CN112382514A - NiCo for all-solid-state flexible supercapacitor2O4Preparation method of @ Ni-Co LDH composite electrode - Google Patents
NiCo for all-solid-state flexible supercapacitor2O4Preparation method of @ Ni-Co LDH composite electrode Download PDFInfo
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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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- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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 provides NiCo for an all-solid-state flexible supercapacitor2O4The preparation method of the @ Ni-Co LDH composite electrode comprises the following steps: (1) mixing NiCl2·6H2O、CoCl2·6H2O, urea and deionized water according to the mass ratio of 1: 2: 5: 20, slowly adding NH 4F; (2) putting the carbon cloth into the solution, preserving heat and cooling to normal temperature along with the furnace; (3) taking out the carbon cloth, cleaning, and annealing; (4) mixing Ni (NO)3)2·6H2O、Co(NO3)2·6H2O and NH4F are in a ratio of 4: 1: 2.8 mixing evenly; (5) obtaining NiCo by electrodeposition2O4@ Ni-Co LDH/CFC electrode material, taken out and thenAnd sequentially cleaning and drying by using deionized water and absolute ethyl alcohol. The all-solid-state flexible supercapacitor disclosed by the invention has good charge storage capacity and ion diffusion capacity, and also has good cycling stability, the preparation method is simple, and the electrochemical performance of the product is good.
Description
Technical Field
The invention belongs to the technical field of capacitors, and particularly relates to NiCo for an all-solid-state flexible supercapacitor2O4A @ Ni-Co LDH composite electrode and a preparation method thereof.
Background
Energy is the material basis on which humans rely for survival. In modern society, with the rapid development of economic society, the demand of human beings for energy is increasing. Due to the use of fossil fuels and the development of human beings, fossil energy is gradually exhausted, and the exploitation and use of fossil fuels cause serious pollution to the environment and threaten the sustainable development of human and social economy.
Supercapacitors have high specific capacity and power density, but the development of supercapacitors faces a series of problems. The research on the super capacitor is mainly carried out around three parts of the development of electrode materials, the selection of electrolyte and the assembly of the capacitor. The primary factor of concern to researchers is the electrode material. While supercapacitors still face many difficulties in terms of production technology and practical application, it is believed that these problems will eventually be resolved as researchers have conducted intensive research into new materials and technologies.
Layered Double Hydroxides (LDHs) are layered compounds composed of two or more metal hydroxides, and have proven to be very promising electrode materials for super capacitors due to the advantages of high capacitance, high redox activity, environmental friendliness and the like. Meanwhile, the LDHs have wide application prospects in the fields of adsorption, electrocatalysis, drug release, energy storage devices and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a NiCo2O4@ Ni-Co LDH composite electrode for an all-solid-state flexible supercapacitor and a preparation method thereof, so as to solve the problems of poor mechanical property and stability, complex preparation, poor chemical property and the like of electrode materials of the supercapacitor.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a NiCo2O4@ Ni-Co LDH composite electrode for an all-solid-state flexible supercapacitor comprises the following steps:
(1) NiCl2 & 6H2O, CoCl2 & 6H2O, urea and deionized water are mixed according to the mass ratio of 1: 2: 5: 20, stirring uniformly to obtain a solution, and slowly adding NH4F into the prepared solution, wherein the mass ratio of the deionized water to NH4F is 400: 1-200: 1, simultaneously stirring for 10 minutes by magnetic force, and uniformly mixing;
(2) putting the carbon cloth into the solution, placing the carbon cloth into a vacuum blast drying oven, preserving the heat in an environment of 120 ℃, and cooling the carbon cloth to the normal temperature along with the furnace;
(3) taking out the carbon cloth, repeatedly cleaning the carbon cloth for more than three times by using deionized water and absolute ethyl alcohol in sequence, placing the carbon cloth in a vacuum drying oven to dry the carbon cloth for 12 hours at the temperature of 70 ℃, placing the dried carbon cloth in a quartz tube furnace to heat the carbon cloth from room temperature to 350 ℃, wherein the heating rate is 2 ℃ for min-1, and annealing the carbon cloth for 2 hours to obtain a NiCo2O4 material;
(4) mixing Ni (NO3)2 & 6H2O, Co (NO3)2 & 6H2O and NH4F according to the mass ratio of 4: 1: 2.8, uniformly mixing and cleaning in a cleaner;
(5) and (3) taking the NiCo2O4 material prepared in the step (3) as a working electrode, taking the solution prepared in the step (4) as an electrolyte, obtaining a NiCo2O4@ Ni-Co LDH/CFC electrode material by using an electrodeposition method, namely taking the NiCo2O4-N/CFC as the working electrode, taking a platinum electrode and a calomel electrode as a counter electrode and a reference electrode, controlling the current of a cathode and an anode to be 10mA, preparing the material by using a method with the electrodeposition time of 10 minutes, taking out the material, sequentially washing the material by using deionized water and absolute ethyl alcohol for three times, and drying the material for 12 hours in a vacuum drying oven at the temperature of 70 ℃.
