CN113593923A - Preparation method of cobalt sulfide/graphene-multiwalled carbon nanotube composite material, application of composite material in supercapacitor and testing method - Google Patents

Preparation method of cobalt sulfide/graphene-multiwalled carbon nanotube composite material, application of composite material in supercapacitor and testing method Download PDF

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Publication number
CN113593923A
CN113593923A CN202110852442.9A CN202110852442A CN113593923A CN 113593923 A CN113593923 A CN 113593923A CN 202110852442 A CN202110852442 A CN 202110852442A CN 113593923 A CN113593923 A CN 113593923A
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China
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graphene
composite material
cobalt sulfide
carbon nanotube
nanotube composite
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CN202110852442.9A
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Chinese (zh)
Inventor
孙蕾
龚洁
孙志鹏
赵建勇
李茂华
周皓
孙炜
赵丽萍
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Guangdong University of Technology
Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Research Institute
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Guangdong University of Technology
Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Research Institute
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Priority to CN202110852442.9A priority Critical patent/CN113593923A/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
    • H01G11/22—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
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • 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 discloses a preparation method of a cobalt sulfide/graphene-multiwalled carbon nanotube composite material, and an application and a test method thereof in a super capacitor, belonging to the field of super capacitor materials, wherein the cobalt sulfide/graphene-multiwalled carbon nanotube composite material comprises the following steps: co (NO)3)2·6H2O, thiourea, graphene oxide, a multi-walled carbon nanotube suspension and distilled water. The cobalt sulfide, the graphene and the carbon nano tube in the prepared cobalt sulfide/graphene-multi-walled carbon nano tube composite material can be effectively combined; can reduce the stacking degree of graphene and the agglomeration of carbon nano tubes, and the prepared cobalt sulfide/graphene-multi-walled carbon nano tube composite material has a unique multi-stage structure and effectively inhibitsDue to the self-aggregation of the cobalt sulfide, the cobalt sulfide nanosheet with high electrochemical activity is fully exposed, the material shows that abundant carbon nanotubes are distributed, and the carbon nanotube composite cobalt sulfide nanomaterial has high conductivity.

