to high abundance, good accessibility and high cleanliness, and is widely applied to the fields of catalysis, photoelectric devices, energy conversion and the like. Among them, a photo-assisted charging energy storage device, such as a photo-assisted super capacitor, is an effective way to realize solar energy utilization.
In recent years, as the core component of the super capacitor, a plurality of electrode materials with high performance, such as metal oxides, metal sulfides, metal hydroxides, porous carbon materials, etc., have been reported, and have been widely researched, synthesized and successfully applied to a three-electrode system. Wherein, the cobaltosic oxide is a variable valence transition metal oxide, can generate reversible oxidation-reduction reaction, is beneficial to charge storage, and has higher theoretical capacitance (3560F/g)-1) And is favored by most researchers. However, their poor conductivity limits the practical application of energy storage.
Disclosure of Invention
The invention aims to provide a preparation method with simple method and low price aiming at the insufficient energy storage capacity of a super capacitor, and cobaltosic oxide porous microspheres are obtained and used as energy storage materials to be applied to photo-assisted super capacitors.
The photo-assisted supercapacitor prepared by the invention takes cobaltosic oxide porous microspheres as a working electrode, saturated Ag/AgCl as a reference electrode, a Pt net as a counter electrode, titanium dioxide as a photo-assisted electrode and 6M KOH as an electrolyte solution. The specific capacitance value of the light-assisted supercapacitor constructed by the invention before and after illumination is obviously improved, and the light-assisted supercapacitor also has excellent performances in cycle stability, energy density and power density.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of cobaltosic oxide porous microspheres comprises the following steps:
the method comprises the following steps: cobaltosic oxide precursor: mixing Co (NO)3)2·6H2Adding O and NaOH into distilled water at the same time, stirring and dissolving, transferring the whole system into a high-pressure kettle for reaction, cooling to room temperature, filtering, washing, and drying in vacuum to obtain a cobaltosic oxide precursor;
step two: cobaltosic oxide porous microspheres: and (4) firing the cobaltosic oxide precursor obtained in the step one in a muffle furnace, taking out the cobaltosic oxide precursor, and cooling to room temperature to obtain the cobaltosic oxide porous microspheres.
In the step one, Co (NO) is added according to the molar ratio3)2·6H2O:NaOH=4-8:1。
In the first step, Co (NO) is added according to the solid-to-liquid ratio3)2·6H2O: distilled water 11-60 g: 40 mL.
In the step one, the reactant is dispersed in distilled water, and the mixture is transferred to a high-pressure reaction kettle to react for 5 hours at 180 ℃.
In the second step, the firing temperature in the muffle furnace is 500 ℃, and the firing time is 4 hours.
The application of any cobaltosic oxide porous microsphere in the photo-assisted supercapacitor is as follows: in a three-electrode system, titanium dioxide is used as a light auxiliary electrode, and cobaltosic oxide porous microspheres are used as electrode materials of a super capacitor for illumination.
In the application, the three-electrode system takes foamed nickel loaded with cobaltosic oxide porous microspheres as a working electrode of a super capacitor, saturated Ag/AgCl as a reference electrode, a Pt net as a counter electrode and 6M KOH as an electrolyte solution.
In the application, the preparation method of the working electrode comprises the steps of weighing cobaltosic oxide porous microspheres, carbon black and PVDF, dissolving in absolute ethyl alcohol to obtain a mixed solution, transferring the mixed solution, dropwise adding the mixed solution onto foamed nickel, drying, and tabletting to obtain the working electrode.
The preparation method of the titanium dioxide photo-assisted electrode comprises the steps of adding tetrabutyl titanate into a hydrochloric acid solution, stirring the mixed solution, transferring the stirred mixed solution into an autoclave lined with polytetrafluoroethylene, placing the FTO glass in the autoclave with the conductive surface facing downwards, reacting for 20 hours at 150 ℃, cooling to room temperature, and washing to obtain the titanium dioxide photo-assisted electrode.
In the above application, the illumination condition is that a 500W xenon lamp is used as a light source, and a filter with a wavelength smaller than 400nm controls the wavelength range of incident light in a visible light region.
Compared with the prior art, the invention has the following remarkable advantages:
1) according to the invention, the cobaltosic oxide porous microspheres are prepared by a hydrothermal method, the process is simple, the operation is easy, and the cost is low.
2) The invention selects titanium dioxide with wide band gap (3.20eV) as the light auxiliary electrode, has good biocompatibility, high electron mobility and chemical stability, is easy for surface modification, and can be obtained by a simple and low-cost mode.
