CN109243843A - A kind of ultra-fine sulfide/graphene Two-dimensional Composites and its preparation method and application - Google Patents
A kind of ultra-fine sulfide/graphene Two-dimensional Composites and its preparation method and application 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
- 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
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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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- 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 present invention provides a kind of ultra-fine sulfide/graphene Two-dimensional Composites and its preparation method and application, comprising the following steps: step 1, graphene oxide and bridging agent are added to the water, form mixed solution；Step 2, mixed solution is reacted at 60 DEG C -120 DEG C, functionalization graphene material is made；Step 3, the functionalization graphene material in step 2 is distributed in water, and soluble metallic salt and sulphur source is added, be mixed evenly；Step 4, gained mixed solution in step 3 is reacted at 100 DEG C -200 DEG C, resulting product centrifuge washing is dried, and ultra-fine sulfide/graphene composite material is made in grinding.Gained sulfide diameter is 5-10nm.Ultra-fine sulfide/the graphene composite material of gained can show stronger interaction between the two, and the more active sites of exposure, the electrode as supercapacitor have many advantages, such as height ratio capacity, high magnification, long circulation life.
Description
Technical field
The invention belongs to inorganic material preparation and technical field of new energy application, are related to a kind of ultra-fine sulfide/graphene
Two-dimensional Composites and its preparation method and application.
Background technique
With the fast development of electric car and portable electronic device, the research of energy stores and converting system is by pass
Note.Supercapacitor is played the part of more and more important due to having the characteristics that high power density and long circulation life in energy storage field
Role.Core of the electrode material as supercapacitor, determines the chemical property of supercapacitor to a certain extent.It crosses
Metal sulfide is crossed, because of its surface electrochemical site abundant and higher theoretical capacity, is widely used in super capacitor
The electrode material of device, but this kind of material often be faced with poorly conductive, it is easy to reunite the disadvantages of.By transient metal sulfide and two-dimentional stone
Black alkene combines and constructs composite material, and the electrode as supercapacitor has wide application potential.Usual transition metal vulcanization
Object can show diversified form, such as nanometer rods, nanometer sheet, nanotube, nano particle on two-dimensional graphene surface.
However, there are still problems for the direct combination of the two, on the one hand, graphene and sulfide species are incompatible in structure
Property, cause the interaction between each component undesirable, active material is easy to fall off after being recycled for multiple times, and then influences its electricity
Chemical property；On the other hand, graphene/sulfide composite material preparation method lacks the tune to active specy size at present
Control causes active sites exposure less, and whole chemical property is bad.
Summary of the invention
To solve problems of the prior art, the object of the present invention is to provide a kind of ultra-fine sulfide/graphenes two
Dimension composite material and preparation method and application, the ultra-fine sulfide/graphene composite material of gained can show between the two
Stronger interaction, and the more active sites of exposure, the electrode as supercapacitor have height ratio capacity, high magnification, length
The advantages that cycle life.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of ultra-fine sulfide/graphene Two-dimensional Composites, comprising the following steps:
Step 1, graphene oxide and bridging agent are added to the water, are stirred evenly, form mixed solution；
Step 2, the mixed solution in step 1 is reacted at 60 DEG C -120 DEG C, function fossil is made in products therefrom washing
Black alkene material；
Step 3, the functionalization graphene material in step 2 is distributed in water, and soluble metallic salt and sulphur source is added,
It is mixed evenly, obtains mixed solution；
Step 4, gained mixed solution in step 3 is reacted at 100 DEG C -200 DEG C, resulting product centrifuge washing dries
Dry, ultra-fine sulfide/graphene composite material is made in grinding.
Preferably, in step 1, bridging agent is one of polyaniline, polyethyleneimine and poly-dopamine.
Preferably, in step 1, the mass ratio of graphene oxide and bridging agent is (10-100): (10-200).
Preferably, in step 2, the reaction time is 3-48 hours.
Preferably, in step 3, the mass ratio of soluble metallic salt and sulphur source is (0.1-1.0): (0.1-1.0).
Preferably, in step 3, soluble metallic salt is selected from cobalt nitrate, nickel nitrate, cobalt chloride, nickel chloride, ferric nitrate and chlorine
Change one or both of iron.
Preferably, in step 3, sulphur source is one of trithiocyanuric acid trisodium salt, thiocarbamide and vulcanized sodium.
Preferably, in step 4, the reaction time is 5-24 hours.