Description

Preparation method of cobalt sulfide/graphene-multiwalled carbon nanotube composite material, application of composite material in supercapacitor and testing method
Technical Field
The invention belongs to the field of super capacitor materials, and relates to a preparation method of a cobalt sulfide/graphene-multiwalled carbon nanotube composite material, and an application and a test method of the cobalt sulfide/graphene-multiwalled carbon nanotube composite material in a super capacitor.
Background
Graphene has excellent physicochemical properties, such as higher conductivity, excellent mechanical properties, high specific surface area, low mass-light density, good chemical stability and the like. Due to the special properties, the material is widely applied to the fields of catalyst carriers, high-molecular nano composite materials, flexible substrate materials of energy conversion and storage devices and the like, and is considered to be one of ten most potential new materials in the future.
However, graphene sheets are easy to stack, so that the excellent performance of graphene cannot be fully utilized, and the volume of the carrier expands in the charge and discharge processes, thereby reducing the capacity.
Disclosure of Invention
The invention aims to solve the problems and provide a preparation method and application of a cobalt sulfide/graphene-multi-walled carbon nanotube composite material, the prepared cobalt sulfide/graphene-multi-walled carbon nanotube composite material shows that abundant carbon nanotubes are distributed, the carbon nanotube composite cobalt sulfide nanomaterial has high conductivity, and an electrode can keep good capacity under the current density of 1-5A/g.
The preparation method of the cobalt sulfide/graphene-multi-walled carbon nanotube composite material according to the embodiment of the first aspect of the invention comprises the following steps:
1. a preparation method of a cobalt sulfide/graphene-multiwalled carbon nanotube composite material is characterized by comprising the following steps:
s1, weighing 1.184 parts by weight of Co (NO)3)2·6H2O and 0.3882 parts by weight of thiourea are placed in a beaker, 0.02 part by weight of dispersed graphene oxide and multi-walled carbon nanotube suspension and 9 parts by weight of distilled water are added, and ultrasonic dissolution is carried out for 10-15 min;
s2, after ultrasonic dissolution, strongly stirring for 30min to obtain a uniform solution, then transferring the mixed solution to a stainless steel reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction in an oven at 180 ℃ for 24 h;
and S3, after the reaction is finished, freeze-drying the reaction precipitate for 12 hours to obtain the product, namely the cobalt sulfide/graphene-multi-walled carbon nanotube composite material.
Preferably, in step S1, the mass ratio of graphene oxide to multi-walled carbon nanotubes in the dispersed graphene oxide and multi-walled carbon nanotube suspension is 8: 2.
According to the application of the cobalt sulfide/graphene-multiwall carbon nanotube composite material in the supercapacitor, the cobalt sulfide/graphene-multiwall carbon nanotube composite material is prepared by the preparation method.
The method for testing the cobalt sulfide/graphene-multi-walled carbon nanotube composite material in the supercapacitor according to the third aspect of the invention comprises the following steps:
step one, placing a piece of foamed nickel into a beaker at room temperature, sequentially performing ultrasonic treatment on the nickel for 20 minutes by using acetone, 0.5M hydrochloric acid, distilled water and absolute ethyl alcohol, drying and weighing for later use;
step two, placing the cobalt sulfide/graphene-multi-walled carbon nanotube composite material, the superconducting carbon black and the polyvinylidene fluoride in a mortar for repeated grinding for 0.5h, dropwise adding 2 drops of N-methyl pyrrolidone solution for grinding again, and uniformly coating the slurry on the cleaned and dried foamed nickel;
and step three, drying in vacuum to obtain a positive working electrode, weighing, and then carrying out three-electrode electrochemical test by using 6M KOH as electrolyte, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode.
Preferably, the nickel foam is 1 x 4cm in size2。
Preferably, the cobalt sulfide/graphene-multiwalled carbon nanotube composite material, the superconducting carbon black and the polyvinylidene fluoride are respectively 80%, 10% and 10% in percentage by weight.
Preferably, vacuum drying is carried out for 6h, maintaining the temperature at 60 ℃.
The invention has the beneficial effects that: the prepared cobalt sulfide/graphene-multiwalled carbon nanotube composite material has a diffraction peak at 2 theta of 32.2 degrees, and the cobalt sulfide, the graphene and the carbon nanotube in the composite material can be effectively combined; the carbon nano tube and the graphene are interacted, the stacking degree of the graphene can be reduced, meanwhile, the agglomeration of the carbon nano tube can also be reduced, the prepared cobalt sulfide/graphene-multiwalled carbon nano tube composite material has a unique multistage structure, the agglomeration of the cobalt sulfide is effectively inhibited, the cobalt sulfide nanosheet with high electrochemical activity is fully exposed, the material shows that the abundant carbon nano tubes are distributed, and the carbon nano tube composite cobalt sulfide nano material has high conductivity; the electrode of the invention can keep better capacity under the current density of 1-5A/g.
Drawings
FIG. 1 shows cobalt sulfide (CoS) of the present invention2) An X-ray diffraction pattern of the/graphene-multi-walled carbon nanotube composite material;
FIG. 2 shows cobalt sulfide (CoS) of the present invention2) Scanning electron microscope photos of the/graphene-multi-walled carbon nanotube composite material;
FIG. 3 shows cobalt sulfide (CoS) according to the present invention2) Specific capacity curve diagram of the/graphene-multi-walled carbon nanotube composite material under different current densities.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood 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.
Examples
A cobalt sulfide/graphene-multiwalled carbon nanotube composite material comprises the following components in parts by weight:
1.184gCo(NO3)2·6H2O；
0.3882g of thiourea;
20mg of dispersed graphene oxide and multi-walled carbon nanotube suspension;
90ml of distilled water.
Specifically, the mass ratio of the graphene oxide to the multi-walled carbon nanotubes in the dispersed graphene oxide and multi-walled carbon nanotube suspension is 8: 2.
A preparation method of a cobalt sulfide/graphene-multiwalled carbon nanotube composite material comprises the following steps:
s1, weighing 1.184g Co (NO)3)2·6H2Placing O and 0.3882g thiourea in a 250ml beaker, adding 20mg of dispersed graphene oxide and multi-walled carbon nanotube suspension and 90ml of distilled water, and ultrasonically dissolving for 10-15 min;
s2, after ultrasonic dissolution, strongly stirring for 30min to obtain a uniform solution, then transferring the mixed solution to a stainless steel reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction in an oven at 180 ℃ for 24 h;
s3, after the reaction is finished, freeze-drying the reaction precipitate for 12 hours to obtain a product, namely the cobalt sulfide/graphene-multi-walled carbon nanotube composite material;
s4, as comparison, in the above process, no GO solution is added, and the obtained product is pure CoS2。
Assembling and testing a cobalt sulfide/graphene-multiwalled carbon nanotube composite material supercapacitor device, putting a piece of foamed nickel into a beaker at room temperature, sequentially performing ultrasonic treatment on the foamed nickel for 20 minutes by using acetone, 0.5M hydrochloric acid, distilled water and absolute ethyl alcohol, drying and weighing for later use; placing the cobalt sulfide/graphene-multiwalled carbon nanotube composite material, the superconducting carbon black and the polyvinylidene fluoride in a mortar for repeated grinding for 0.5h, dropwise adding 2 drops of N-methylpyrrolidone solution for grinding again, uniformly coating the slurry on the cleaned and dried foam nickel, performing vacuum drying to obtain a positive working electrode, weighing, and then performing electrochemical test of three electrodes by using 6M KOH as an electrolyte, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode.
Specifically, the foamed nickel has a size of 1 × 4cm2。
Specifically, the cobalt sulfide/graphene-multiwalled carbon nanotube composite material, the superconducting carbon black and the polyvinylidene fluoride respectively account for 80%, 10% and 10% in percentage by weight.
Specifically, vacuum drying was carried out for 6 hours, maintaining the temperature at 60 ℃.
The prepared cobalt sulfide/graphene-multi-walled carbon nanotube composite material has a diffraction peak at 2 theta of 32.2 degrees, and the cobalt sulfide, the graphene and the carbon nanotube in the composite material can be effectively combined.
The carbon nano tube and the graphene interact with each other, the stacking degree of the graphene can be reduced, meanwhile, the agglomeration of the carbon nano tube can also be reduced, the prepared cobalt sulfide/graphene-multiwalled carbon nano tube composite material has a unique multistage structure, the agglomeration of the cobalt sulfide is effectively inhibited, the cobalt sulfide nanosheet with high electrochemical activity is fully exposed, the material shows that the abundant carbon nano tubes are distributed, and the carbon nano tube composite cobalt sulfide nano material has high conductivity.
The electrode of the invention can keep better capacity under the current density of 1-5A/g.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (7)

