CN111627724B - Carbon-coated nickel-based film electrode material and preparation method and application thereof - Google Patents
Carbon-coated nickel-based film electrode material and preparation method and application thereof Download PDFInfo
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- 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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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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Abstract
The invention provides a carbon-coated nickel-based film electrode material and a preparation method and application thereof, wherein the preparation method comprises the following steps: dispersing nickel nanowires in a dispersing agent, drying after suction filtration, enabling a filter membrane to fall off, then tabletting and slicing to obtain a nickel nanowire film, mixing the nickel nanowire film with a hydrogen peroxide solution, washing and drying a product after hydrothermal reaction treatment to obtain a nickel/nickel hydroxide film, and mixing the nickel/nickel hydroxide film with a glucose solution to perform hydrothermal reaction; the electrode material takes the nickel nanowire film as a substrate, the nickel/nickel hydroxide film energy storage electrode material is prepared by a hydrothermal method and a carbon coating method, the carbon coating can improve the conductivity and the circulation stability of the electrode material, and the electrode material has the characteristics of high volume capacity, excellent rate capability and the like, so that the electrode material is applied to a capacitor or a battery; therefore, the invention can improve the conductivity and enhance the stability of the nickel-based electrode material through carbon coating, thereby enhancing the cycling stability of the electrode and prolonging the service life.
Description
Technical Field
The invention belongs to the technical field of energy storage electrode material preparation, and particularly relates to a carbon-coated nickel-based film electrode material and a preparation method and application thereof.
Background
Super capacitor is also called electrochemical capacitor, is a new type electrochemical energy storage device, and has received more and more attention in recent years. Compared with energy storage devices such as lithium ion batteries and the like, the super capacitor has the advantages of rapid charge and discharge, long service life, high power density, low internal resistance, higher energy density than a traditional capacitor and the like. Therefore, it is often used in fields requiring a long cycle period and high power density, including personal electronics, hybrid cars, and backup power supplies. With the continuous expansion of the application field, the requirements on the electrode material are higher and higher.
Electrode materials are important components of energy storage devices. In recent years, nickel-based oxides, hydroxides, sulfides, and the like have attracted more and more attention due to their advantages of high theoretical specific capacitance, low cost, environmental protection, and the like. But its application is limited due to its poor conductivity and stability.
Disclosure of Invention
Aiming at the defects in the prior art, the invention mainly aims to provide a preparation method of a carbon-coated nickel-based film electrode material. The method comprises the steps of preparing uniform one-dimensional ultra-long nickel nanowires by a simple one-step liquid phase method, obtaining a nickel nanowire film by vacuum filtration and tabletting, obtaining a nickel/nickel hydroxide film by hydrothermal reaction, and then carrying out carbon coating on the nickel/nickel hydroxide film by taking glucose as a carbon source to finally obtain the carbon-coated nickel/nickel hydroxide film which is used as an energy storage electrode material.
The second purpose of the invention is to provide the carbon-coated nickel-based thin-film electrode material.
The third purpose of the invention is to provide the application of the carbon-coated nickel-based thin-film electrode material.
In order to achieve the above primary object, the solution of the present invention is:
a preparation method of a carbon-coated nickel-based film electrode material comprises the following steps:
(1) dispersing the nickel nanowires in a dispersing agent, drying after suction filtration, enabling a filter membrane to fall off, and then tabletting and slicing to obtain a nickel nanowire film;
(2) mixing the nickel nanowire film with a hydrogen peroxide solution, washing and drying a product after hydrothermal reaction treatment to obtain a nickel/nickel hydroxide film;
(3) and mixing the nickel/nickel hydroxide film with the glucose solution, carrying out hydrothermal reaction, washing and drying to obtain the carbon-coated nickel-based film electrode material, namely the carbon-coated nickel/nickel hydroxide film electrode material.
As a preferred embodiment of the present invention, in the step (1), the dispersant is an ethanol solution containing 1 to 5 wt% of polyvinylpyrrolidone.
As a preferred embodiment of the invention, in the step (1), the drying time is 10-30 min; the pressure of tabletting is 8-10MPa, and the tabletting time is 1-5 min.
As a preferred embodiment of the present invention, in the step (2), the mass of the nickel nanowire thin film is 30-200 mg.
As a preferred embodiment of the present invention, in the step (2), the hydrogen peroxide solution contains 0 to 30% by mass of hydrogen peroxide and 30 to 60mL of hydrogen peroxide in volume.
As a preferred embodiment of the present invention, in the step (2), the temperature of the hydrothermal reaction is 140-.