3) The invention designs a novel light-assisted super capacitor which utilizes electric energy and solar energy to charge and store energy. The research provides a new idea for the development of photosensitive energy devices and promotes the effective utilization of solar energy.
Drawings
Fig. 1 is a scanning electron microscope image of cobaltosic oxide porous microspheres.
Fig. 2 is an XRD pattern of the cobaltosic oxide porous microspheres.
Fig. 3 is a schematic diagram of a photo-assisted supercapacitor applied in a three-electrode system.
Fig. 4 is an ultraviolet-visible diffuse reflectance spectrum of a titanium dioxide photo-assisted electrode.
FIG. 5 is a cyclic voltammogram of a photo-assisted supercapacitor at 50mV/s in a three-electrode system.
FIG. 6(a) is a constant current charge and discharge curve of a photo-assisted supercapacitor at 2A/g in a three-electrode system.
FIG. 6(b) is a graph of the discharge of a photo-assisted supercapacitor at 2A/g in a three-electrode system.
Fig. 7 is a comparison graph of specific capacitance values of the photo-assisted supercapacitor at different current densities in a three-electrode system.
Detailed Description
Example 1 preparation of porous Cobaltosic oxide microspheres
The preparation method comprises the following steps:
the preparation method comprises the following steps: 116.4g of Co (NO)3)2·6H2O and 0.8g NaOH were simultaneously added to 40mL of distilled water, and the mixture was sufficiently stirred. After complete dissolution, the whole system was transferred to an autoclave and allowed to react at 180 ℃ for 5 hours. After naturally cooling to room temperature, the resulting product was washed several times with ethanol and deionized water, and then dried at 60 ℃ for 24 hours. Obtaining the cobaltosic oxide precursor.
Step two, preparing the cobaltosic oxide porous microspheres: and (3) placing the obtained dried cobaltosic oxide precursor in a muffle furnace, calcining for 4 hours at 500 ℃, taking out, and cooling to room temperature to obtain the cobaltosic oxide porous microspheres. As shown in figure 1, the particle size of the cobaltosic oxide porous microspheres is 10-20 nm, and the particle size is uniform. The corresponding XRD data are shown in figure 2, the prepared sample has good correspondence with the diffraction peak of cobaltosic oxide (JCPDS No. 43-1003), and no impurity peak exists, which indicates that the cobaltosic oxide material is successfully synthesized in the embodiment.
Example 2 application of Cobaltosic oxide porous microspheres in supercapacitor
The preparation method of the electrode comprises the following steps:
the preparation method comprises the following steps: weighing 8mg of cobaltosic oxide porous microspheres, 1mg of carbon black and 1mg of PVDF, dissolving in 1mL of absolute ethanol, transferring 125 mu L of mixed solution by using a liquid transfer gun, and dropwise adding the mixed solution to 1cm2×1cm2On the foamed nickel and dried in an infrared drying oven(ii) a Subsequently, the mixture was processed at 10MPa for 5 minutes using a tablet press. The load capacity of the cobaltosic oxide porous microspheres on each working electrode is about 1mg, and the electrode area and the load capacity can be expanded according to the corresponding proportion.
Step two, preparing a titanium dioxide photo-assisted electrode: 15mL of concentrated hydrochloric acid was added to 15mL of deionized water, and the mixture was stirred at room temperature for 5 min. Then, 0.5mL of tetrabutyl titanate was added to the above solution and stirred for 5 min. The mixed solution was transferred to an autoclave lined with polytetrafluoroethylene, and an FTO glass conductive surface was placed in the autoclave, facing down, and reacted at 150 ℃ for 20 hours. And naturally cooling to room temperature, and washing with deionized water for several times to obtain the titanium dioxide photo-assisted electrode. The ultraviolet-visible diffuse reflection test was performed thereon, and the results are shown in fig. 4. The initial response position of the titanium dioxide to the ultraviolet-visible light can be observed to be ultraviolet light with the wavelength of about 410nm, which shows that the titanium dioxide has good response to the visible light.
A500W xenon lamp is used as a light source, an optical filter with the wavelength range of less than 400nm controls the wavelength range of incident light in a visible light region, and the cobaltosic oxide porous microspheres are applied to an electrode material of a photo-assisted supercapacitor. As shown in FIG. 3, cobaltosic oxide porous microspheres are used as a working electrode, saturated Ag/AgCl is used as a reference electrode, a Pt net is used as a counter electrode, titanium dioxide is used as a light auxiliary electrode, and 6M KOH is used as an electrolyte solution.
