CN112700969B - Sheet CeO2/Co1.29Ni1.71O4 electrode material and preparation method thereof - Google Patents
Sheet CeO2/Co1.29Ni1.71O4 electrode material and preparation method thereof Download PDFInfo
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- CN112700969B CN112700969B CN202011426878.3A CN202011426878A CN112700969B CN 112700969 B CN112700969 B CN 112700969B CN 202011426878 A CN202011426878 A CN 202011426878A CN 112700969 B CN112700969 B CN 112700969B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a flaky CeO2/Co1.29Ni1.71O4An electrode material and a preparation method thereof, belonging to the technical field of electrode materials. The method comprises the following specific steps: ultrasonically cleaning and drying the foamed nickel to obtain clean foamed nickel; adding sodium dodecyl sulfate, urea, nickel nitrate and cobalt nitrate into water for dissolving, then dropwise adding a cerous nitrate aqueous solution to form a uniform solution, then adding foamed nickel for hydrothermal reaction, washing the reacted foamed nickel with water, washing with ethanol, drying, and oxidizing to obtain flaky CeO2/Co1.29Ni1.71O4An electrode material. The method is simple, the price of reactants is low, the preparation process is convenient, and the energy consumption is low. CeO prepared by the invention2/Co1.29Ni1.71O4The surface of the electrode material has a folded sheet structure, the specific surface area is large, the electrochemical performance is excellent, and the electrode material is suitable for the electrode material of the super capacitor.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and particularly relates to flaky CeO2/Co1.29Ni1.71O4An electrode material and a preparation method thereof, wherein the material is used as an electrode material of a super capacitor.
Background
With the progress of energy transformation, the demand of renewable intermittent energy matching equipment is increasingly seen, so that the society urgently searches for an efficient and environment-friendly energy storage device. As a novel energy storage device, the super capacitor has the advantages of long cycle life, instantaneous power maintenance, high-power pulse application and the like, is wide in application scene, can be used for various industrial equipment, and therefore an electrode material with high specific capacitance needs to be prepared, so that the performance of the super capacitor is improved.
The transition metal oxide has the advantages of high specific capacitance, good reversibility, multiple oxidation states in redox reaction, higher electrochemical activity and the like, so that the transition metal oxide is an excellent electrode material and is widely applied. However, most metal compounds have poor conductivity and cycling stability, thereby affecting the performance of the supercapacitor.
Disclosure of Invention
In order to solve the above problems, the present invention discloses a sheet-shaped CeO as a supercapacitor material2/Co1.29Ni1.71O4An electrode material and a preparation method thereof. The preparation method has simple process, and CeO growing on the foamed nickel is obtained by a one-step hydrothermal method and oxidation2/Co1.29Ni1.71O4A material. The price of the reactant is low and green, the surfactant is biodegradable and environment-friendly, and the obtained CeO2/Co1.29Ni1.71O4The electrode material has a high specific capacitance.
The technical scheme of the invention is as follows:
flaky CeO2/Co1.29Ni1.71O4The electrode material is characterized in that a folded sheet structure is longitudinally grown on the surface of three-dimensional reticular foamed nickel, the sheet structure is thin and is uniformly distributed at intervals, and CeO is doped2To improve the conductivity at the interface between the electrolyte and the active material, thereby improving the electrochemical performance of the electrode; the electrode material is directly grown on the foamed nickel substrate, so that the conductivity and stability of the material are obviously enhanced.
Flaky CeO2/Co1.29Ni1.71O4The preparation method of the electrode material comprises the following steps:
(1) cleaning of foamed nickel
And (2) placing the foamed nickel in hydrochloric acid for ultrasonic cleaning, then placing the foamed nickel in deionized water for continuous ultrasonic cleaning, finally placing the foamed nickel in absolute ethyl alcohol for ultrasonic cleaning, and drying in vacuum at 50-60 ℃ to obtain clean foamed nickel.
The pore size of the nickel foam is 110ppi, and the length x width x height is 30mm x 10mm x 1.5 mm.
The ultrasonic cleaning time is 10-15 min.