A kind of ultra-fine sulfide/graphene Two-dimensional Composites that the preparation method is prepared, sulfide diameter are
5-10nm。
The ultra-fine sulfide/application of the graphene Two-dimensional Composites in terms of electrode material for super capacitor.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention uses bridging agent, graphene oxide is carried out functionalization, the functional group using bridging agent surface promotes sulphur
Compound nano particle is evenly dispersed on the surface of graphene, forms Two-dimensional Composites, and make sulfide nanoparticle and graphite
Stronger interaction is showed between alkene.Simultaneously because the restriction effect of bridging agent, prepared sulfide nanoparticle are in
Reveal lesser size, more active sites can be exposed, greatly promoted energy storage effect, therefore the target material have it is excellent
Chemical property, be used for that electrode material for super capacitor is high with specific capacity, multiplying power property is good, has extended cycle life etc. one
Number of advantages.In addition, it is the preparation method simple process, safe operation, low in cost, there is broad prospect of application.
Detailed description of the invention
Fig. 1 is the ultra-fine sulfide/graphene Two-dimensional Composites scanning electron microscope (SEM) photograph prepared；
Fig. 2 is ultra-fine sulfide/circulation of the graphene Two-dimensional Composites as electrode material for super capacitor prepared
Volt-ampere curve figure.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The preparation method of ultra-fine sulfide/graphene composite material of the present invention, comprising the following steps:
Step 1 adds graphene oxide into deionized water, and ultrasonic mixing stirs evenly, and is added into above-mentioned solution,
Ultrasonic mixing forms homogeneous solution, and bridging agent is one of polyaniline, polyethyleneimine, poly-dopamine.Graphene oxide is gone
The ratio of ionized water and bridging agent is (10-100) mg:(50-250) mL:(10-200) mg.
Mixed solution in step 1 is transferred in 60-120 DEG C of constant temperature oil bath or water-bath by step 2, keeps 3-48 small
When, by obtained product centrifuge washing to neutrality, functionalization graphene material is made.
Functionalization graphene material in step 2 is distributed in 20-100mL water by step 3, at room temperature will be soluble
Metal salt, sulphur source are according to mass ratio (0.1-1.0): (0.1-1.0) is added separately to the water-soluble of above-mentioned functionalization graphene material
In liquid, it is mixed evenly；The soluble metallic salt is selected from cobalt nitrate, nickel nitrate, ferric nitrate, iron chloride, cobalt chloride and chlorine
Change one or both of nickel, sulphur source is one of trithiocyanuric acid trisodium salt, thiocarbamide, vulcanized sodium.
Step 4, by step 3 gained mixed solution 100-200 DEG C reaction 5-24 hours, by obtained product be centrifuged wash
It washs to neutrality, dries, ultra-fine sulfide/graphene Two-dimensional Composites are made in grinding.
Wherein, the mass ratio of graphene oxide, bridging agent, soluble metallic salt and sulphur source is (10-100): (10-200):
(0.1-1.0): (0.1-1.0).
The particle size of sulfide is 5- in ultra-fine sulfide/graphene Two-dimensional Composites that the preparation method obtains
10nm can expose more active sites, can be used as electrode material for super capacitor use.
Embodiment 1
20mg graphene oxide is added in 100mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 30mg polyethyleneimine, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 80 DEG C of water bath with thermostatic control, is protected
It holds 12 hours, by obtained product centrifuge washing to neutrality.Obtained polyethyleneimine/graphene composite material is distributed to
In 50mL solution, 0.3g cobalt chloride, 0.5g trithiocyanuric acid trisodium salt are added at room temperature, is mixed evenly, it is anti-at 120 DEG C
It answers 18 hours, obtained product centrifuge washing to neutrality is dried, ultra-fine cobalt sulfide/graphene two dimension composite wood is made in grinding
Material.
It is characterized using scanning electron microscope to ultra-fine cobalt sulfide/graphene Two-dimensional Composites are made, characterization result such as Fig. 1
It is shown, it can be seen that ultra-fine vulcanization cobalt nano-particle may be uniformly dispersed in graphene surface, and cobalt sulfide nanoparticle size
It is smaller, diameter 5-10nm.
Embodiment 2
20mg graphene oxide is added in 100mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 30mg polyethyleneimine, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 80 DEG C of water bath with thermostatic control, is protected
It holds 12 hours, by obtained product centrifuge washing to neutrality.Obtained polyethyleneimine/graphene composite material is distributed to
In 50mL solution, 0.3g cobalt chloride, 0.5g trithiocyanuric acid trisodium salt are added at room temperature, is mixed evenly, it is anti-at 180 DEG C
It answers 12 hours, obtained product centrifuge washing to neutrality is dried, ultra-fine cobalt sulfide/graphene two dimension composite wood is made in grinding
Material.