In step (2), as a preferred embodiment of the present invention, the washing is performed 2 to 4 times by using deionized water and ethanol, respectively.
As a preferred embodiment of the present invention, in the step (2), the drying temperature is 50-70 ℃ and the drying time is 6-12 h.
As a preferred embodiment of the present invention, in step (3), the concentration of the glucose solution is 0.5 to 3mg/mL, and the volume is 20 to 50 mL.
As a preferred embodiment of the present invention, in the step (3), the mass of the nickel/nickel hydroxide film is 30 to 80 mg.
As a preferred embodiment of the present invention, in the step (3), the temperature of the hydrothermal reaction is 100-140 ℃, and the time of the hydrothermal reaction is 4-10 h.
In order to achieve the second objective, the solution of the invention is:
the carbon-coated nickel-based film electrode material is obtained by the preparation method.
In order to achieve the third object, the solution of the invention is:
the carbon-coated nickel-based film electrode material is applied to capacitors or batteries, and particularly can be applied to asymmetric supercapacitors or batteries.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the electrode material takes a nickel nanowire film as a substrate, and a nickel/nickel hydroxide film energy storage electrode material is prepared by a hydrothermal method and a carbon coating method; the carbon coating can not only improve the conductivity of the electrode material, but also improve the cycling stability of the electrode material, thereby improving the specific capacity value of the electrode material. In addition, the coating of the carbon nano material can avoid the collapse of the active material in the charge and discharge process. Therefore, the electrode material prepared by the invention has the characteristics of higher volume capacity, excellent rate capability and the like, thereby being applied to capacitors or batteries.
Secondly, the electrical conductivity of the nickel-based electrode material can be improved and the stability of the nickel-based electrode material can be enhanced through carbon coating, so that the cycling stability of the electrode is enhanced, and the service life of the electrode is prolonged; in addition, the preparation method is simple, easy to operate, good in performance and convenient for industrial application.
Drawings
FIG. 1 is a schematic diagram of the preparation process of the carbon-coated nickel/nickel hydroxide thin film electrode material of the present invention.
Fig. 2 is a schematic view of a Scanning Electron Microscope (SEM) of the carbon-coated nickel/nickel hydroxide thin film electrode material of example 1 in the present invention.
FIG. 3 is a schematic illustration of the cycling stability of the carbon-coated nickel/nickel hydroxide thin film electrode material of example 1 of the present invention.
Detailed Description
The invention provides a carbon-coated nickel-based film electrode material and a preparation method and application thereof.
< preparation method of carbon-coated nickel-based thin-film electrode Material >
As shown in fig. 1, the preparation method of the carbon-coated nickel-based thin film electrode material of the present invention comprises the following steps:
(1) and preparing the nickel nanowire film: uniformly dispersing the nickel nanowires in a dispersing agent, naturally drying after vacuum filtration, enabling a filter membrane to fall off, and then tabletting and slicing to obtain a nickel nanowire film;
(2) and preparing the nickel/nickel hydroxide film: mixing the nickel nanowire film and a hydrogen peroxide solution, putting the mixture into a high-pressure reaction kettle, washing and drying a product after hydrothermal reaction treatment to obtain a nickel/nickel hydroxide film;
(3) preparing a carbon-coated nickel-based film electrode material: and mixing the nickel/nickel hydroxide film and the glucose solution, putting the mixture into an oven for hydrothermal reaction, washing and drying to obtain the carbon-coated nickel-based film electrode material, namely the carbon-coated nickel/nickel hydroxide film electrode material.
Wherein, in the step (1), the dispersing agent is ethanol solution containing 1-5 wt% of polyvinylpyrrolidone.
In the step (1), natural drying refers to drying in the air environment, and the time can be 10-30min, preferably 10 min; the pressure of the tabletting can be 8-10MPa, preferably 10 MPa; the tabletting time may be 1-5min, preferably 5 min.
In the step (2), the mass of the nickel nanowire thin film may be 30-200mg, preferably 32 mg.
In step (2), the mass fraction of hydrogen peroxide in the hydrogen peroxide solution may be 0 to 30%, preferably 15%; the volume may be 30-60mL, preferably 20 mL.
In the step (2), the temperature of the hydrothermal reaction may be 140-; the hydrothermal reaction time may be 6-12h, preferably 12 h.
In the step (2), washing is performed 2 to 4 times by using deionized water and ethanol, respectively.
In step (2), the temperature for drying may be 50 to 70 ℃, preferably 60 ℃; the drying time may be 6-12h, preferably 6 h.
In step (3), the concentration of the glucose solution may be 0.5-3mg/mL, preferably 1 mg/mL; the volume may be 20-50mL, preferably 30 mL.
