CN110148527A - 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 PDFInfo
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- CN110148527A CN110148527A CN201910365041.3A CN201910365041A CN110148527A CN 110148527 A CN110148527 A CN 110148527A CN 201910365041 A CN201910365041 A CN 201910365041A CN 110148527 A CN110148527 A CN 110148527A
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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
-
- 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
Technical field
The present invention relates to electrode material for super capacitor technical field, in particular to a kind of cobalt molybdenum for supercapacitor
The preparation method of sulfide electrode material.
Background technique
High power density of the supercapacitor as a kind of high-energy density for having both lithium ion battery and traditional capacitor
A kind of model electrochemical energy storage device, it is big with capacity, charge discharge life is long, charge-discharge velocity is fast, it is very high to can provide
The advantages that discharge current, operating temperature range are wide, environmentally protective and cheap, easy to use and reliable.Therefore, super electricity
Container can obtain in many fields such as electronics field, solar energy electricity generation system, smart electric grid system, new-energy automobile
To being widely applied.
Supercapacitor can be divided into electric double layer capacitance and faraday's capacity capacitor according to the difference of energy storage mechnism, electrification
The chemical property for learning active material is the core content of supercapacitor area research, and the chemical property of active material is direct
Determine the performance of supercapacitor.At present in research, generally require to add in the preparation process of electrode material for super capacitor
Entering carbon black as conductive agent, polytetrafluoroethylene (PTFE) not only complicates preparation process as bonding agent, and cost is got higher, and
It also will affect the chemical property of electrode material itself.It thus needs to develop a kind of new electrode material for super capacitor preparation side
Formula, by can be avoided it is existing using carbon black and polytetrafluoroethylene (PTFE) in a manner of deficiency.
Summary of the invention
In view of this, the present invention is directed to propose a kind of preparation side of the cobalt molybdenum sulphide electrode material for supercapacitor
Method, to be capable of providing a kind of new electrode material for super capacitor preparation method.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of preparation method of the cobalt molybdenum sulphide electrode material for supercapacitor, which includes following
Step:
A, cobalt source is dissolved in deionized water and is stirred and is configured to containing Co2+The homogeneous solution A of ion；
B, tetrathiomolybdate is dissolved in the volume ratio of deionized water and dehydrated alcohol is in the ethyl alcohol water mixed solution of 1.5:1
It is configured to containing MoS4 2-The homogeneous solution B of ion；
C, it takes the solution A of 1 volume to be slowly dropped in the solution B of 5 volumes, and is stirred to obtain the molybdenum sulphide containing cobalt
Mixed solution C；
D, solution C is transferred in crystallizing kettle, and nickel foam is placed in crystallizing kettle, solution is made not have nickel foam, sealed
Crystallizing kettle reacts 4-12h at 90-120 DEG C, makes cobalt molybdenum sulphide homoepitaxial in nickel foam；
E, crystallizing kettle is cooled to room temperature, nickel foam is taken out, and dried at 30-60 DEG C, to obtain with nickel foam
For the cobalt molybdenum sulphide electrode material of substrate.
Further, the cobalt source is one of cobalt chloride and cobalt nitrate.
Further, the tetrathiomolybdate is one of four sulphur sodium molybdates, four sulphur potassium molybdates, ammonium tetrathiomolybdate.
Further, the drying carries out in the vacuum oven that absolute pressure is 5KPa, and dries 10h.
Further, the nickel foam is placed in crystallizing kettle to be preprocessed, and the pretreatment includes successively using hydrogen-oxygen
Change potassium solution, acetone soln, second alcohol and water and carries out carrying out washing treatment.
It further, is using magnetic agitation in the step a and step b.
Further, Co in the solution A2+The concentration of ion is 0.2mol/L, the MoS in the solution B4 2-Ion
Concentration is 0.04mol/L, and the solution A of 1 volume is to be slowly dropped in the solution B of 5 volumes in 0.5h.