Preferably, the incubation time in step (2) is 5 to 6 hours.
Preferably, the cleaning device in the step (4) is an ultrasonic cleaning agent.
Preferably, the washing time in step (4) is 15 to 20 minutes.
The invention provides a preparation method of an all-solid-state flexible supercapacitor electrode material, which not only endows the electrode with good mechanical properties, but also has good charge storage capacity and ion diffusion capacity, and also has good cycling stability. Moreover, the preparation time of the sample in the constant current electrodeposition process is short, the efficiency is high, and the experimental instrument and the operation are simple. The preparation method is simple, and the product has good electrochemical performance, strong availability and great application potential.
Drawings
FIG. 1 is a scanning electron microscope image of NiCo2O4 and NiCo2O4@ Ni-Co LDH composite electrode material.
FIG. 2 is a graph of electrochemical performance test of NiCo2O4@ Ni-Co LDH composite electrode material.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
(1) 2mmol of NiCl2 & 6H2O, 4mmol of CoCl2 & 6H2O, 10mmol of urea and 40ml of deionized water were mixed and stirred to obtain a solution, and 0.1g of NH4F was added thereto and stirred uniformly to obtain a uniform solution.
(2) Vertically putting the carbon cloth into the solution, and then putting the solution into a vacuum forced-air drying oven to react for 6 hours at 120 ℃, wherein the reaction time is too short, and the active substances on the surface of the carbon cloth are too little; too long a time, the active substance that has grown up is too dense and results in agglomeration.
(3) And taking out the carbon cloth, repeatedly cleaning the carbon cloth for more than three times by using deionized water and absolute ethyl alcohol in sequence, drying the carbon cloth in a vacuum drying oven at 70 ℃ for 12 hours, placing the dried carbon cloth in a quartz tube furnace, heating the carbon cloth from room temperature to 350 ℃ at the heating rate of 2 ℃ for min-1, and annealing the carbon cloth for 2 hours to obtain the NiCo2O4 material.
(4) 3.6mmol of Ni (NO3) 2.6H 2O, 0.9mmol of Co (NO3) 2.6H 2O, 50ml of deionized water and 2.52mmol of NH4F are mixed uniformly and then mixed ultrasonically in an ultrasonic cleaner for 15 minutes, wherein the ultrasonic cleaner is used for dissolving the solute in the solvent more fully.
(5) The prepared NiCo2O4 material is used as a working electrode, a constant current time-counting electrodeposition method is used, NiCo2O4-N/CFC is used as the working electrode, a platinum electrode and a calomel electrode are used as a counter electrode and a reference electrode, the cathode and anode currents are 10mA, the electrodeposition time is 10 minutes, and the NiCo2O4@ Ni-Co LDH/CFC electrode material is obtained. And taking out the material, cleaning and drying.
