CN109243843B - Superfine sulfide/graphene two-dimensional composite material and preparation method and application thereof - Google Patents
Superfine sulfide/graphene two-dimensional composite material and preparation method and application thereof Download PDFInfo
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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
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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
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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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
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- 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 superfine sulfide/graphene two-dimensional composite material and a preparation method and application thereof, wherein the preparation method comprises the following steps: step 1, adding graphene oxide and a bridging agent into water to form a mixed solution; step 2, reacting the mixed solution at 60-120 ℃ to prepare a functionalized graphene material; step 3, dispersing the functionalized graphene material in the step 2 into water, adding soluble metal salt and a sulfur source, and mixing and stirring uniformly; and 4, reacting the mixed solution obtained in the step 3 at 100-200 ℃, centrifuging and washing the obtained product, drying, and grinding to obtain the superfine sulfide/graphene composite material. The diameter of the obtained sulfide is 5-10 nm. The obtained superfine sulfide/graphene composite material can show strong interaction between the two materials, exposes more active sites, and has the advantages of high specific capacity, high multiplying power, long cycle life and the like when used as an electrode of a super capacitor.
Description
Technical Field
The invention belongs to the technical field of inorganic material preparation and new energy application, and relates to a superfine sulfide/graphene two-dimensional composite material and a preparation method and application thereof.
Background
With the rapid development of electric vehicles and portable electronic devices, research on energy storage and conversion systems is receiving attention. Super capacitors have high power density and long cycle life, and thus play an increasingly important role in the field of energy storage. The electrode material is used as the core of the super capacitor and determines the electrochemical performance of the super capacitor to a certain extent. Transition metal sulfide is widely applied to electrode materials of super capacitors due to abundant electrochemical active sites on the surface and high theoretical capacity, but the materials usually have the defects of poor conductivity, easy agglomeration and the like. The transition metal sulfide and the two-dimensional graphene are combined to construct a composite material, and the composite material has wide application potential as an electrode of a super capacitor. In general, transition metal sulfides can exhibit a wide variety of morphologies, such as nanorods, nanosheets, nanotubes, nanoparticles, and the like, on the surface of two-dimensional graphene. However, the direct compounding of the graphene and the sulfide still has a plurality of problems, on one hand, the incompatibility of the graphene and the sulfide species in the structure causes the undesirable interaction among the components, and the active material is easy to fall off after being recycled for a plurality of times, thereby influencing the electrochemical performance of the active material; on the other hand, the existing preparation method of the graphene/sulfide composite material lacks regulation and control on the size of active species, so that the active sites are less exposed, and the overall electrochemical performance is poor.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide the superfine sulfide/graphene two-dimensional composite material, and the preparation method and the application thereof.
The invention is realized by the following technical scheme:
a preparation method of an ultrafine sulfide/graphene two-dimensional composite material comprises the following steps:
step 2, reacting the mixed solution obtained in the step 1 at 60-120 ℃, and washing an obtained product to obtain a functionalized graphene material;
step 3, dispersing the functionalized graphene material in the step 2 into water, adding soluble metal salt and a sulfur source, and uniformly mixing and stirring to obtain a mixed solution;
and 4, reacting the mixed solution obtained in the step 3 at 100-200 ℃, centrifuging and washing the obtained product, drying, and grinding to obtain the superfine sulfide/graphene composite material.
Preferably, in step 1, the bridging agent is one of polyaniline, polyethyleneimine and polydopamine.
Preferably, in the step 1, the mass ratio of the graphene oxide to the bridging agent is (10-100): (10-200).
Preferably, in step 2, the reaction time is 3 to 48 hours.
Preferably, in step 3, the mass ratio of the soluble metal salt to the sulfur source is (0.1-1.0): (0.1-1.0).
Preferably, in step 3, the soluble metal salt is selected from one or two of cobalt nitrate, nickel nitrate, cobalt chloride, nickel chloride, ferric nitrate and ferric chloride.
Preferably, in step 3, the sulfur source is one of trisodium trithiocyanate, thiourea and sodium sulfide.
Preferably, in step 4, the reaction time is 5 to 24 hours.
The superfine sulfide/graphene two-dimensional composite material prepared by the preparation method has the sulfide diameter of 5-10 nm.
The superfine sulfide/graphene two-dimensional composite material is applied to the electrode material of a super capacitor.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the invention, the graphene oxide is functionalized by adopting the bridging agent, and the sulfide nanoparticles are promoted to be uniformly dispersed on the surface of the graphene by using the functional groups on the surface of the bridging agent, so that a two-dimensional composite material is formed, and the sulfide nanoparticles and the graphene show stronger interaction. Meanwhile, due to the limiting effect of the bridging agent, the prepared sulfide nano-particles have smaller sizes, can expose more active sites, and greatly improve the energy storage effect, so that the target material has excellent electrochemical performance, and has a series of advantages of high specific capacity, good rate characteristic, long cycle life and the like when being used as a super capacitor electrode material. In addition, the preparation method has the advantages of simple process, safe operation, low cost and wide application prospect.
