CN110148527B - Preparation method of cobalt molybdenum sulfide electrode material for super capacitor - Google Patents

Preparation method of cobalt molybdenum sulfide electrode material for super capacitor Download PDF

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CN110148527B
CN110148527B CN201910365041.3A CN201910365041A CN110148527B CN 110148527 B CN110148527 B CN 110148527B CN 201910365041 A CN201910365041 A CN 201910365041A CN 110148527 B CN110148527 B CN 110148527B
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solution
electrode material
molybdenum sulfide
cobalt
foamed nickel
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CN110148527A (en
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张向京
刘倩倩
徐晓阳
赵莹
胡永琪
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Hebei University of Science and Technology
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Hebei University of Science and Technology
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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
    • 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
    • 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
    • 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 a preparation method of a cobalt molybdenum sulfide electrode material for a super capacitor, which comprises the steps of dissolving a cobalt source in deionized water and stirring to obtain a solution A, dissolving tetrathiomolybdate in an ethanol-water mixed solution and stirring to obtain a solution B, slowly dropping the solution A into the solution B and stirring to obtain a mixed solution C, transferring the mixed solution C into a crystallization kettle, placing foamed nickel into the crystallization kettle to enable the solution to be submerged in the foamed nickel, reacting for 4-12 hours at 90-120 ℃, cooling the crystallization kettle to room temperature after complete reaction, taking out the foamed nickel, and drying at 30-60 ℃ to obtain the cobalt molybdenum sulfide electrode material taking the foamed nickel as a substrate. The preparation method can provide a novel preparation mode of the electrode material of the super capacitor, simplify the preparation process and provide an excellent electrode material of the super capacitor.

Description

Preparation method of cobalt molybdenum sulfide electrode material for super capacitor
Technical Field
The invention relates to the technical field of electrode materials of a super capacitor, in particular to a preparation method of a cobalt molybdenum sulfide electrode material for a super capacitor.
Background
The super capacitor is used as a novel electrochemical energy storage device with high energy density of a lithium ion battery and high power density of a traditional capacitor, and has the advantages of large capacity, long charging and discharging service life, high charging and discharging speed, capability of providing high discharging current, wide working temperature range, environmental friendliness, low price, convenience and reliability in use and the like. Therefore, the super capacitor can be widely applied to the fields of electronic products, solar energy power generation systems, smart grid systems, new energy automobiles and the like.
The super capacitor can be divided into a double electric layer capacitor and a Faraday capacitor according to different energy storage mechanisms, the electrochemical performance of an electrochemical active material is the core content of research in the field of the super capacitor, and the electrochemical performance of the active material directly determines the performance of the super capacitor. In the current research, carbon black is often required to be added as a conductive agent and polytetrafluoroethylene is used as a binder in the preparation process of the electrode material of the supercapacitor, which not only complicates the preparation process and increases the cost, but also affects the electrochemical performance of the electrode material. Therefore, it is needed to develop a new method for preparing an electrode material of a supercapacitor, so as to avoid the disadvantages of the existing methods using carbon black and polytetrafluoroethylene.
Disclosure of Invention
In view of the above, the present invention is directed to a method for preparing a cobalt molybdenum sulfide electrode material for a supercapacitor, so as to provide a new method for preparing an electrode material for a supercapacitor.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a cobalt molybdenum sulfide electrode material for a super capacitor comprises the following steps:
a. dissolving cobalt source in deionized water and stirring to prepare the Co-containing material2+A homogeneous solution A of ions;
b. dissolving tetrathiomolybdate into deionized water and absolute ethyl alcohol according to the volume ratio of 1.5:1 is prepared into the solution containing MoS in the ethanol-water mixed solution4 2-A homogeneous solution B of ions;
c. slowly dripping 1 volume of the solution A into 5 volumes of the solution B, and stirring and mixing to obtain a mixed solution C containing cobalt-molybdenum sulfide;
d. transferring the solution C into a crystallization kettle, placing the foamed nickel into the crystallization kettle to enable the solution to submerge the foamed nickel, sealing the crystallization kettle, and reacting at the temperature of 90-120 ℃ for 4-12 hours to enable the cobalt molybdenum sulfide to uniformly grow on the foamed nickel;
e. and cooling the crystallization kettle to room temperature, taking out the foamed nickel, and drying at the temperature of 30-60 ℃ to obtain the cobalt molybdenum sulfide electrode material taking the foamed nickel as the substrate.
