CN104934233A - Porous conductive graphene/carbon nanohorn composite material, and preparation method and applications thereof - Google Patents
Porous conductive graphene/carbon nanohorn composite material, and preparation method and applications thereof Download PDFInfo
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- 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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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- H01G11/32—Carbon-based
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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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
- Y02E60/10—Energy storage using batteries
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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
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention provides a Porous conductive graphene/carbon nanohorn composite material. The composite material is characterized in that carbon nanohorn is distributed between graphene sheet layers or on the surfaces of the graphene sheet layers. The composite material effectively prevents or reduces lamination and agglomeration of the graphene sheet layers, a lot of hierarchical structural pores including micropores and meso pores are formed, and the specific surface area is large; and graphene plays a bridging role among the carbon nanohorns, a conductive network structure is formed, and the conductivity is enhanced. The invention also provides a preparation method and applications of the composite material, the material can be used as electrode material or additive in super capacitors, lithium ion batteries, fuel cells and the like, the electrode material is large in electric capacity and high in charging and discharging speed, and the circulation times are increased.
Description
Technical field
The present invention relates to a kind of porous, electrically conductive graphene/carbon nanometer angle composite material and preparation method thereof, belong to material, electrochemistry, energy storage, field of Environment Protection.
Background technology
In the past few decades, material with carbon element is due to itself good conductivity, specific area is large, chemistry and good mechanical stability, in fields such as electronics, chemical industry, machinery, environmental protection, especially in clean energy storage, as the aspects such as electrochemical energy storage (as lithium ion battery, ultracapacitor) attract wide attention.Wherein, the material with carbon element such as carbon fiber (CNFs), carbon nano-tube (CNTs), Graphene has broad application prospects at electrode or as in the important additives in high-performance electric chemistry energy storing device.Such as, although the theoretical specific surface area of Graphene and carbon nano-tube is very large, but, the reunion of Graphene, graphene film are stacked or carbon nano-tube bundle structure is piled up, reunite (interacted by the Van der Waals force of adjacent aspect and cause), greatly reduce specific area and the micropore volume of these material with carbon elements, the performance of its electrochemical energy storage (as lithium ion battery, ultracapacitor etc.) aspect is reduced.In addition, in practical application, the load capacity of Graphene is low, and stability etc. also exist more problem.According to the literature, in order to reduce, graphene film is stacked, agglomeration, and researcher develops Graphene or graphene sol, the gel of fold, and its electric capacity reaches 180F/g; Be supported on graphene film interlayer by carbon nano-tube or carbon nano-tube is inserted between graphene sheet layer, the capacitance up to 187F/g can be obtained.Also have bibliographical information, the metal of fake capacitance performance will be had and metal oxide embeds graphene film interlayer, can stop graphene sheet layer stacked, increase its specific area and pore volume, reach the object improving its capacitance.But, not only there is unstable properties, cycle-index is low, useful life is short shortcoming, also there is poisonous and problem that is environmental pollution aspect in the capacitor containing metal and metal oxide.According to another bibliographical information, adopt chemicals dispersed graphite alkene and carbon nano-tube and adopt chemicals (as hydrazine hydrate) redox graphene, not only synthesize cost high, also there is toxicity and problem of environmental pollution.
Summary of the invention
The present invention is intended to the foregoing problems solving prior art, provides simple, the eco-friendly production technology of a kind of method and technology, and synthesis has the conductive graphene/carbon nanohorn sandwich of porous.The feature of described composite material is that carbon nanohorn is distributed in graphene film interlayer or graphene sheet layer on the surface, effectively stops the stacked of graphene sheet layer and reunites, forms a large amount of hierarchical structure hole (comprise micropore and mesoporous) and bigger serface; Meanwhile, Graphene plays bridging effect between carbon nanohorn, forms conductive network structure, increases its conductivity.This material is for electrode material or electrochemical energy storing device such as ultracapacitor, lithium ion battery, fuel cells, and capacitance is large, charge/discharge rates is fast, recycles increased frequency.
The present invention is achieved through the following technical solutions:
Have conductive graphene/carbon nanohorn composite material of porous, it is characterized in that, described carbon nanohorn is distributed in graphene film interlayer and/or graphene sheet layer on the surface.