Drawings
FIG. 1 is a scanning electron microscope image of the prepared superfine sulfide/graphene two-dimensional composite material;
FIG. 2 is a cyclic voltammetry curve diagram of the prepared superfine sulfide/graphene two-dimensional composite material as a supercapacitor electrode material.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The preparation method of the superfine sulfide/graphene composite material comprises the following steps:
And 2, transferring the mixed solution in the step 1 into a constant-temperature oil bath or water bath at the temperature of 60-120 ℃, keeping for 3-48 hours, and centrifugally washing the obtained product to be neutral to obtain the functionalized graphene material.
And 3, dispersing the functionalized graphene material in the step 2 into 20-100mL of water, and mixing the soluble metal salt and the sulfur source according to a mass ratio (0.1-1.0): (0.1-1.0) respectively adding the materials into the aqueous solution of the functionalized graphene material, and uniformly mixing and stirring; the soluble metal salt is selected from one or two of cobalt nitrate, nickel nitrate, ferric chloride, cobalt chloride and nickel chloride, and the sulfur source is one of trisodium trithiocyanate, thiourea and sodium sulfide.
And 4, reacting the mixed solution obtained in the step 3 at 100-200 ℃ for 5-24 hours, centrifuging and washing the obtained product to be neutral, drying, and grinding to obtain the superfine sulfide/graphene two-dimensional composite material.
Wherein the mass ratio of the graphene oxide, the bridging agent, the soluble metal salt and the sulfur source is (10-100): (10-200): (0.1-1.0): (0.1-1.0).
The particle size of the sulfide in the superfine sulfide/graphene two-dimensional composite material obtained by the preparation method is 5-10nm, more active sites can be exposed, and the superfine sulfide/graphene two-dimensional composite material can be used as a supercapacitor electrode material.
Example 1
Adding 20mg of graphene oxide into 100mL of deionized water, ultrasonically mixing and stirring uniformly, adding 30mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 80 ℃ for 12 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.3g of cobalt chloride and 0.5g of trisodium trithiocyanate at room temperature, mixing and stirring uniformly, reacting at 120 ℃ for 18 hours, centrifugally washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
The prepared superfine cobalt sulfide/graphene two-dimensional composite material is characterized by a scanning electron microscope, and the characterization result is shown in fig. 1, so that the superfine cobalt sulfide nanoparticles can be uniformly dispersed on the surface of the graphene, and the cobalt sulfide nanoparticles have small size and diameter of 5-10 nm.
Example 2
Adding 20mg of graphene oxide into 100mL of deionized water, ultrasonically mixing and stirring uniformly, adding 30mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 80 ℃ for 12 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.3g of cobalt chloride and 0.5g of trisodium trithiocyanate at room temperature, mixing and stirring uniformly, reacting at 180 ℃ for 12 hours, centrifugally washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
The superfine cobalt sulfide/graphene two-dimensional composite material is used as an electrode material of a super capacitor to be tested, and fig. 2 is a cyclic voltammetry curve diagram of the electrode material, and the result shows that the electrode material shows excellent capacitance characteristics compared with a pure cobalt sulfide electrode.
Example 3
Adding 50mg of graphene oxide into 100mL of deionized water, ultrasonically mixing and stirring uniformly, adding 80mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 80 ℃ for 24 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.3g of cobalt nitrate and 0.5g of trisodium trithiocyanate at room temperature, mixing and stirring uniformly, reacting at 180 ℃ for 12 hours, centrifugally washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
Example 4
Adding 50mg of graphene oxide into 100mL of deionized water, ultrasonically mixing and stirring uniformly, adding 80mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 80 ℃ for 24 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.3g of cobalt nitrate and 1.0g of trisodium trithiocyanate at room temperature, mixing and stirring uniformly, reacting at 120 ℃ for 24 hours, centrifugally washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
Example 5
Adding 50mg of graphene oxide into 100mL of deionized water, ultrasonically mixing and stirring uniformly, adding 80mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 80 ℃ for 24 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.1g of cobalt chloride, 0.1g of nickel chloride and 1.0g of trisodium trithiocyanate at room temperature, mixing and stirring uniformly, reacting at 120 ℃ for 24 hours, centrifugally washing the obtained product to be neutral, drying, and grinding to obtain the superfine nickel cobalt sulfide/graphene two-dimensional composite material.
Example 6
Adding 30mg of graphene oxide into 100mL of deionized water, ultrasonically mixing and stirring uniformly, adding 80mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 80 ℃ for 24 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.2g of cobalt chloride, 0.1g of nickel chloride and 1.0g of trithiocyanuric acid trisodium salt at room temperature, mixing and stirring uniformly, reacting at 180 ℃ for 12 hours, centrifugally washing the obtained product to be neutral, drying, and grinding to obtain the superfine nickel cobalt sulfide/graphene two-dimensional composite material.