Further, the cobalt source is one of cobalt chloride and cobalt nitrate.
Further, the tetrathiomolybdate is one of sodium tetrathiomolybdate, potassium tetrathiomolybdate and ammonium tetrathiomolybdate.
Further, the drying is carried out in a vacuum drying oven with the absolute pressure of 5KPa, and the drying is carried out for 10 h.
Further, the nickel foam is pretreated and then placed in a crystallization kettle, and the pretreatment comprises washing treatment by sequentially using a potassium hydroxide solution, an acetone solution, ethanol and water.
Further, magnetic stirring is adopted in both the step a and the step b.
Further, Co in the solution A2+The concentration of ions is 0.2mol/L, and MoS in the solution B4 2-The concentration of the ions was 0.04mol/L, and 1 volume of solution A was added slowly dropwise to 5 volumes of solution B over 0.5 h.
Compared with the prior art, the invention has the following advantages:
according to the preparation method of the cobalt molybdenum sulfide electrode material, a product is synthesized in situ on the foamed nickel through a hydrothermal method, the preparation process can be simplified by utilizing the electrode material synthesized in situ on the foamed nickel, a binder can be omitted in an electrochemical test of the prepared electrode material, the obstruction of the binder to the electrochemical test can be reduced, the transmission of electrons and ions can be enhanced, the utilization rate of active substances can be greatly improved, the specific capacity is increased, the circulating performance is improved, the electrochemical performance of the electrode material can be improved, an excellent supercapacitor electrode material can be provided, and the popularization and the application in the field of supercapacitor electrode materials are facilitated.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a scanning electron micrograph of an electrode material prepared in example 1;
FIG. 2 is a scanning electron micrograph of the electrode material prepared in example 2;
FIG. 3 is a scanning electron micrograph of the electrode material prepared in example 3;
FIG. 4 is a graph showing specific capacitance values of the electrode materials prepared in examples 1 to 3, wherein 4h, 8h, and 12h correspond to the specific capacitance values of the electrode materials prepared in examples 1, 2, and 3, respectively.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The embodiment relates to a preparation method of a cobalt molybdenum sulfide electrode material for a super capacitor, which comprises the steps of dissolving a cobalt source in deionized water and stirring to prepare a cobalt-containing electrode material2+Dissolving tetrathiomolybdate into the uniform solution A of ions, wherein the volume ratio of the tetrathiomolybdate to the deionized water to the absolute ethyl alcohol is 1.5:1 is prepared into the solution containing MoS in the ethanol-water mixed solution4 2-Homogeneous solution B of ions. And then, slowly dripping 1 volume of the solution A into 5 volumes of the solution B within 0.5 hour, stirring and mixing to obtain a mixed solution C containing cobalt-molybdenum sulfide, then transferring the solution C into a crystallization kettle, placing foamed nickel into the crystallization kettle to enable the solution to be submerged in the foamed nickel, sealing the crystallization kettle, and reacting for 4-12 hours at 90-120 ℃ to enable the cobalt-molybdenum sulfide to uniformly grow on the foamed nickel. And finally, cooling the crystallization kettle to room temperature, taking out the foamed nickel, and drying at the temperature of 30-60 ℃ to obtain the cobalt molybdenum sulfide electrode material taking the foamed nickel as the substrate.
In this embodiment, the cobalt source is specifically cobalt chloride (CoCl)2) And cobalt nitrate (Co (NO)3)2) One of the four sulfur molybdate is sodium tetrasulfur molybdate (Na)2MoS4) Potassium tetrathiomolybdate (K)2MoS4) Ammonium tetrathiomolybdate ((NH)4)2MoS4) And both solution a and solution B are preferably magnetically stirred to form a homogeneous solution containing the corresponding ion. The drying of the embodiment is specifically performed in a vacuum drying oven with an absolute pressure of 5KPa, and the drying time is 10 hours. Meanwhile, the foamed nickel is pretreated and then placed in a crystallization kettle, and the pretreatment comprises washing treatment by sequentially using a potassium hydroxide solution, an acetone solution, ethanol and water, wherein the concentration of the potassium hydroxide solution and the concentration of the acetone solution are 1 mol/L.