In step (3), the mass of the nickel/nickel hydroxide film may be 30 to 80mg, preferably 30 mg.
In the step (3), the temperature of the hydrothermal reaction may be 100-; the hydrothermal reaction time may be 4 to 10 hours, preferably 5 hours.
< carbon-coated nickel-based thin-film electrode Material >
The carbon-coated nickel-based film electrode material is prepared by the preparation method.
< application of carbon-coated nickel-based thin-film electrode Material >
The carbon-coated nickel-based film electrode material can be applied to capacitors or batteries, and particularly can be applied to asymmetric supercapacitors or batteries.
The present invention will be further described with reference to the following examples.
Example 1:
the preparation method of the carbon-coated nickel-based film electrode material comprises the following steps:
(1) uniformly dispersing the nickel nanowires in 1 wt% ethanol solution of polyvinylpyrrolidone, naturally drying for 10min after vacuum filtration, and finally pressing for 5min under 10MPa to obtain the nickel nanowire film.
(2) Mixing 32mg of nickel nanowire film and 20mL of 15 wt% hydrogen peroxide solution, putting the mixture into a 50mL polytetrafluoroethylene high-pressure reaction kettle, carrying out hydrothermal reaction at 140 ℃ for 12h, and then washing the product with deionized water and drying the product at 60 ℃ for 6h to obtain the nickel/nickel hydroxide film.
(3) And putting the 30mg nickel/nickel hydroxide film into 30mL of 1mg/mL glucose solution, carrying out hydrothermal reaction in an oven at 120 ℃ for 5h, and cleaning after the reaction is finished to finally obtain the carbon-coated nickel-based film electrode material.
The prepared electrode material is used as a working electrode, mercury/mercury oxide is used as a reference electrode, a platinum electrode with the same area is used as an auxiliary electrode, and a three-electrode system is formed by using 6mol/L potassium hydroxide solution as electrolyte. Constant current charge and discharge tests are carried out on the research electrode in a CHI760E electrochemical workstation in a potential range of 0-0.55V (vs. mercury/mercury oxide), a nickel/nickel hydroxide electrode material is used as a comparative example and sucrose is used as a carbon source electrode material (namely, sucrose-coated nickel/nickel hydroxide) as shown in FIG. 3, the number of test turns is 10000, the tested current density is 5A, the capacitance retention rate of the electrode material taking glucose as the carbon source (namely, glucose-coated nickel/nickel hydroxide) in the embodiment is 96.2%, the capacitance retention rate of the electrode material taking nickel/nickel hydroxide in the comparative example is 59.4%, the capacitance retention rate of the electrode material taking sucrose as the carbon source (namely, sucrose-coated nickel/nickel hydroxide) in the comparative example is 81.3%, the stability effect is not as good as the stability of the material in the embodiment, and the glucose coating effect is most uniform, and the tested performance is also the best, so that the electrode material of the embodiment has high stable performance as an energy storage material.
Example 2:
the preparation method of the carbon-coated nickel-based film electrode material comprises the following steps:
(1) uniformly dispersing the nickel nanowires in 1 wt% ethanol solution of polyvinylpyrrolidone, naturally drying for 10min after vacuum filtration, and finally pressing for 3min under 9MPa to obtain the nickel nanowire film.
(2) Mixing 50mg of nickel nanowire film and 50mL of 20 wt% hydrogen peroxide solution, putting the mixture into a 100mL polytetrafluoroethylene high-pressure reaction kettle, carrying out hydrothermal reaction at 140 ℃ for 8h, and then washing the product with deionized water and drying the product at 65 ℃ for 7h to obtain the nickel/nickel hydroxide film.
(3) And putting the 40mg nickel/nickel hydroxide film into 50mL of 2mg/mL glucose solution, carrying out hydrothermal reaction in an oven at 120 ℃ for 10h, and cleaning after the reaction is finished to finally obtain the carbon-coated nickel-based film electrode material.
Example 3:
the preparation method of the carbon-coated nickel-based film electrode material comprises the following steps:
(1) uniformly dispersing the nickel nanowires in 1 wt% ethanol solution of polyvinylpyrrolidone, naturally drying for 10min after vacuum filtration, and finally pressing for 5min under 8MPa to obtain the nickel nanowire film.
(2) And mixing 70mg of the nickel nanowire film with 60mL of 30 wt% hydrogen peroxide solution, putting the mixture into a 100mL polytetrafluoroethylene high-pressure reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 10h, and then washing the product with deionized water and drying the product at 65 ℃ for 10h to obtain the nickel/nickel hydroxide film.