1. A preparation method of a cobalt sulfide/graphene-multiwalled carbon nanotube composite material is characterized by comprising the following steps:
s1, weighing 1.184 parts by weight of Co (NO)3)2·6H2O and 0.3882 parts by weight of thiourea are placed in a beaker, 0.02 part by weight of dispersed graphene oxide and multi-walled carbon nanotube suspension and 9 parts by weight of distilled water are added, and ultrasonic dissolution is carried out for 10-15 min;
s2, after ultrasonic dissolution, strongly stirring for 30min to obtain a uniform solution, then transferring the mixed solution to a stainless steel reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction in an oven at 180 ℃ for 24 h;
and S3, after the reaction is finished, freeze-drying the reaction precipitate for 12 hours to obtain the product, namely the cobalt sulfide/graphene-multi-walled carbon nanotube composite material.
2. The method for preparing the cobalt sulfide/graphene-multiwall carbon nanotube composite material according to claim 1, wherein in step S1, the mass ratio of the graphene oxide to the multiwall carbon nanotubes in the dispersed graphene oxide and multiwall carbon nanotube suspension is 8: 2.
3. The use of the cobalt sulfide/graphene-multiwall carbon nanotube composite material prepared by the method of claim 1 or 2 in a supercapacitor.
4. The method for testing the cobalt sulfide/graphene-multiwall carbon nanotube composite material in the supercapacitor according to claim 3, comprising the following steps:
step one, placing a piece of foamed nickel into a beaker at room temperature, sequentially performing ultrasonic treatment on the nickel for 20 minutes by using acetone, 0.5M hydrochloric acid, distilled water and absolute ethyl alcohol, drying and weighing for later use;
step two, placing the cobalt sulfide/graphene-multi-walled carbon nanotube composite material, the superconducting carbon black and the polyvinylidene fluoride in a mortar for repeated grinding for 0.5h, dropwise adding 2 drops of N-methyl pyrrolidone solution for grinding again, and uniformly coating the slurry on the cleaned and dried foamed nickel;
and step three, drying in vacuum to obtain a positive working electrode, weighing, and then carrying out three-electrode electrochemical test by using 6M KOH as electrolyte, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode.
5. Use of the cobalt sulfide/graphene-multiwall carbon nanotube composite material according to claim 4, wherein: the foamed nickel size is 1 x 4cm2。
6. The preparation method and the application of the cobalt sulfide/graphene-multi-walled carbon nanotube composite material as claimed in claim 4, wherein the preparation method comprises the following steps: the cobalt sulfide/graphene-multi-walled carbon nanotube composite material, the superconducting carbon black and the polyvinylidene fluoride respectively account for 80 percent, 10 percent and 10 percent by weight.
7. Use of the cobalt sulfide/graphene-multiwall carbon nanotube composite material according to claim 4, wherein: vacuum drying for 6h, keeping the temperature at 60 ℃.
CN202110852442.9A 2021-07-27 2021-07-27 Preparation method of cobalt sulfide/graphene-multiwalled carbon nanotube composite material, application of composite material in supercapacitor and testing method Pending CN113593923A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN106207172A (en) * 2016-08-30 2016-12-07 安徽师范大学 The preparation method of a kind of cobalt sulfide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery
CN112885614A (en) * 2021-01-19 2021-06-01 广东工业大学 Nickel-based metal organic framework derived nitrogen-phosphorus-oxygen co-doped nickel/carbon composite material and preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105244482A (en) * 2015-09-12 2016-01-13 复旦大学 Nickel cobalt sulfide/graphene/carbon nanotube composite material and preparation method and application thereof
CN105883939A (en) * 2016-04-07 2016-08-24 河北科技师范学院 Preparation method for nickel sulfide/graphene/carbon nano tube/cobalt sulfide three-dimensional composite hydrogen storage material
CN106207172A (en) * 2016-08-30 2016-12-07 安徽师范大学 The preparation method of a kind of cobalt sulfide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery
CN112885614A (en) * 2021-01-19 2021-06-01 广东工业大学 Nickel-based metal organic framework derived nitrogen-phosphorus-oxygen co-doped nickel/carbon composite material and preparation method and application thereof

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Title
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