Compared with the existing technology, present invention has the advantage that
The preparation method of cobalt molybdenum sulphide electrode material of the invention, by the method for hydro-thermal in nickel foam fabricated in situ
Product can simplify preparation process using fabricated in situ electrode material in nickel foam, and the electrode material prepared is in electrochemistry
It can be not necessarily to binder in test, binder can be reduced to the obstruction of electro-chemical test, and the transmission of electronics and ion can be enhanced,
Active material utilization can be made to greatly improve, specific capacity increases, and cycle performance improves, and can be improved the electrochemistry of electrode material
Performance can provide a kind of excellent electrode material for super capacitor, and is conducive to the popularization in super capacitance electrode material field
Using.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention
It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the scanning electron microscopic picture of electrode material prepared by example 1；
Fig. 2 is the scanning electron microscopic picture of electrode material prepared by example 2；
Fig. 3 is the scanning electron microscopic picture of electrode material prepared by example 3；
Fig. 4 is the specific capacitance value of electrode material prepared by example 1-3, and 4h, 8h, 12h respectively correspond example 1, reality in figure
The specific capacitance value of electrode material prepared by example 2, example 3.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
The present embodiment is related to a kind of preparation method of cobalt molybdenum sulphide electrode material for supercapacitor, the preparation side
Method includes that first cobalt source is dissolved in deionized water and is stirred to be configured to containing Co2+The homogeneous solution A of ion, then tetrathiomolybdate is molten
It is configured in the ethyl alcohol water mixed solution that deionized water and the volume ratio of dehydrated alcohol are 1.5:1 containing MoS4 2-Ion it is uniform
Solution B.Then, it takes the solution A of 1 volume to be slowly dropped in the solution B of 5 volumes in 0.5h, and is stirred to obtain containing cobalt
The mixed solution C of molybdenum sulphide then, then solution C is transferred in crystallizing kettle, and nickel foam is placed in crystallizing kettle, is made molten
Liquid did not had nickel foam, reacts 4-12h at 90-120 DEG C after sealing crystallizing kettle, makes cobalt molybdenum sulphide homoepitaxial in nickel foam
On.Finally, crystallizing kettle is cooled to room temperature, nickel foam is taken out, and dried at 30-60 DEG C and be to get to nickel foam
The cobalt molybdenum sulphide electrode material of substrate.
Wherein, the above-described cobalt source of the present embodiment is specially cobalt chloride (CoCl2) and cobalt nitrate (Co (NO3)2) in one
Kind, tetrathiomolybdate is specially four sulphur sodium molybdate (Na2MoS4), four sulphur potassium molybdate (K2MoS4), ammonium tetrathiomolybdate ((NH4)2MoS4One of), and solution A and solution B use magnetic agitation mode preferably to be formed containing the uniform molten of corresponding ion
Liquid.And the drying of the present embodiment is then specially to carry out in the vacuum oven that absolute pressure is 5KPa, and drying time is 10h.Together
When, nickel foam be also first pass through pretreatment after be placed in crystallizing kettle again, and the pretreatment include successively with potassium hydroxide solution,
Acetone soln, second alcohol and water carry out carrying out washing treatment, wherein potassium hydroxide solution, acetone soln concentration be 1mol/L.
In addition, Co in the solution A configured in the present embodiment2+The concentration of ion is 0.2mol/L, in the solution B of configuration
MoS4 2-The concentration of ion is then 0.04mol/L.
The preparation method of the present embodiment fabricated in situ product in nickel foam by the method for hydro-thermal, can simplify preparation work
Skill, and the electrode material prepared can enhance the transmission of electronics and ion, active material utilization can be made to greatly improve, specific capacity increases
Adding, cycle performance improves, the chemical property of electrode material can be improved, and it is capable of providing a kind of excellent electrode of super capacitor
Material.
It is described further below in conjunction with specific preparating example with the preparation method to the present embodiment.