The concentration of the hydrochloric acid is 1-2M.
(2) Stirring to obtain uniform solution
Adding sodium dodecyl sulfate, urea, nickel nitrate hexahydrate and cobalt nitrate hexahydrate into deionized water, and stirring to dissolve the sodium dodecyl sulfate, the urea, the nickel nitrate hexahydrate and the cobalt nitrate hexahydrate; and adding 10mL of cerium nitrate aqueous solution under stirring, and then continuously stirring for 60-90 min to obtain a uniform solution.
The addition amount of the sodium dodecyl sulfate is 0.05-0.055 g, and the mass ratio of cobalt nitrate hexahydrate to nickel nitrate hexahydrate is 1: 1, the adding amount of the urea is 0.045-0.055 g, and the concentration of the cerium nitrate aqueous solution is 1.84-3.68 mmol/L.
(3) The foam nickel and the uniform solution are subjected to hydrothermal reaction to obtain a first-step product
Pouring the foamed nickel obtained in the step (1) and the uniform solution obtained in the step (2) into a reaction kettle, carrying out hydrothermal reaction at 170-180 ℃, and obtaining a first-step product after 10-13 h.
The reaction temperature of the hydrothermal reaction is preferably 170 ℃, and the reaction time is preferably 12 hours.
(4) Washing the product obtained in the first step in the step (3) with water and ethanol, oxidizing the washed product in a muffle furnace at 300-400 ℃ for 2-4 h to obtain flaky CeO2/Co1.29Ni1.71O4An electrode material.
The invention has the beneficial effects that: 1) in the preparation process of the material, a hydrothermal method is adopted, the preparation process is simple to operate, and the requirement on synthesis conditions is low. 2) The raw materials are low in price and environment-friendly, and the performance of the electrode is improved by doping a proper amount of cerium. 3) The foamed nickel is used as a substrate to effectively relieve the defects of poor conductivity and poor cycling stability of the traditional metal oxide electrode material.
Drawings
FIG. 1 shows a flaky CeO prepared according to the present invention2/Co1.29Ni1.71O4Scanning electron micrographs of the electrode material.
FIGS. 2(a) to 2(d) are flaky CeO prepared by the present invention2/Co1.29Ni1.71O4Mapping element distribution diagram of the electrode material; in fig. 2(a), the distribution diagram of three elements, i.e., Ni, Co, and Ce, fig. 2(b), the distribution diagram of Ce, fig. 2(c), and the distribution diagram of Ni are shown, respectively.
FIG. 3(a)) FIG. 3(d) is a sheet-like CeO prepared according to the present invention2/Co1.29Ni1.71O4XPS plot of electrode material; wherein, fig. 3(a) is a full spectrum, fig. 3(b) is a spectrum of O1s, fig. 3(c) is a spectrum of Ce3d and Ni2p, and fig. 3(d) is a spectrum of Co2 p.
FIG. 4 shows a flaky CeO prepared by the present invention2/Co1.29Ni1.71O4Electrode material with current density of 1Ag-1Lower constant current charge-discharge diagram.
Detailed Description
The invention is further described below with reference to examples and figures.
Example 1
Cutting foamed nickel with the aperture of 110ppi and the diameter of 30mm multiplied by 10mm multiplied by 1.5mm, soaking in 2M HCL for ultrasonic cleaning for 15min, then performing ultrasonic cleaning for 10min by deionized water, finally performing ultrasonic cleaning for 10min by absolute ethyl alcohol, and drying the foamed nickel subjected to ultrasonic cleaning for 12h at the temperature of 60 ℃ in vacuum.
Weighing 0.050g of sodium dodecyl sulfate, 0.050g of urea, 0.116g of nickel nitrate hexahydrate and 0.116g of cobalt nitrate hexahydrate, dissolving in 20mL of deionized water, and stirring for 20min to obtain an initial solution; weighing 0.012g of cerous nitrate hexahydrate to be dissolved in 10mL of deionized water to obtain a cerous nitrate aqueous solution with the concentration of 2.76 mmol/L; and slowly dropwise adding a cerous nitrate aqueous solution into the initial solution under stirring, and continuously stirring for 1h to obtain a uniform solution.
