CN114758903A - Preparation method of supercapacitor electrode material - Google Patents

Preparation method of supercapacitor electrode material Download PDF

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Publication number
CN114758903A
CN114758903A CN202210413864.0A CN202210413864A CN114758903A CN 114758903 A CN114758903 A CN 114758903A CN 202210413864 A CN202210413864 A CN 202210413864A CN 114758903 A CN114758903 A CN 114758903A
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China
Prior art keywords
electrode material
preparation
blue mixture
supercapacitor
cobalt
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CN202210413864.0A
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Chinese (zh)
Inventor
滕飞
郝唯一
张家威
马奔
程港桠
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Nanjing University of Information Science and Technology
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Nanjing University of Information Science and Technology
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Priority to CN202210413864.0A priority Critical patent/CN114758903A/en
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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
    • 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
    • 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
    • H01G11/54—Electrolytes
    • H01G11/58—Liquid electrolytes

Abstract

The invention relates to the technical field of capacitors, in particular to a preparation method of a supercapacitor electrode material, which comprises the following steps: uniformly grinding 1g of cobalt nitrate and 1g of thiourea in a mortar to form a blue mixture; calcining the blue mixture in a muffle furnace for 4 hours to obtain the cobalt-based electrode material, wherein the calcining temperature of the blue mixture in the muffle furnace is constant at 600 ℃, and the Co in the invention is Co3O4The electrode material is simple in manufacturing method and low in cost, the material has excellent electrochemical performance, and the prepared super capacitor has good energy storage performance.