(3) And putting the 70mg nickel/nickel hydroxide film into 50mL of 2mg/mL glucose solution, carrying out hydrothermal reaction in an oven at 100 ℃ for 8h, and cleaning after the reaction is finished to finally obtain the carbon-coated nickel-based film electrode material.
Example 4:
the preparation method of the carbon-coated nickel-based film electrode material comprises the following steps:
(1) uniformly dispersing the nickel nanowires in 1 wt% ethanol solution of polyvinylpyrrolidone, naturally drying for 10min after vacuum filtration, and finally pressing for 3min under 10MPa to obtain the nickel nanowire film.
(2) Mixing 60mg of nickel nanowire film and 60mL of 25 wt% hydrogen peroxide solution, putting the mixture into a 100mL polytetrafluoroethylene high-pressure reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 12h, and then washing the product with deionized water and drying the product at 65 ℃ for 12h to obtain the nickel/nickel hydroxide film.
(3) And putting the 50mg nickel/nickel hydroxide film into 50mL of 3mg/mL glucose solution, carrying out hydrothermal reaction in an oven at 130 ℃ for 10h, and cleaning after the reaction is finished to finally obtain the carbon-coated nickel-based film electrode material.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (10)
1. A preparation method of a carbon-coated nickel-based film electrode material is characterized by comprising the following steps: which comprises the following steps:
(1) dispersing the nickel nanowires in a dispersing agent, drying after suction filtration, enabling a filter membrane to fall off, and then tabletting and slicing to obtain a nickel nanowire film;
(2) mixing the nickel nanowire film with a hydrogen peroxide solution, washing and drying a product after reaction treatment to obtain a nickel/nickel hydroxide film;
(3) mixing the nickel/nickel hydroxide film with a glucose solution, reacting, washing and drying to obtain a carbon-coated nickel-based film electrode material;
in the step (1), the dispersing agent is ethanol solution containing 1-5 wt% of polyvinylpyrrolidone;
in the step (3), the concentration of the glucose solution is 0.5-3mg/mL, and the volume is 20-50 mL;
in the step (3), the reaction temperature is 100-140 ℃, and the reaction time is 4-10 h.
2. The method of claim 1, wherein: in the step (1), the drying time is 10-30 min; the pressure of the tabletting is 8-10MPa, and the tabletting time is 1-5 min.
3. The method of claim 1, wherein: in the step (2), the mass of the nickel nanowire film is 30-200 mg.
4. The method of claim 1, wherein: in the step (2), the mass fraction of the hydrogen peroxide in the hydrogen peroxide solution is 0-30%, and the volume of the hydrogen peroxide solution is 30-60 mL.
5. The method of claim 1, wherein: in the step (2), the reaction temperature is 140-200 ℃, and the reaction time is 6-12 h.
6. The method of claim 1, wherein: in the step (2), the washing is performed for 2-4 times by using deionized water and ethanol respectively.
7. The method of claim 1, wherein: in the step (2), the drying temperature is 50-70 ℃, and the drying time is 6-12 h.
8. The method of claim 1, wherein: in the step (3), the mass of the nickel/nickel hydroxide film is 30-80 mg.
9. A carbon-coated nickel-based film electrode material is characterized in that: which is obtained by the production method according to any one of claims 1 to 8.
10. Use of the carbon-coated nickel-based thin film electrode material according to claim 9 in a capacitor or a battery.
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| CN110311133A (en) * | 2019-06-21 | 2019-10-08 | 南京农业大学 | A kind of three-dimensional carbon negative pole material and preparation method thereof, application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8920682B2 (en) * | 2010-03-19 | 2014-12-30 | Eastern Michigan University | Nanoparticle dispersions with ionic liquid-based stabilizers |
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| KR20130059472A (en) * | 2011-11-28 | 2013-06-07 | 삼성에스디아이 주식회사 | Negative active material and lithium battery containing the material |
| CN103219169A (en) * | 2013-03-29 | 2013-07-24 | 东华大学 | Preparation method for carbon-coated nickel oxide NiO/C as supercapacitor electrode material |
| CN105244185A (en) * | 2015-10-09 | 2016-01-13 | 上海交通大学 | Electrochemical preparation method for nickel/nickel hydroxide energy storage electrode material |
| CN107093717A (en) * | 2017-04-17 | 2017-08-25 | 陕西科技大学 | Carbon coating cobalt oxide nano-wire array and preparation method thereof is grown in nickel foam |
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| CN110311133A (en) * | 2019-06-21 | 2019-10-08 | 南京农业大学 | A kind of three-dimensional carbon negative pole material and preparation method thereof, application |
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