Example 7
Adding 10mg of graphene oxide into 50mL of deionized water, ultrasonically mixing and stirring uniformly, adding 10mg of polyaniline into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a constant temperature oil bath at 60 ℃ for 48 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyaniline/graphene composite material into 50mL of solution, adding 0.1g of nickel nitrate and 0.1g of thiourea at room temperature, mixing and stirring uniformly, reacting at 100 ℃ for 18 hours, centrifuging and washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
Example 8
Adding 100mg of graphene oxide into 200mL of deionized water, ultrasonically mixing and stirring uniformly, adding 30mg of polydopamine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a constant temperature oil bath at 100 ℃ for 35 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polydopamine/graphene composite material into 50mL of solution, adding 0.5g of nickel chloride and 0.1g of sodium sulfide at room temperature, mixing and stirring uniformly, reacting at 150 ℃ for 10 hours, centrifuging and washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
Example 9
Adding 80mg of graphene oxide into 250mL of deionized water, ultrasonically mixing and stirring uniformly, adding 150mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 120 ℃ for 3 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.5g of ferric chloride, 0.3g of cobalt nitrate and 0.7g of trisodium trithiocyanate at room temperature, mixing and stirring uniformly, reacting for 5 hours at 200 ℃, centrifugally washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
Example 10
Adding 100mg of graphene oxide into 250mL of deionized water, ultrasonically mixing and stirring uniformly, adding 10mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 120 ℃ for 3 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.2g of ferric nitrate, 0.8g of nickel nitrate and 0.5g of thiourea at room temperature, mixing and stirring uniformly, reacting at 200 ℃ for 5 hours, centrifuging and washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
Example 11
Adding 10mg of graphene oxide into 80mL of deionized water, ultrasonically mixing and stirring uniformly, adding 200mg of polyethyleneimine into the solution, and ultrasonically mixing to form a uniform solution. The mixed solution was then transferred to a thermostatic water bath at 120 ℃ for 3 hours, and the resulting product was washed to neutrality by centrifugation. Dispersing the obtained polyethyleneimine/graphene composite material into 50mL of solution, adding 0.2g of cobalt chloride, 0.2g of cobalt nitrate and 0.3g of trisodium trithiocyanate at room temperature, mixing and stirring uniformly, reacting for 5 hours at 200 ℃, centrifugally washing the obtained product to be neutral, drying, and grinding to obtain the superfine cobalt sulfide/graphene two-dimensional composite material.
Claims (6)
1. The preparation method of the superfine sulfide/graphene two-dimensional composite material is characterized by comprising the following steps:
step 1, adding graphene oxide and a bridging agent into water, and uniformly stirring to form a mixed solution;
step 2, reacting the mixed solution obtained in the step 1 at 60-120 ℃, and washing an obtained product to obtain a functionalized graphene material;
step 3, dispersing the functionalized graphene material in the step 2 into water, adding soluble metal salt and a sulfur source, and uniformly mixing and stirring to obtain a mixed solution;
step 4, reacting the mixed solution obtained in the step 3 at 100-200 ℃, and centrifugally washing, drying and grinding the obtained product to obtain the superfine sulfide/graphene composite material;
in the step 1, the bridging agent is polyethyleneimine;
in the step 3, the soluble metal salt is selected from one or two of cobalt nitrate, nickel nitrate, cobalt chloride, nickel chloride, ferric nitrate and ferric chloride;
in the step 3, the sulfur source is one of trisodium trithiocyanate, thiourea and sodium sulfide.
2. The method for preparing the superfine sulfide/graphene two-dimensional composite material according to claim 1, wherein in the step 1, the mass ratio of graphene oxide to the bridging agent is (10-100): (10-200).
3. The method for preparing the superfine sulfide/graphene two-dimensional composite material according to claim 1, wherein in the step 2, the reaction time is 3-48 hours.
4. The method for preparing the superfine sulfide/graphene two-dimensional composite material according to claim 1, wherein in the step 4, the reaction time is 5-24 hours.
5. The superfine sulfide/graphene two-dimensional composite material prepared by the preparation method of any one of claims 1 to 4, wherein the diameter of sulfide is 5-10 nm.
6. The application of the superfine sulfide/graphene two-dimensional composite material of claim 5 in the aspect of electrode materials of supercapacitors.
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| CN110828191B (en) * | 2019-09-27 | 2020-11-10 | 西安交通大学 | Carbon nitride/graphene/nickel disulfide supercapacitor material with porous layered structure and preparation method thereof |
| CN111463018B (en) * | 2020-04-08 | 2021-07-09 | 桂林理工大学 | Titanium tricarboxide/molybdenum disulfide composite film and preparation method and application thereof |
| CN113996278B (en) * | 2021-09-30 | 2023-09-05 | 黑龙江大学 | Molybdenum nickel sulfide/graphene complex and preparation method thereof |
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