Description

Preparation method of supercapacitor electrode material
Technical Field
The invention relates to the technical field of capacitors, in particular to a preparation method of a supercapacitor electrode material.
Background
Supercapacitors have received much attention as a high performance energy storage system because they have a greater energy storage capacity than conventional capacitors and higher work than batteriesAnd (4) efficiency. Cobaltosic oxide (Co)3O4) Is a high-efficiency electrode material, has a theoretical specific capacitance of 800F/g (oxidation-reduction potential of 1V), and is widely concerned due to its low cost, environmental friendliness and excellent electrochemical stability. Among the various preparation methods, calcination is a mass production of Co 3O4A very simple process but Co produced by calcination of a single cobalt nitrate salt (sulphate, chloride, etc.)3O4Has low conductivity and inert surface chemical reactivity, resulting in undesirable specific capacitance. Co prepared by post-treatment, on the other hand3O4Although the performance is excellent, the process is complex and the cost is high, which is contrary to the industrial preparation concept.
Through retrieval, the Chinese patent application No. 202010065652.9 discloses a cobaltosic oxide nanotube array assembled by an anodic oxidation method and a method thereof, the cobaltosic oxide nanotube array is assembled on the surface of a cobalt foil, in addition, the Chinese patent application No. 202110038368.7 discloses a cobaltosic oxide composite material rich in oxygen vacancies and a preparation method and application thereof, cobalt salt and a precipitator are added into polydopamine-reduced graphene suspension, and the cobaltosic oxide is prepared by calcining after hydrothermal reaction. However, these methods are complicated and expensive.
Disclosure of Invention
The invention aims to provide a preparation method of a super capacitor electrode material, which aims to solve the problems in the background technology.
The technical scheme of the invention is as follows: a preparation method of a supercapacitor electrode material comprises the following steps:
S1, grinding 1g of cobalt nitrate and 1g of thiourea uniformly in a mortar to form a blue mixture;
and S2, calcining the blue mixture in a muffle furnace for 4 hours to obtain the cobalt-based electrode material.
Preferably, in S2, the temperature at which the blue mixture is calcined in the muffle furnace is constantly 600 ℃.
A super capacitor prepared by the preparation method of the super capacitor electrode material takes a potassium hydroxide solution as an electrolyte.
Preferably, the concentration of potassium hydroxide in the electrolyte is 1M.
The invention provides a preparation method of a super capacitor electrode material by improvement, compared with the prior art, the preparation method has the following improvements and advantages:
co in the invention3O4The electrode material has the advantages of simple manufacturing method and low cost, the material has excellent electrochemical performance, and the prepared super capacitor has good energy storage performance.
Drawings
The invention is further explained below with reference to the figures and examples:
FIG. 1 shows the prepared Co3O4An X-ray diffraction (XRD) pattern of the electrode material;
FIG. 2 shows the prepared Co3O4A Scanning Electron Microscope (SEM) image of the electrode material;
FIG. 3 shows the prepared Co3O4A capacitance value graph of the electrode material under different current densities;
Fig. 4 is a flow chart of a method for preparing the supercapacitor electrode material according to the present invention.
Detailed Description
The present invention is described in detail below, and technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a super capacitor electrode material through improvement, and the technical scheme of the invention is as follows:
as shown in fig. 4, a method for preparing an electrode material of a supercapacitor comprises the following steps:
s1, grinding 1g of cobalt nitrate and 1g of thiourea uniformly in a mortar to form a blue mixture;
and S2, calcining the blue mixture in a muffle furnace at 600 ℃ for 4 hours to obtain the cobalt-based electrode material.
The super capacitor is prepared by using a potassium hydroxide solution as an electrolyte, and the concentration of potassium hydroxide in the electrolyte is 1M.
And (3) testing:
s1, grinding 1g of cobalt nitrate and 1g of thiourea uniformly in a mortar to form a blue mixture;
s2, calcining the blue mixture in a muffle furnace at 600 ℃ for 4 hours to obtain a cobalt-based electrode material;
s3, mixing the prepared Co3O4 electrode material, conductive carbon black and polyvinylidene fluoride in a mass ratio of 8:1:1, dispersing the mixture in 1-methyl-2-pyrrolidone, and stirring to form uniform slurry;
s4, coating the slurry on carbon fiber cloth, and drying at room temperature for 24 hours to obtain Co with a coating area of 0.5cm × 0.5cm3O4An electrode;
and S5, testing by adopting a three-electrode system.
The test results show that: the capacitance value of the capacitor is 79.48F/g under the current density of 0.2A/g, the capacitance value of the capacitor is 60.8F/g under the condition of the large current density of 2A/g, and the capacitance value is only reduced by 23.5 percent under the condition that the current density is improved by 10 times, so that the capacitor has better rate performance.
FIG. 1 is a view showing prepared Co, as shown in FIGS. 1 to 33O4The X-ray diffraction (XRD) pattern of the electrode material can be seen from figure 1, and the characteristic peak and Co of the prepared product3O4Standard card (JCPDS:
#43-1003) was performed, and the prepared product was Co in pure phase3O4An electrode material; FIG. 2 shows the prepared Co3O4Scanning Electron Microscope (SEM) image of the electrode material, as can be seen from FIG. 2, prepared Co 3O4The electrode material consists of particles with a diameter of 1 μm; FIG. 3 shows the prepared Co3O4The capacitance values of the electrode material at different current densities are plotted, as can be seen from FIG. 3, Co3O4Electrode for electrochemical cellThe material exhibits excellent electrochemical properties, and bulk Co3O4Compared with the capacitor made by directly calcining cobalt nitrate, the capacitance value is improved by 13-16 times.
Co in the invention3O4The electrode material has the advantages of simple manufacturing method and low cost, the material has excellent electrochemical performance, and the prepared super capacitor has good energy storage performance.
The previous description is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (4)