Example 1
In the preparation for the cobalt molybdenum sulphide electrode material of supercapacitor of this example, first by CoCl2It is dissolved in
Magnetic agitation is configured to containing Co in ionized water2+The homogeneous solution A of ion 0.2mol/L, then by (NH4)2MoS4It is dissolved in deionized water
It is configured to for magnetic agitation in the ethyl alcohol water mixed solution of 1.5:1 containing MoS with dehydrated alcohol volume ratio4 2-Ion 0.04mol/L's
Homogeneous solution B.Then, it takes the solution A of 1 volume to be slowly dropped in 5 bulk solution B in 0.5h, and is stirred and is mixed
Close solution C.
Then, obtained mixed solution C is transferred in crystallizing kettle, and the nickel foam pre-processed is placed in crystallizing kettle
It is interior, so that solution was not had nickel foam, reacts 4h under the conditions of 90 DEG C after sealing crystallizing kettle.After fully reacting, crystallizing kettle is cooled to
Room temperature takes out nickel foam, and dries 10h in the vacuum oven that temperature is 30 DEG C, absolute pressure is 5kPa, just obtained after drying with
Nickel foam is the cobalt molybdenum sulphide electrode material of substrate.
The scanning electron microscopic picture of obtained cobalt molybdenum sulphide electrode material is as shown in Figure 1.Obtained cobalt molybdenum is vulcanized
Object electrode material carries out electro-chemical test.In electro-chemical test three-electrode system, using nickel foam as the cobalt molybdenum sulphide of substrate
Electrode material for super capacitor is working electrode, and platinum electrode is auxiliary electrode, and saturated calomel electrode is mole dense as reference electrode
The KOH aqueous solution that degree is 1mol/L carries out constant current charge-discharge (GCD) electro-chemical test as electrolyte.As shown in Figure 4,
Test discovery is in 0-0.5V voltage range, and specific capacitance value reaches 769F/g under the current density of 0.5A/g.
Example 2
In the preparation for the cobalt molybdenum sulphide electrode material of supercapacitor of this example, first by CoCl2It is dissolved in
Magnetic agitation is configured to containing Co in ionized water2+The homogeneous solution A of ion 0.2mol/L, then by K2MoS4It is dissolved in deionized water and nothing
Water-ethanol volume ratio is that magnetic agitation is configured to containing MoS in the ethyl alcohol water mixed solution of 1.5:14 2-Ion 0.04mol/L's is uniform
Solution B.Then, it takes the solution A of 1 volume to be slowly dropped in the solution B of 5 volumes in 0.5h, and is stirred and is mixed
Solution C.
Then, obtained mixed solution C is transferred in crystallizing kettle, and the nickel foam pre-processed is placed in crystallizing kettle
It is interior, so that solution was not had nickel foam, reacts 8h under the conditions of 90 DEG C after sealing crystallizing kettle.After fully reacting, crystallizing kettle is cooled to
Room temperature takes out nickel foam, and dries 10h in the vacuum oven that temperature is 30 DEG C, absolute pressure is 5kPa, just obtained after drying with
Nickel foam is the cobalt molybdenum sulphide electrode material of substrate.
The scanning electron microscopic picture of obtained cobalt molybdenum sulphide electrode material is as shown in Figure 2.Obtained cobalt molybdenum is vulcanized
Object electrode material carries out electro-chemical test, and test condition is identical with example 1, as shown in Figure 4, test discovery is in 0-0.5V electricity
It presses in range, specific capacitance value reaches 1030F/g under the current density of 0.5A/g.
Example 3
In the preparation for the cobalt molybdenum sulphide electrode material of supercapacitor of this example, first by Co (NO3)2It is dissolved in
Magnetic agitation is configured to containing Co in deionized water2+The homogeneous solution A of ion 0.2mol/L, then by Na2MoS4It is dissolved in deionized water
It is configured to for magnetic agitation in the ethyl alcohol water mixed solution of 1.5:1 containing MoS with dehydrated alcohol volume ratio4 2-Ion 0.04mol/L's
Homogeneous solution B.Then, it takes the solution A of 1 volume to be slowly dropped in the solution B of 5 volumes in 0.5h, and is stirred to obtain
Mixed solution C.