Transferring the dried foam nickel and the uniform solution into a reaction kettle, reacting for 12 hours at 170 ℃, washing the reacted foam nickel with water and ethanol, drying, and oxidizing for 2 hours at 300 ℃ in a muffle furnace to obtain flaky CeO2/Co1.29Ni1.71O4An electrode material.
FIG. 1 is a prepared CeO2/Co1.29Ni1.71O4Scanning electron micrograph of the electrode material, from which CeO can be seen2/Co1.29Ni1.71O4The electrode material is in the form of a sheet.
FIG. 2(a) to FIG. 2(d) are prepared flake-shaped CeO2/Co1.29Ni1.71O4Mapping elemental distribution of the electrode material, elemental distribution can be seen in FIGS. 2(a) - (d)Is very uniform.
FIGS. 3(a) to 3(d) are prepared CeO2/Co1.29Ni1.71O4XPS diagram of electrode material, FIG. 3(a) shows that the electrode material contains Ce, Co, Ni, O elements, and Ce3d diagram of FIG. 3(b) shows that the electrode material contains Ce3+And Ce4+Is apparent as CeO2In the presence of Ce3+And Ce4+，Ce3+Indicates oxygen vacancies, thereby increasing conductivity and facilitating redox reactions. The peaks at 855.7eV and 873.4eV in the Ni2p spectrum of FIG. 3(c) correspond to Ni3+. The peaks at 780.3eV and 795.6eV in the Co2p spectrum of FIG. 3(d) correspond to Co2+. FIG. 3(b) the spectrum of O1s, 531.4eV shows a defect site with low oxygen coordination, 529.5eV shows a typical metal-oxygen bond.
FIG. 4 is a prepared CeO2/Co1.29Ni1.71O4Electrode material in 1Ag-1The constant current charge-discharge diagram can be calculated by the discharge time and the specific capacitancespCalculating electrode material at 1Ag ═ It/S.DELTA.V-1Specific capacitance of 1488Fg-1The galvanostatic charge-discharge curve shows good symmetry, indicating an excellent reversible redox reaction.
Example 2
Cutting foamed nickel with the aperture of 110ppi and the diameter of 30mm multiplied by 10mm multiplied by 1.5mm, soaking in 1M HCL for ultrasonic cleaning for 10min, then performing ultrasonic cleaning for 10min by deionized water, finally performing ultrasonic cleaning for 10min by absolute ethyl alcohol, and drying the foamed nickel subjected to ultrasonic cleaning for 12h at the temperature of 60 ℃ in vacuum.
Weighing 0.055g of sodium dodecyl sulfate, 0.050g of urea, 0.185g of nickel nitrate hexahydrate and 0.185g of cobalt nitrate hexahydrate, dissolving in 20mL of deionized water, and stirring for 20min to obtain an initial solution; weighing 0.008 g of cerous nitrate hexahydrate to be dissolved in 10mL of deionized water to obtain a cerous nitrate aqueous solution with the concentration of 1.84 mmol/L; and slowly dropwise adding a cerous nitrate aqueous solution into the initial solution under stirring, and continuously stirring for 1h to obtain a uniform solution.
Transferring the dried foam nickel and the uniform solution into a reaction kettle to react for 11h at 170 ℃, washing the reacted foam nickel with water and ethanol, drying and oxidizing for 3h at 300 ℃ to obtain flaky CeO2/Co1.29Ni1.71O4An electrode material.
Example 3
Cutting foamed nickel with the aperture of 110ppi and the diameter of 30mm multiplied by 10mm multiplied by 1.5mm, soaking in 2M HCL for ultrasonic cleaning for 15min, then performing ultrasonic cleaning for 10min by deionized water, finally performing ultrasonic cleaning for 10min by absolute ethyl alcohol, and drying the foamed nickel subjected to ultrasonic cleaning for 12h at the temperature of 60 ℃ in vacuum.