1. A preparation method of a super capacitor electrode material is characterized by comprising the following steps: the method comprises the following steps:
s1, grinding 1g of cobalt nitrate and 1g of thiourea uniformly in a mortar to form a blue mixture;
And S2, calcining the blue mixture in a muffle furnace for 4 hours to obtain the cobalt-based electrode material.
2. The preparation method of the electrode material of the supercapacitor according to claim 1, characterized in that: in S2, the temperature at which the blue mixture was calcined in the muffle furnace was constantly 600 ℃.
3. The supercapacitor made by the preparation method of the supercapacitor electrode material according to claim 1, wherein the preparation method comprises the following steps: the super capacitor takes potassium hydroxide solution as electrolyte.
4. A supercapacitor according to claim 3, characterised in that: the concentration of potassium hydroxide in the electrolyte is 1M.
CN202210413864.0A 2022-04-14 2022-04-14 Preparation method of supercapacitor electrode material Pending CN114758903A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
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CN103084189A (en) * 2013-01-29 2013-05-08 南昌大学 Preparation method of hydrogen production photocatalyst suitable for seawater or salt lake brine
CN104577126A (en) * 2015-01-28 2015-04-29 山东大学 Method for preparing MWCNT@a-C@Co9S8 composite electrode material with uniform morphology and application of material in lithium electrode
CN105140517A (en) * 2015-09-14 2015-12-09 天津大学 Preparation method of non-water-soluble transition metal disulphide nanosheets
CN108043439A (en) * 2017-11-23 2018-05-18 江南大学 A kind of preparation method of cobalt sulfide/class graphene carbon nitrogen compound composite catalyst
CN108172798A (en) * 2017-12-27 2018-06-15 东华大学 A kind of cobalt sulfide nickel/cobalt sulfide/carbon composite and its preparation and application
CN109888307A (en) * 2019-03-14 2019-06-14 武汉理工大学 A kind of cobalt sulphur compound/nitrogen sulfur doping carbon composite catalytic agent and preparation method thereof
CN110299510A (en) * 2019-07-11 2019-10-01 青岛科技大学 A kind of preparation using conductive carbon cloth as the bimetallic sulfide of substrate and its application in terms of negative electrode of lithium ion battery
WO2021219759A1 (en) * 2020-04-29 2021-11-04 Toyota Motor Europe (bi)metal sulfide polymer composite material, and its use as catalyst for hydrogen production
CN114156467A (en) * 2021-11-05 2022-03-08 湖南理工学院 NC @ CoS with porous layered structure2Composite material and preparation method thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103084189A (en) * 2013-01-29 2013-05-08 南昌大学 Preparation method of hydrogen production photocatalyst suitable for seawater or salt lake brine
CN104577126A (en) * 2015-01-28 2015-04-29 山东大学 Method for preparing MWCNT@a-C@Co9S8 composite electrode material with uniform morphology and application of material in lithium electrode
CN105140517A (en) * 2015-09-14 2015-12-09 天津大学 Preparation method of non-water-soluble transition metal disulphide nanosheets
CN108043439A (en) * 2017-11-23 2018-05-18 江南大学 A kind of preparation method of cobalt sulfide/class graphene carbon nitrogen compound composite catalyst
CN108172798A (en) * 2017-12-27 2018-06-15 东华大学 A kind of cobalt sulfide nickel/cobalt sulfide/carbon composite and its preparation and application
CN109888307A (en) * 2019-03-14 2019-06-14 武汉理工大学 A kind of cobalt sulphur compound/nitrogen sulfur doping carbon composite catalytic agent and preparation method thereof
CN110299510A (en) * 2019-07-11 2019-10-01 青岛科技大学 A kind of preparation using conductive carbon cloth as the bimetallic sulfide of substrate and its application in terms of negative electrode of lithium ion battery
WO2021219759A1 (en) * 2020-04-29 2021-11-04 Toyota Motor Europe (bi)metal sulfide polymer composite material, and its use as catalyst for hydrogen production
CN114156467A (en) * 2021-11-05 2022-03-08 湖南理工学院 NC @ CoS with porous layered structure2Composite material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
WEIYI HAO, CHEN YUAN, WANSHENG RUAN, BEN MA, FEI TENG: ""Easy-Controlled Vacancy Concentration and Effect on Electrochemical Performance of Co3O4"", JANUARY 2022SSRN ELECTRONIC JOURNAL *

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