The electrochemical performance test method comprises the following steps: in order to compare the electrochemical performances of different electrode materials, Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) tests were performed on three electrode materials, NiCo2O4@ Ni-Co LDH, by using an electrochemical workstation in a three-electrode system. And (3) the CV curve of the electrode material at the scanning rate of 10mV · s < -1 >, and the potential window of the tested sample is-0.2-0.8V.
The series of electrochemical performance test methods can be used, and the material prepared by the embodiment can reach 4901.8mF/cm2 when the current density is 2mA/cm 2; the circulation is carried out for 5000 times, and the circulation efficiency is 86.7 percent.
Example 2
(1) 4mmol of NiCl2 & 6H2O, 8mmol of CoCl2 & 6H2O, 20mmol of urea and 80ml of deionized water were mixed and stirred to obtain a solution, and 0.2g of NH4F was added thereto and stirred uniformly to obtain a uniform solution.
(2) Vertically putting the carbon cloth into the solution, and then putting the solution into a vacuum forced-air drying oven to react for 6 hours at 120 ℃, wherein the reaction time is too short, and the active substances on the surface of the carbon cloth are too little; too long a time, the active substance that has grown up is too dense and results in agglomeration.
(3) And taking out the carbon cloth, repeatedly cleaning the carbon cloth for more than three times by using deionized water and absolute ethyl alcohol in sequence, drying the carbon cloth in a vacuum drying oven at 70 ℃ for 12 hours, placing the dried carbon cloth in a quartz tube furnace, heating the carbon cloth from room temperature to 350 ℃ at the heating rate of 2 ℃ for min-1, and annealing the carbon cloth for 2 hours to obtain the NiCo2O4 material.
(4) 3.6mmol of Ni (NO3) 2.6H 2O, 0.9mmol of Co (NO3) 2.6H 2O, 50ml of deionized water and 2.52mmol of NH4F are mixed uniformly and then mixed ultrasonically in an ultrasonic cleaner for 10 minutes, wherein the ultrasonic cleaner is used for dissolving the solute in the solvent more fully.
(5) The prepared NiCo2O4 material is used as a working electrode, a constant current time-counting electrodeposition method is used, NiCo2O4-N/CFC is used as the working electrode, a platinum electrode and a calomel electrode are used as a counter electrode and a reference electrode, the cathode and anode currents are 10mA, the electrodeposition time is 10 minutes, and the NiCo2O4@ Ni-Co LDH/CFC electrode material is obtained. And taking out the material, cleaning and drying.
The electrochemical performance test method comprises the following steps: in order to compare the electrochemical performances of different electrode materials, Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) tests were performed on three electrode materials, NiCo2O4@ Ni-Co LDH, by using an electrochemical workstation in a three-electrode system. And (3) the CV curve of the electrode material at the scanning rate of 10mV · s < -1 >, and the potential window of the tested sample is-0.2-0.8V.
The series of electrochemical performance test methods can be used, and the material prepared by the embodiment can reach 4806.8mF/cm2 when the current density is 2mA/cm 2; the circulation is carried out for 5000 times, and the circulation efficiency is 87.6 percent.
Example 3
(1) 2mmol of NiCl2 & 6H2O, 4mmol of CoCl2 & 6H2O, 10mmol of urea and 40ml of deionized water were mixed and stirred to obtain a solution, and 0.2g of NH4F was added thereto and stirred uniformly to obtain a uniform solution.
(2) Vertically putting the carbon cloth into the solution, and then putting the carbon cloth into a vacuum forced-air drying oven to react for 5 hours at 150 ℃, wherein the reaction time is too short, and the active substances on the carbon cloth are too little; too long a time, the active substance that has grown up is too dense and results in agglomeration.
(3) And taking out the carbon cloth, repeatedly cleaning the carbon cloth for more than three times by using deionized water and absolute ethyl alcohol in sequence, drying the carbon cloth in a vacuum drying oven at 70 ℃ for 12 hours, placing the dried carbon cloth in a quartz tube furnace, heating the carbon cloth from room temperature to 350 ℃ at the heating rate of 2 ℃ for min-1, and annealing the carbon cloth for 2 hours to obtain the NiCo2O4 material.