Ultra-fine cobalt sulfide/graphene Two-dimensional Composites are tested as the electrode material of supercapacitor, and Fig. 2 is should
The cyclic voltammetry curve figure of electrode material, the results show that the electrode material shows excellent electricity compared to bright sulfur cobalt electrode
Hold characteristic.
Embodiment 3
50mg graphene oxide is added in 100mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 80mg polyethyleneimine, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 80 DEG C of water bath with thermostatic control, is protected
It holds 24 hours, by obtained product centrifuge washing to neutrality.Obtained polyethyleneimine/graphene composite material is distributed to
In 50mL solution, 0.3g cobalt nitrate, 0.5g trithiocyanuric acid trisodium salt are added at room temperature, is mixed evenly, it is anti-at 180 DEG C
It answers 12 hours, obtained product centrifuge washing to neutrality is dried, ultra-fine cobalt sulfide/graphene two dimension composite wood is made in grinding
Material.
Embodiment 4
50mg graphene oxide is added in 100mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 80mg polyethyleneimine, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 80 DEG C of water bath with thermostatic control, is protected
It holds 24 hours, by obtained product centrifuge washing to neutrality.Obtained polyethyleneimine/graphene composite material is distributed to
In 50mL solution, 0.3g cobalt nitrate, 1.0g trithiocyanuric acid trisodium salt are added at room temperature, is mixed evenly, it is anti-at 120 DEG C
It answers 24 hours, obtained product centrifuge washing to neutrality is dried, ultra-fine cobalt sulfide/graphene two dimension composite wood is made in grinding
Material.
Embodiment 5
50mg graphene oxide is added in 100mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 80mg polyethyleneimine, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 80 DEG C of water bath with thermostatic control, is protected
It holds 24 hours, by obtained product centrifuge washing to neutrality.Obtained polyethyleneimine/graphene composite material is distributed to
In 50mL solution, 0.1g cobalt chloride, 0.1g nickel chloride, 1.0g trithiocyanuric acid trisodium salt are added at room temperature, is mixed equal
It is even, it is reacted 24 hours at 120 DEG C, obtained product centrifuge washing to neutrality is dried, ultra-fine vulcanization nickel cobalt/stone is made in grinding
Black alkene Two-dimensional Composites.
Embodiment 6
30mg graphene oxide is added in 100mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 80mg polyethyleneimine, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 80 DEG C of water bath with thermostatic control, is protected
It holds 24 hours, by obtained product centrifuge washing to neutrality.Obtained polyethyleneimine/graphene composite material is distributed to
In 50mL solution, 0.2g cobalt chloride, 0.1g nickel chloride, 1.0g trithiocyanuric acid trisodium salt are added at room temperature, is mixed equal
It is even, it is reacted 12 hours at 180 DEG C, obtained product centrifuge washing to neutrality is dried, ultra-fine vulcanization nickel cobalt/stone is made in grinding
Black alkene Two-dimensional Composites.
Embodiment 7
10mg graphene oxide is added in 50mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 10mg polyaniline, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 60 DEG C of constant temperature oil bath, keeps 48
Hour, by obtained product centrifuge washing to neutrality.Obtained polyaniline/graphene composite material is distributed to 50mL solution
In, 0.1g nickel nitrate, 0.1g thiocarbamide are added at room temperature, is mixed evenly, is reacted 18 hours at 100 DEG C, the production that will be obtained
Object centrifuge washing is dried, ultra-fine cobalt sulfide/graphene Two-dimensional Composites are made in grinding to neutrality.
Embodiment 8
100mg graphene oxide is added in 200mL deionized water, ultrasonic mixing stirs evenly, into above-mentioned solution
30mg poly-dopamine is added, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 100 DEG C of constant temperature oil bath,
It is kept for 35 hours, by obtained product centrifuge washing to neutrality.Obtained poly-dopamine/graphene composite material is distributed to
In 50mL solution, 0.5g nickel chloride, 0.1g vulcanized sodium are added at room temperature, is mixed evenly, is reacted 10 hours at 150 DEG C,
It by obtained product centrifuge washing to neutrality, dries, ultra-fine cobalt sulfide/graphene Two-dimensional Composites are made in grinding.