Then, obtained mixed solution C is transferred in crystallizing kettle, and the nickel foam pre-processed is placed in crystallizing kettle
It is interior, so that solution was not had nickel foam, reacts 12h under the conditions of 120 DEG C after sealing crystallizing kettle.It is after fully reacting, crystallizing kettle is cooling
To room temperature, nickel foam is taken out, and dries 10h in the vacuum oven that temperature is 30 DEG C, absolute pressure is 5kPa, is just obtained after drying
Using nickel foam as the cobalt molybdenum sulphide electrode material of substrate.
The scanning electron microscopic picture of obtained cobalt molybdenum sulphide electrode material is as shown in Figure 3.Obtained cobalt molybdenum is vulcanized
Object electrode material carries out electro-chemical test, and test condition is identical with example 1, as shown in Figure 4, test discovery is in 0-0.5V electricity
It presses in range, specific capacitance value reaches 2514F/g under the current density of 0.5A/g.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of the cobalt molybdenum sulphide electrode material for supercapacitor, it is characterised in that: the preparation method
It comprises the following steps that
A, cobalt source is dissolved in deionized water and is stirred and is configured to containing Co2+The homogeneous solution A of ion；
B, tetrathiomolybdate is dissolved in the volume ratio of deionized water and dehydrated alcohol to configure in the ethyl alcohol water mixed solution of 1.5:1
At containing MoS4 2-The homogeneous solution B of ion；
C, it takes the solution A of 1 volume to be slowly dropped in the solution B of 5 volumes, and is stirred to obtain the mixing of the molybdenum sulphide containing cobalt
Solution C；
D, solution C is transferred in crystallizing kettle, and nickel foam is placed in crystallizing kettle, solution is made not have nickel foam, seal crystallization
Kettle reacts 4-12h at 90-120 DEG C, makes cobalt molybdenum sulphide homoepitaxial in nickel foam；
E, crystallizing kettle is cooled to room temperature, nickel foam is taken out, and dried at 30-60 DEG C, to obtain using nickel foam as base
The cobalt molybdenum sulphide electrode material at bottom.
2. the preparation method of the cobalt molybdenum sulphide electrode material according to claim 1 for supercapacitor, feature
Be: the cobalt source is one of cobalt chloride and cobalt nitrate.
3. the preparation method of the cobalt molybdenum sulphide electrode material according to claim 1 for supercapacitor, feature
Be: the tetrathiomolybdate is one of four sulphur sodium molybdates, four sulphur potassium molybdates, ammonium tetrathiomolybdate.
4. the preparation method of the cobalt molybdenum sulphide electrode material according to claim 1 for supercapacitor, feature
Be: the drying carries out in the vacuum oven that absolute pressure is 5KPa, and dries 10h.
5. the preparation method of the cobalt molybdenum sulphide electrode material according to claim 1 for supercapacitor, feature
Be: the nickel foam is placed in crystallizing kettle to be preprocessed, and the pretreatment includes successively using potassium hydroxide solution, acetone
Solution, second alcohol and water carry out carrying out washing treatment.
6. the preparation method of the cobalt molybdenum sulphide electrode material according to claim 1 for supercapacitor, feature
It is: is using magnetic agitation in the step a and step b.
7. the preparation of the cobalt molybdenum sulphide electrode material according to any one of claim 1 to 6 for supercapacitor
Method, it is characterised in that: Co in the solution A2+The concentration of ion is 0.2mol/L, the MoS in the solution B4 2-Ion it is dense
Degree is 0.04mol/L, and the solution A of 1 volume is to be slowly dropped in the solution B of 5 volumes in 0.5h.
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Cited By (4)
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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 |
| CN113270276A (en) * | 2021-05-19 | 2021-08-17 | 河北科技大学 | Preparation process of supercapacitor electrode |
| CN113380551A (en) * | 2021-05-18 | 2021-09-10 | 三峡大学 | Method for improving capacity of Mo-Co-S super capacitor |
| CN113838684A (en) * | 2021-09-27 | 2021-12-24 | 太原理工大学 | CoMo2S4Preparation method of foamed nickel supercapacitor electrode material |
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