(4) 7.2mmol of Ni (NO3) 2.6H 2O, 1.8mmol of Co (NO3) 2.6H 2O, 100ml of deionized water and 5mmol of NH4F are uniformly mixed and then ultrasonically mixed in an ultrasonic cleaner for 10 minutes, wherein the ultrasonic cleaner is used for dissolving the solute in the solvent more fully.
(5) The prepared NiCo2O4 material is used as a working electrode, a constant current time-counting electrodeposition method is used, NiCo2O4-N/CFC is used as the working electrode, a platinum electrode and a calomel electrode are used as a counter electrode and a reference electrode, the cathode and anode currents are 10mA, the electrodeposition time is 10 minutes, and the NiCo2O4@ Ni-Co LDH/CFC electrode material is obtained. And taking out the material, cleaning and drying.
The electrochemical performance test method comprises the following steps: in order to compare the electrochemical performances of different electrode materials, Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) tests were performed on three electrode materials, NiCo2O4@ Ni-Co LDH, by using an electrochemical workstation in a three-electrode system. And (3) the CV curve of the electrode material at the scanning rate of 10mV · s < -1 >, and the potential window of the tested sample is-0.2-0.8V.
The series of electrochemical performance test methods can be used, and the material prepared by the embodiment can reach 4801.8mF/cm2 when the current density is 2mA/cm 2; the circulation is carried out for 3000 times, and the circulation efficiency is 88.6 percent.
Example 4
(1) 4mmol of NiCl2 & 6H2O, 8mmol of CoCl2 & 6H2O, 20mmol of urea and 80ml of deionized water were mixed and stirred to obtain a solution, and 0.2g of NH4F was added thereto and stirred uniformly to obtain a uniform solution.
(2) Vertically putting the carbon cloth into the solution, and then putting the carbon cloth into a vacuum forced-air drying oven to react for 5 hours at 150 ℃, wherein the reaction time is too short, and the active substances on the carbon cloth are too little; too long a time, the active substance that has grown up is too dense and results in agglomeration.
(3) And taking out the carbon cloth, repeatedly cleaning the carbon cloth for more than three times by using deionized water and absolute ethyl alcohol in sequence, drying the carbon cloth in a vacuum drying oven at 70 ℃ for 12 hours, placing the dried carbon cloth in a quartz tube furnace, heating the carbon cloth from room temperature to 350 ℃ at the heating rate of 2 ℃ for min-1, and annealing the carbon cloth for 2 hours to obtain the NiCo2O4 material.
(4) 7.2mmol of Ni (NO3) 2.6H 2O, 1.8mmol of Co (NO3) 2.6H 2O, 100ml of deionized water and 5mmol of NH4F are uniformly mixed, and then are ultrasonically mixed for 15 minutes in an ultrasonic cleaner, wherein the ultrasonic cleaner is used for leading the solute to be more fully dissolved in the solvent.
(5) The prepared NiCo2O4 material is used as a working electrode, a constant current time-counting electrodeposition method is used, NiCo2O4-N/CFC is used as the working electrode, a platinum electrode and a calomel electrode are used as a counter electrode and a reference electrode, the cathode and anode currents are 10mA, the electrodeposition time is 10 minutes, and the NiCo2O4@ Ni-Co LDH/CFC electrode material is obtained. And taking out the material, cleaning and drying.
As shown in FIG. 1, the microscopic morphology of the material can be observed by a scanning electron microscope, and the needle-shaped NiCo2O4 is wrapped by the flaky Ni-Co LDH material to form a core-shell structure with an oxide as a core and a hydroxide as a shell. The structure has abundant open space, is beneficial to the rapid transmission of ions of the electrode and the electrolyte, can provide more active sites due to lower ion transmission resistance, and is beneficial to the oxidation-reduction reaction in an electrochemical test.