Embodiment 9
80mg graphene oxide is added in 250mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 150mg polyethyleneimine, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 120 DEG C of water bath with thermostatic control,
It is kept for 3 hours, by obtained product centrifuge washing to neutrality.Obtained polyethyleneimine/graphene composite material is distributed to
In 50mL solution, 0.5g iron chloride, 0.3g cobalt nitrate, 0.7g trithiocyanuric acid trisodium salt are added at room temperature, is mixed equal
It is even, it is reacted 5 hours at 200 DEG C, obtained product centrifuge washing to neutrality is dried, ultra-fine cobalt sulfide/graphite is made in grinding
Alkene Two-dimensional Composites.
Embodiment 10
100mg graphene oxide is added in 250mL deionized water, ultrasonic mixing stirs evenly, into above-mentioned solution
10mg polyethyleneimine is added, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred to 120 DEG C of water bath with thermostatic control
In, it is kept for 3 hours, by obtained product centrifuge washing to neutrality.By obtained polyethyleneimine/graphene composite material dispersion
Into 50mL solution, 0.2g ferric nitrate, 0.8g nickel nitrate, 0.5g thiocarbamide are added at room temperature, is mixed evenly, at 200 DEG C
Obtained product centrifuge washing to neutrality is dried in reaction 5 hours, and it is compound that ultra-fine cobalt sulfide/graphene two dimension is made in grinding
Material.
Embodiment 11
10mg graphene oxide is added in 80mL deionized water, ultrasonic mixing stirs evenly, and adds into above-mentioned solution
Enter 200mg polyethyleneimine, ultrasonic mixing forms homogeneous solution.Then mixed solution is transferred in 120 DEG C of water bath with thermostatic control,
It is kept for 3 hours, by obtained product centrifuge washing to neutrality.Obtained polyethyleneimine/graphene composite material is distributed to
In 50mL solution, 0.2g cobalt chloride, 0.2g cobalt nitrate, 0.3g trithiocyanuric acid trisodium salt are added at room temperature, is mixed equal
It is even, it is reacted 5 hours at 200 DEG C, obtained product centrifuge washing to neutrality is dried, ultra-fine cobalt sulfide/graphite is made in grinding
Alkene Two-dimensional Composites.
Claims (10)
1. a kind of preparation method of ultra-fine sulfide/graphene Two-dimensional Composites, which comprises the following steps:
Step 1, graphene oxide and bridging agent are added to the water, are stirred evenly, form mixed solution；
Step 2, the mixed solution in step 1 is reacted at 60 DEG C -120 DEG C, functionalization graphene is made in products therefrom washing
Material；
Step 3, the functionalization graphene material in step 2 is distributed in water, and soluble metallic salt and sulphur source is added, mixed
It stirs evenly, obtains mixed solution；
Step 4, gained mixed solution in step 3 is reacted at 100 DEG C -200 DEG C, resulting product centrifuge washing, drying is ground
Mill, is made ultra-fine sulfide/graphene composite material.
2. the preparation method of ultra-fine sulfide/graphene Two-dimensional Composites according to claim 1, which is characterized in that
In step 1, bridging agent is one of polyaniline, polyethyleneimine and poly-dopamine.
3. the preparation method of ultra-fine sulfide/graphene Two-dimensional Composites according to claim 1, which is characterized in that
In step 1, the mass ratio of graphene oxide and bridging agent is (10-100): (10-200).
4. the preparation method of ultra-fine sulfide/graphene Two-dimensional Composites according to claim 1, which is characterized in that
In step 2, the reaction time is 3-48 hours.
5. the preparation method of ultra-fine sulfide/graphene Two-dimensional Composites according to claim 1 or 3, feature exist
In in step 3, the mass ratio of soluble metallic salt and sulphur source is (0.1-1.0): (0.1-1.0).
6. the preparation method of ultra-fine sulfide/graphene Two-dimensional Composites according to claim 1, which is characterized in that
In step 3, soluble metallic salt be selected from one of cobalt nitrate, nickel nitrate, cobalt chloride, nickel chloride, ferric nitrate and iron chloride or
Two kinds.
7. the preparation method of ultra-fine sulfide/graphene Two-dimensional Composites according to claim 1, which is characterized in that
In step 3, sulphur source is one of trithiocyanuric acid trisodium salt, thiocarbamide and vulcanized sodium.
8. the preparation method of ultra-fine sulfide/graphene Two-dimensional Composites according to claim 1, which is characterized in that
In step 4, the reaction time is 5-24 hours.
9. a kind of ultra-fine sulfide/graphene two dimension that the described in any item preparation methods of claim 1-8 are prepared is compound
Material, which is characterized in that sulfide diameter is 5-10nm.
10. a kind of ultra-fine sulfide/graphene Two-dimensional Composites as claimed in claim 9 are in electrode material for super capacitor side
The application in face.
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