And (3) detection:
1) cyclic voltammetric analysis of photo-assisted supercapacitors
FIG. 5 is a plot of cyclic voltammetry for a photo-assisted supercapacitor before and after exposure to light at a sweep rate of 50 mV/s. It can be seen that the cyclic voltammograms both show a pair of redox peaks before and after the light exposure. At the same scan speed, the integrated area of the cyclic voltammogram after illumination is larger than that without illumination, i.e. the photocurrent generated under illumination is much larger than that generated under non-illumination, which indicates that the specific capacitance is significantly increased because the integrated area of the cyclic voltammogram is proportional to the number of charges passed during scanning.
2) Constant-current charging and discharging curve analysis of photo-assisted supercapacitor
FIG. 6 is a constant current charge and discharge curve diagram of the photo-assisted supercapacitor before and after illumination at a current density of 2A/g. It can be observed that the charge-discharge time is significantly enhanced after illumination. As can be seen from the interpolation graph, the discharge time increases after illumination, indicating that the specific capacitance value is improved after illumination.
3) Specific capacitance performance analysis of light-assisted supercapacitor
The formula is calculated from the following specific capacitance C (F/g):
wherein, I: charge-discharge current (A)
Δ t: discharge time(s)
m: mass (g) of Cobaltosic oxide loaded on foamed Nickel
Δ V: charging and discharging voltage (V)
The specific capacitance values of the photo-assisted supercapacitor before and after illumination were calculated, as shown in fig. 7. Under 2A/g, the highest specific capacitance value can reach 352F/g after illumination, which is higher than 317F/g when the illumination is not performed. After illumination, the specific capacitance value is improved by 11%.
Claims (10)
1. The cobaltosic oxide porous microsphere is characterized in that the preparation method comprises the following steps:
the method comprises the following steps: cobaltosic oxide precursor: mixing Co (NO)3)2·6H2Adding O and NaOH into distilled water at the same time, stirring and dissolving, transferring the whole system into a high-pressure kettle for reaction, cooling to room temperature, filtering, washing, and drying in vacuum to obtain a cobaltosic oxide precursor;
step two: cobaltosic oxide porous microspheres: and (4) firing the cobaltosic oxide precursor obtained in the step one in a muffle furnace, taking out the cobaltosic oxide precursor, and cooling to room temperature to obtain the cobaltosic oxide porous microspheres.
2. The porous cobaltosic oxide microspheres according to claim 1, wherein the porous cobaltosic oxide microspheres are prepared by mixing a mixture of aIn step one, in terms of molar ratio, Co (NO)3)2·6H2O:NaOH=4-8:1。
3. The porous cobaltosic oxide microspheres of claim 2, wherein in the first step, Co (NO) is added in a solid-to-liquid ratio3)2·6H2O: distilled water 11-160 g: 40 mL.
4. The porous cobaltosic oxide microspheres of claim 3, wherein in the first step, the reactant is dispersed in distilled water, transferred to an autoclave and reacted at 180 ℃ for 5 hours.
5. The porous cobaltosic oxide microspheres of claim 4, wherein in the second step, the firing temperature in the muffle furnace is 500 ℃ and the firing time is 4 hours.
6. The use of any of the cobaltosic oxide porous microspheres of claims 1-5 in a photo-assisted supercapacitor, characterized in that the method is as follows: in a three-electrode system, titanium dioxide is used as a light auxiliary electrode, and cobaltosic oxide porous microspheres are used as electrode materials of a super capacitor for illumination.
7. The application of claim 6, wherein the three-electrode system is characterized in that foamed nickel loaded with cobaltosic oxide porous microspheres is used as a working electrode of a supercapacitor, saturated Ag/AgCl is used as a reference electrode, a Pt net is used as a counter electrode, and 6MKOH is used as an electrolyte solution.
8. The application of claim 7, wherein the working electrode is prepared by dissolving cobaltosic oxide porous microspheres, carbon black and PVDF in absolute ethanol to obtain a mixed solution, dripping the mixed solution on foamed nickel, drying, and tabletting.
9. The use according to claim 8, wherein the titania photo-assisted electrode is prepared by adding tetrabutyl titanate to a hydrochloric acid solution, stirring the mixed solution, transferring the stirred mixed solution into an autoclave lined with polytetrafluoroethylene, placing the autoclave with the FTO glass conductive surface facing downward, reacting at 150 ℃ for 20 hours, cooling to room temperature, and washing to obtain the titania photo-assisted electrode.
10. The use according to claim 9, wherein the light irradiation conditions are such that a 500W xenon lamp is used as a light source and a filter of less than 400nm controls the wavelength range of the incident light in the visible region.
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