As shown in fig. 2, electrochemical performance test method: in order to compare the electrochemical performances of different electrode materials, Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) tests were performed on three electrode materials, NiCo2O4@ Ni-Co LDH, by using an electrochemical workstation in a three-electrode system. And (3) the CV curve of the electrode material at the scanning rate of 10mV · s < -1 >, and the potential window of the tested sample is-0.2-0.8V.
The series of electrochemical performance test methods can be used, and the material prepared by the embodiment can reach 4895.8mF/cm2 when the current density is 2mA/cm 2; the circulation is carried out for 5000 times, and the circulation efficiency is 87.0 percent.
Claims (4)
1. NiCo for all-solid-state flexible supercapacitor2O4The preparation method of the @ Ni-Co LDH composite electrode is characterized by comprising the following steps of:
(1) mixing NiCl2·6H2O、CoCl2·6H2O, urea and deionized water according to the mass ratio of 1: 2: 5: 20, stirring uniformly to obtain a solution, and slowly adding NH4F into the prepared solution, wherein the mass of the added deionized water is NH4F is 200 to 400 times of the weight of the mixture, and the mixture is stirred for 10 minutes by magnetic force and is uniformly mixed;
(2) putting the carbon cloth into the solution, placing the carbon cloth into a vacuum blast drying oven, preserving the heat in an environment of 120 ℃, and cooling the carbon cloth to the normal temperature along with the furnace;
(3) taking out the carbon cloth, repeatedly cleaning with deionized water and anhydrous ethanol for more than three times, drying at 70 deg.C for 12 hr in a vacuum drying oven, heating the dried carbon cloth in a quartz tube furnace from room temperature to 350 deg.C at a heating rate of 2 deg.C for min-1Then annealing for 2 hours to obtain NiCo2O4A material;
(4) mixing Ni (NO)3)2·6H2O、Co(NO3)2·6H2O and NH4F is 4: 1: 2.8, uniformly mixing and cleaning in a cleaner;
(5) using the NiCo2O4 material prepared in the step (3) as a working electrode, using the solution in the step (4) as an electrolyte, and obtaining NiCo by using an electrodeposition method2O4@ Ni-Co LDH/CFC electrode material, i.e. NiCo2O4And (2) taking the-N/CFC as a working electrode, taking a platinum electrode and a calomel electrode as a counter electrode and a reference electrode, taking the obtained product out, sequentially cleaning the product for three times by using deionized water and absolute ethyl alcohol after the product is prepared by a method that the current of a cathode and an anode is 10mA and the electrodeposition time is 10 minutes, and drying the product for 12 hours in a vacuum drying oven at 70 ℃.
2. The NiCo for all-solid-state flexible supercapacitor according to claim 12O4The preparation method of the @ Ni-Co LDH composite electrode is characterized in that the heat preservation time in the step (2) is 5-6 hours.
3. The NiCo for all-solid-state flexible supercapacitor according to claim 12O4The preparation method of the @ Ni-Co LDH composite electrode is characterized in that the cleaning device in the step (4) adopts an ultrasonic cleaning agent.
4. The NiCo for all-solid-state flexible supercapacitor according to claim 12O4The preparation method of the @ Ni-Co LDH composite electrode is characterized in that the cleaning time in the step (4) is 15-20 minutes.
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| CN114940517A (en) * | 2022-04-21 | 2022-08-26 | 安徽大学 | FeCoNi basic carbonate electrode material and preparation method thereof |
| CN116864317A (en) * | 2023-06-16 | 2023-10-10 | 长沙理工大学 | Three-dimensional NiCo for electrochemical energy storage 2 O 4 Preparation method of Ni-C nanocomposite |
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| CN116864317A (en) * | 2023-06-16 | 2023-10-10 | 长沙理工大学 | Three-dimensional NiCo for electrochemical energy storage 2 O 4 Preparation method of Ni-C nanocomposite |
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