In addition, Co in solution A provided in the present embodiment2+The concentration of the ions is 0.2mol/L, and the prepared MoS in the solution B4 2-The concentration of the ions was 0.04 mol/L.
According to the preparation method, the product is synthesized in situ on the foamed nickel by a hydrothermal method, the preparation process can be simplified, the prepared electrode material can enhance the transmission of electrons and ions, the utilization rate of active substances can be greatly improved, the specific capacity is increased, the cycle performance is good, the electrochemical performance of the electrode material can be improved, and the excellent supercapacitor electrode material can be provided.
The preparation method of this example will be further described with reference to specific preparation examples.
Example 1
In the preparation of the cobalt molybdenum sulfide electrode material for a supercapacitor of this example, CoCl was first added2Dissolving in deionized water, stirring by magnetic force to obtain Co-containing solution2+A homogeneous solution A of 0.2mol/L ions, and (NH)4)2MoS4Dissolving the mixture into an ethanol-water mixed solution with the volume ratio of deionized water to absolute ethanol of 1.5:1, magnetically stirring the mixture to prepare the mixture containing MoS4 2-0.04mol/L of ions in the homogeneous solution B. Then, 1 volume of solution A was slowly added dropwise to 5 volumes of solution B over 0.5h, and mixed with stirring to obtain mixed solution C.
And then, transferring the obtained mixed solution C into a crystallization kettle, placing the pretreated foamed nickel into the crystallization kettle to enable the solution to cover the foamed nickel, sealing the crystallization kettle, and reacting for 4 hours at 90 ℃. And after the reaction is completed, cooling the crystallization kettle to room temperature, taking out the foamed nickel, and drying the foamed nickel in a vacuum drying oven at the temperature of 30 ℃ and the absolute pressure of 5kPa for 10 hours to obtain the cobalt molybdenum sulfide electrode material taking the foamed nickel as the substrate.
The scanning electron microscope picture of the obtained cobalt molybdenum sulfide electrode material is shown in fig. 1. And carrying out electrochemical test on the obtained cobalt molybdenum sulfide electrode material. In an electrochemical test three-electrode system, a cobalt molybdenum sulfide supercapacitor electrode material taking foamed nickel as a substrate is taken as a working electrode, a platinum electrode is taken as an auxiliary electrode, a saturated calomel electrode is taken as a reference electrode, a KOH aqueous solution with the molar concentration of 1mol/L is taken as an electrolyte, and a constant current charging and discharging (GCD) electrochemical test is carried out. As shown in FIG. 4, the test found that the specific capacitance reached 769F/g at a current density of 0.5A/g in the voltage range of 0-0.5V.
Example 2
In the preparation of the cobalt molybdenum sulfide electrode material for a supercapacitor of this example, CoCl was first added2Dissolving in deionized water, stirring by magnetic force to obtain Co-containing solution2+A homogeneous solution A of 0.2mol/L ions, and then K2MoS4Dissolving the mixture into an ethanol-water mixed solution with the volume ratio of deionized water to absolute ethanol of 1.5:1, magnetically stirring the mixture to prepare the mixture containing MoS4 2-0.04mol/L of ions in the homogeneous solution B. Then, 1 volume of solution A was slowly added dropwise to 5 volumes of solution B over 0.5h, and mixed with stirring to obtain a mixed solution C.
And then, transferring the obtained mixed solution C into a crystallization kettle, placing the pretreated foamed nickel into the crystallization kettle to enable the solution to be submerged in the foamed nickel, sealing the crystallization kettle, and reacting for 8 hours at 90 ℃. And after the reaction is completed, cooling the crystallization kettle to room temperature, taking out the foamed nickel, and drying the foamed nickel in a vacuum drying oven at the temperature of 30 ℃ and the absolute pressure of 5kPa for 10 hours to obtain the cobalt molybdenum sulfide electrode material taking the foamed nickel as the substrate.
The scanning electron microscope picture of the obtained cobalt molybdenum sulfide electrode material is shown in fig. 2. The obtained cobalt molybdenum sulfide electrode material was subjected to electrochemical tests under the same test conditions as in example 1, and as shown in fig. 4, the test found that the specific capacitance value reached 1030F/g at a current density of 0.5A/g within a voltage range of 0 to 0.5V.