Weighing 0.050g of sodium dodecyl sulfate, 0.055g of urea, 0.245g of nickel nitrate hexahydrate and 0.245g of cobalt nitrate hexahydrate, dissolving in 20mL of deionized water, and stirring for 20min to obtain an initial solution; weighing 0.016 g of cerous nitrate hexahydrate to be dissolved in 10mL of deionized water to obtain a cerous nitrate aqueous solution with the concentration of 3.68 mmol/L; slowly dropwise adding a cerous nitrate aqueous solution into the initial solution under stirring, continuously stirring for 1.5h to obtain a uniform solution, transferring the dried foamed nickel and the uniform solution into a reaction kettle for reaction at 180 ℃ for 12h, washing the reacted foamed nickel with water and ethanol, drying, and oxidizing at 300 ℃ for 4h to obtain flaky CeO2/Co1.29Ni1.71O4An electrode material.
Example 4
Cutting foamed nickel with the aperture of 110ppi and the diameter of 30mm multiplied by 10mm multiplied by 1.5mm, soaking in 2M HCL for ultrasonic cleaning for 15min, then performing ultrasonic cleaning for 15min by deionized water, finally performing ultrasonic cleaning for 15min by absolute ethyl alcohol, and drying the foamed nickel subjected to ultrasonic cleaning for 12h at the temperature of 60 ℃ in vacuum.
Weighing 0.050g of sodium dodecyl sulfate, 0.045g of urea, 0.3g of nickel nitrate hexahydrate and 0.3g of cobalt nitrate hexahydrate, dissolving in 20mL of deionized water, and stirring for 20min to obtain an initial solution; weighing 0.012g of cerous nitrate hexahydrate to be dissolved in 10mL of deionized water to obtain a cerous nitrate aqueous solution with the concentration of 2.76 mmol/L; and slowly dropwise adding a cerous nitrate aqueous solution into the initial solution under stirring, and continuously stirring for 1.5h to obtain a uniform solution.
Transferring the dried foamed nickel and the uniform solution into a reaction kettle to react for 13h at 180 ℃, washing the foamed nickel after reaction with water and ethanol, drying, and oxidizing for 2h at 350 ℃ to obtain flaky CeO2/Co1.29Ni1.71O4An electrode material.
Example 5
Cutting foamed nickel with the aperture of 110ppi and the diameter of 30mm multiplied by 10mm multiplied by 1.5mm, soaking in 2M HCL for ultrasonic cleaning for 15min, then performing ultrasonic cleaning for 10min by deionized water, finally performing ultrasonic cleaning for 10min by absolute ethyl alcohol, and drying the foamed nickel subjected to ultrasonic cleaning for 12h at the temperature of 60 ℃ in vacuum.
Weighing 0.055g of sodium dodecyl sulfate, 0.050g of urea, 0.18g of nickel nitrate hexahydrate and 0.18g of cobalt nitrate hexahydrate, dissolving in 20mL of deionized water, stirring for 20min to obtain an initial solution, weighing 0.01g of cerous nitrate hexahydrate, and dissolving in 10mL of deionized water to obtain a cerous nitrate aqueous solution with the concentration of 2.30 mmol/L; and slowly dropwise adding a cerous nitrate aqueous solution into the initial solution under stirring, and continuously stirring for 1h to obtain a uniform solution.
Transferring the dried foam nickel and the uniform solution into a reaction kettle to react for 10 hours at 170 ℃, washing the reacted foam nickel with water and ethanol, drying and oxidizing for 3 hours at 400 ℃ to obtain flaky CeO2/Co1.29Ni1.71O4An electrode material.
