CN113044887B - 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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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 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 description 92
- 238000005286 illumination Methods 0.000 claims abstract description 18
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- 238000000034 method Methods 0.000 claims abstract description 7
- 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 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000004408 titanium dioxide Substances 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
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- 238000006243 chemical reaction Methods 0.000 claims description 7
- 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
- 238000010304 firing Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
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- 239000007772 electrode material Substances 0.000 claims description 4
- 239000008151 electrolyte solution Substances 0.000 claims description 4
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- 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
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 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
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- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
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- 238000001354 calcination Methods 0.000 abstract description 2
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- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
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- 238000006479 redox reaction Methods 0.000 description 1
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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- 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
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- H01G11/46—Metal oxides
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Abstract
The inventionRelates 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 Process 3 O 4 Calcining the precursor at 500 ℃ for 4 hours to obtain Co 3 O 4 Porous microspheres. Co synthesized by the above 3 O 4 Is a working electrode, a saturated Ag/AgCl electrode is a reference electrode, a Pt net is a counter electrode, and TiO is used 2 For the photo-assisted electrode, co was tested in 6M KOH 3 O 4 Electrochemical 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 and discharge efficiency, high power density and low cost, and is widely applied to the fields of energy storage and conversion, such as laser equipment, smart grid systems, hybrid electric vehicles, 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 the utilization of solar energy.
In recent years, as the core component of the super capacitor, many electrode materials with high performance, such as metal oxides, metal sulfides, metal hydroxides, porous carbon materials, etc., have been reported, have been extensively researched, synthesized and successfully applied to three types of super capacitorsIn an electrode system. Wherein, cobaltosic oxide is a variable valence transition metal oxide, can generate reversible oxidation-reduction reaction, is favorable for 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 the cobaltosic oxide porous microspheres are obtained and used as energy storage materials to be applied to a photo-assisted super capacitor.
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 light-assisted supercapacitor constructed by the method has the advantages that the specific capacitance before and after illumination is obviously improved, and meanwhile, 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 ·6H 2 Adding 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 first step, co (NO) is added according to the mol ratio 3 ) 2 ·6H 2 O：NaOH＝4-8：1。
In the first step, co (NO) is added according to the solid-to-liquid ratio 3 ) 2 ·6H 2 O: distilled water =11-60g:40mL.
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 an electrode material of a supercapacitor 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 application, the illumination condition is that a xenon lamp with 500W is used as a light source, and a filter with the wavelength range of less 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) According to the invention, titanium dioxide with a wide band gap (3.20 eV) is selected as the light auxiliary electrode, so that the titanium dioxide has good biocompatibility, high electron mobility and chemical stability, is easy to modify the surface, and can be obtained in a simple and low-cost manner.
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 light-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 graph comparing specific capacitance values of a 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 of a cobaltosic oxide precursor comprises the following steps: 116.4g of Co (NO) 3 ) 2 ·6H 2 O 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 (polyvinylidene fluoride) dissolved in 1mL of absolute ethanol, transferring 125 mu L of mixed solution by using a liquid transfer gun, and dripping the mixed solution to 1cm 2 ×1cm 2 Drying the foamed nickel in an infrared drying oven; subsequently, the mixture was processed at 10MPa for 5 minutes using a tablet press. The loading capacity of the cobaltosic oxide porous microspheres on each working electrode is about 1mg, and the electrode area and the loading 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 5min. Then, 0.5mL of tetrabutyl titanate was added to the above solution and stirred for 5min. 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 incident light wavelength range is controlled in a visible light region by an optical filter with the wavelength smaller than 400nm, 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 irradiation. 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: charge and discharge 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, after illumination, the highest specific capacitance value can reach 352F/g, which is higher than 317F/g when the illumination is not performed. After illumination, the specific capacitance value is improved by 11%.
Claims (7)
1. The application of the cobaltosic oxide porous microspheres in the photo-assisted supercapacitor is characterized in that the method comprises the following steps: in a three-electrode system, titanium dioxide is used as a light auxiliary electrode, and cobaltosic oxide porous microspheres are used as an electrode material of a supercapacitor for illumination;
the preparation method of the cobaltosic oxide porous microsphere comprises the following steps:
the method comprises the following steps: cobaltosic oxide precursor: mixing Co (NO) 3 ) 2 ·6H 2 Adding 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: 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 cobaltosic oxide porous microspheres;
in the first step, the reactant is dispersed in distilled water, transferred to a high-pressure reaction kettle and reacted for 5 hours at 180 ℃;
in the second step, the firing temperature in the muffle furnace is 500 ℃, and the firing time is 4h.
2. The use as claimed in claim 1, wherein in step one, co (NO) is added in molar ratio 3 ) 2 ·6H 2 O：NaOH=4-8：1。
3. The use according to claim 2, wherein in step one, co (NO) is used as a solid-to-liquid ratio 3 ) 2 ·6H 2 O: distilled water =11-160 g:40 And (mL).
4. The application of claim 1, 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 6M KOH is used as an electrolyte solution.
5. The application of the porous working electrode as claimed in claim 4, wherein the preparation method of the working electrode comprises the steps of dissolving cobaltosic oxide porous microspheres, carbon black and PVDF in absolute ethyl alcohol to obtain a mixed solution, dripping the mixed solution onto foamed nickel, drying, and tabletting to obtain the working electrode.
6. The use according to claim 5, wherein the titanium dioxide photo-assisted electrode is prepared by adding tetrabutyl titanate into hydrochloric acid solution, stirring the mixed solution, transferring the mixed solution into an autoclave lined with polytetrafluoroethylene, placing the autoclave with FTO glass conductive surface facing downwards, reacting at 150 ℃ for 20h, cooling to room temperature, and washing to obtain the titanium dioxide photo-assisted electrode.
7. The use according to claim 6, wherein the lighting conditions are such that a 500W xenon lamp is used as the 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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| CN106856152A (en) * | 2015-12-09 | 2017-06-16 | 中国科学院上海高等研究院 | Light strengthens electrochemical energy storing device structure and method |
| CN108010740A (en) * | 2017-11-24 | 2018-05-08 | 北京欧美中科学技术研究院 | A kind of ultracapacitor |
| CN108470645B (en) * | 2018-04-09 | 2020-04-28 | 济南大学 | Flexible micro super capacitor and manufacturing method thereof |
| CN108597893B (en) * | 2018-05-28 | 2020-08-28 | 江苏大学 | Preparation method of supercapacitor composite electrode material based on foamed nickel |
| CN110323071B (en) * | 2019-05-10 | 2020-09-04 | 北京化工大学 | Titanium dioxide and cobalt-aluminum hydrotalcite heterojunction inorganic composite material and application thereof as photo-charging supercapacitor |
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