Example 3
In the preparation of the cobalt molybdenum sulfide electrode material for a supercapacitor of this example, Co (NO) was first introduced3)2Dissolved in deionized water and stirred by magnetic force to prepare the mixture containing Co2+A homogeneous solution A of 0.2mol/L ions, and Na2MoS4Dissolving the mixture into an ethanol-water mixed solution with the volume ratio of deionized water to absolute ethanol of 1.5:1, magnetically stirring the mixture to prepare the mixture containing MoS4 2-0.04mol/L of ions in the homogeneous solution B. Then, 1 volume of solution A was slowly added dropwise to 5 volumes of solution B over 0.5h, and mixed with stirring to obtain a mixed solution C.
And then, transferring the obtained mixed solution C into a crystallization kettle, placing the pretreated foamed nickel into the crystallization kettle to enable the solution to be submerged in the foamed nickel, sealing the crystallization kettle, and reacting for 12 hours at 120 ℃. And after the reaction is completed, cooling the crystallization kettle to room temperature, taking out the foamed nickel, and drying the foamed nickel in a vacuum drying oven at the temperature of 30 ℃ and the absolute pressure of 5kPa for 10 hours to obtain the cobalt molybdenum sulfide electrode material taking the foamed nickel as the substrate.
The scanning electron microscope picture of the obtained cobalt molybdenum sulfide electrode material is shown in fig. 3. The obtained cobalt molybdenum sulfide electrode material was subjected to electrochemical tests under the same test conditions as in example 1, and as shown in fig. 4, the test found that the specific capacitance value reached 2514F/g at a current density of 0.5A/g within a voltage range of 0 to 0.5V.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (3)

1. A preparation method of a cobalt molybdenum sulfide electrode material for a super capacitor is characterized by comprising the following steps: the preparation method comprises the following steps:
a. dissolving cobalt chloride in deionized water and stirring to prepare the cobalt-containing catalyst2+Homogeneous solution A of ions, Co in said solution A2+The concentration of the ions is 0.2 mol/L;
b. dissolving sodium tetrathiomolybdate or potassium tetrathiomolybdate in an ethanol-water mixed solution with the volume ratio of deionized water to absolute ethyl alcohol of 1.5:1 to prepare the solution containing MoS4 2-Homogeneous solution B of ions, MoS in said solution B4 2-The concentration of the ions is 0.04 mol/L;
c. slowly dripping 1 volume of the solution A into 5 volumes of the solution B, stirring and mixing to obtain a mixed solution C containing cobalt-molybdenum sulfide, wherein the 1 volume of the solution A is slowly dripped into the 5 volumes of the solution B within 0.5 h;
d. transferring the solution C into a crystallization kettle, placing the foamed nickel into the crystallization kettle to enable the solution to submerge the foamed nickel, sealing the crystallization kettle, and reacting at the temperature of 90-120 ℃ for 4-12 hours to enable the cobalt molybdenum sulfide to uniformly grow on the foamed nickel;
e. cooling the crystallization kettle to room temperature, taking out the foamed nickel, and drying at 30-60 ℃ to obtain a cobalt molybdenum sulfide electrode material taking the foamed nickel as a substrate;
the method comprises the following steps of preparing a nickel foam, and placing the nickel foam into a crystallization kettle after pretreatment, wherein the pretreatment comprises washing treatment by sequentially using a potassium hydroxide solution, an acetone solution, ethanol and water.
2. The method of preparing a cobalt molybdenum sulfide electrode material for a supercapacitor according to claim 1, wherein: the drying is carried out in a vacuum drying oven with the absolute pressure of 5KPa, and the drying is carried out for 10 h.
3. The method of preparing a cobalt molybdenum sulfide electrode material for a supercapacitor according to claim 1, wherein: and in the step a and the step b, magnetic stirring is adopted.
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CN110853931A (en) * 2019-11-01 2020-02-28 河北科技大学 Synthesis method of cobalt-molybdenum bimetallic sulfide for supercapacitor electrode material
CN113380551B (en) * 2021-05-18 2022-04-08 三峡大学 Method for improving capacity of Mo-Co-S super capacitor
CN113270276B (en) * 2021-05-19 2022-09-20 河北科技大学 Preparation process of supercapacitor electrode
CN113838684B (en) * 2021-09-27 2023-09-15 太原理工大学 CoMo 2 S 4 Preparation method of foam nickel super capacitor electrode material

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