Claims (9)
1. Flaky CeO2/Co1.29Ni1.71O4A method for preparing an electrode material, characterized in that the method comprises the steps of:
(1) cleaning of foamed nickel
Placing the foamed nickel in hydrochloric acid for ultrasonic cleaning, then placing the foamed nickel in deionized water for continuous ultrasonic cleaning, finally placing the foamed nickel in absolute ethyl alcohol for ultrasonic cleaning, and performing vacuum drying to obtain clean foamed nickel;
(2) stirring to obtain uniform solution
Adding sodium dodecyl sulfate, urea, nickel nitrate hexahydrate and cobalt nitrate hexahydrate into deionized water, and stirring to dissolve the sodium dodecyl sulfate, the urea, the nickel nitrate hexahydrate and the cobalt nitrate hexahydrate; adding 10mL of cerium nitrate aqueous solution under stirring, and then continuously stirring to obtain a uniform solution;
the addition amount of the sodium dodecyl sulfate is 0.05-0.055 g, and the mass ratio of cobalt nitrate hexahydrate to nickel nitrate hexahydrate is 1: 1, the adding amount of urea is 0.045-0.055 g, and the concentration of the cerium nitrate aqueous solution is 1.84-3.68 mmol/L;
(3) the foam nickel and the uniform solution are subjected to hydrothermal reaction to obtain a first-step product
Pouring the foamed nickel obtained in the step (1) and the uniform solution obtained in the step (2) into a reaction kettle, carrying out hydrothermal reaction at 170-180 ℃, and obtaining a first-step product after 10-13 h;
(4) washing the product obtained in the first step in the step (3) with water and ethanol, oxidizing the washed product for 2-4 hours at the temperature of 300-400 ℃ to obtain flaky CeO2/Co1.29Ni1.71O4An electrode material.
2. The production method according to claim 1, wherein in the step (1), the nickel foam has a pore size of 110ppi and a length x width x height of 30mm x 10mm x 1.5 mm.
3. The production method according to claim 1 or 2, wherein in the step (3), the reaction temperature of the hydrothermal reaction is 170 ℃ and the reaction time is 12 hours.
4. The preparation method according to claim 1 or 2, wherein in the step (1), the concentration of hydrochloric acid is 1-2M, the ultrasonic cleaning time is 10-15 min, and the vacuum drying temperature is 50-60 ℃.
5. The preparation method according to claim 3, wherein in the step (1), the concentration of hydrochloric acid is 1-2M, the ultrasonic cleaning time is 10-15 min, and the vacuum drying temperature is 50-60 ℃.
6. The method according to claim 1, 2 or 5, wherein in the step (2), the time for stirring after adding the aqueous solution of cerium nitrate is 60 to 90 min.
7. The preparation method according to claim 3, wherein in the step (2), the time for stirring after adding the aqueous solution of cerium nitrate is 60 to 90 min.
8. The preparation method according to claim 4, wherein in the step (2), the time for stirring after adding the aqueous solution of cerium nitrate is 60 to 90 min.
9. Flake-shaped CeO prepared by the preparation method of any one of claims 1 to 82/Co1.29Ni1.71O4The electrode material is characterized in that the electrode material is a three-dimensional reticular foam nickel surface with a longitudinally-grown wrinkled sheet structure, and the sheet structure is uniformly distributed at intervals.
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| CN103594253A (en) * | 2013-11-21 | 2014-02-19 | 东华大学 | Method for preparing porous NiCo2O4/MnO2 nuclear shell nanowire array supercapacitor electrode material |
| CN106340398A (en) * | 2016-11-17 | 2017-01-18 | 西南大学 | Method for preparing composite nickel-cobalt hydroxide and molybdenum oxide material for supercapacitor electrode material |
| CN110136972A (en) * | 2019-04-25 | 2019-08-16 | 南京国轩电池有限公司 | A kind of preparation method of multilayer hierarchical structure supercapacitor composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103594253A (en) * | 2013-11-21 | 2014-02-19 | 东华大学 | Method for preparing porous NiCo2O4/MnO2 nuclear shell nanowire array supercapacitor electrode material |
| CN106340398A (en) * | 2016-11-17 | 2017-01-18 | 西南大学 | Method for preparing composite nickel-cobalt hydroxide and molybdenum oxide material for supercapacitor electrode material |
| CN110136972A (en) * | 2019-04-25 | 2019-08-16 | 南京国轩电池有限公司 | A kind of preparation method of multilayer hierarchical structure supercapacitor composite material |
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