According to the present invention, described Graphene is selected from graphene oxide, redox graphene, Graphene or thin layer graphite.
According to the present invention, described carbon nanohorn is selected from carbon nanohorn, carbon nanohorn particle, carbon nanohorn micelle, carbon nanohorn assembly or carbon nanohorn, carbon nanohorn particle, carbon nanohorn micelle, carbon nanohorn assembly containing nano-pore; Described carbon nanohorn is single angle or multi-wall carbon nano-tube angle, preferred single angle.
According to the present invention, the mass ratio of described Graphene and carbon nanohorn is 20:1-1:1, preferred 5:1-5:2.
According to the present invention, the porosity (pore volume) of described composite material is for being greater than 0.08cm
3/ g, is preferably greater than 0.1cm
3/ g.
According to the present invention, described composite material has hierarchical pore structure, described pore structure preferred microporous and mesoporous.
Described mesoporous aperture, at 2-50nm, preferably at 2-20nm, is more preferably 2-5nm.
According to the present invention, the aperture of described micropore at 0.4-2nm, between preferred 0.5-1nm.
According to the present invention, described composite material is similar gels structure or loose structure.
According to the present invention, the specific area of described composite material is greater than 100m
2/ g, is preferably greater than 180m
2/ g.
According to the present invention, described composite material is conductive network structure.
The present invention also provides a kind of preparation method of above-mentioned composite material, it is characterized in that, graphene oxide (or redox graphene or Graphene or thin layer graphite) and single angle (or through single angle of red fuming nitric acid (RFNA) process) are first dispersed in solvent or water, again by hydro-thermal reaction, synthesizing graphite alkene/single angle composite material.
According to the present invention, described solvent is selected from organic solvent, acid, water, and composition thereof, preferred acid, water, and mixed liquor.
According to the present invention, described organic solvent is selected from toluene, phenol or dimethylbenzene.
According to the present invention, described acid-soluble dose is selected from red fuming nitric acid (RFNA).Preferably, first with red fuming nitric acid (RFNA), single angle is processed.
According to the present invention, ultrasonic wave dispersion or dispersed with stirring process are carried out to the material be dispersed in solvent or water.Preferably, the graphene oxide after process and single dihedral uniformly colloid or suspended matter.
The present invention also provides the application of above-mentioned composite material, it is characterized in that, described employing is used for electrode material or the additive applications as ultracapacitor, lithium ion battery, fuel cell etc. such as ultracapacitor, lithium ion battery, fuel cell.The capacitance of this material is large, charge/discharge rates fast, recycles increased frequency.
Because current Graphene (or synthesizing graphite alkene) is two layers or more Rotating fields, thus single angle or single angle particle, single angle micelle, single angle aggregation be distributed in graphene oxide (or Graphene) interlayer or its on the surface, effective prevention or reduce that it is stacked, reunite, makes that its specific area is large, voidage (pore volume) is high.Because Graphene and single angle close contact form the network configuration of conduction, this composite material has porousness and high conduction performance.The porous, electrically conductive Graphene synthesized by this technical scheme/single angle composite material, be suitable for the adsorption-desorption of ion, ion rapid diffusion and migration, the rapid diffusion of electrolyte and migration, thus improve its chemical property, can be applied in well in the energy storage devices such as high-performance super capacitor, lithium ion battery, fuel cell.The nano carbon composite material of this technology synthesis does not add poisonous and harmful chemical reagent in containing metal, nano metal or metal oxide, building-up process yet, is therefore a nontoxic environmentally friendly technology and technology.
Accompanying drawing illustrates:
Fig. 1. ESEM (SEM) figure of Graphene/single angle composite material
Fig. 2. the 77K nitrogen adsorption isotherm of Graphene/single angle composite material
Fig. 3. electrochemistry cyclic voltammetry curve (CV) curve that Graphene/single angle composite material records in 1M KOH solution.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.But those skilled in the art understand, and protection scope of the present invention is not limited only to following examples.According to content disclosed by the invention, those skilled in the art will recognize that when the technical characteristic do not departed from given by technical solution of the present invention and scope, to the above embodiment make many changes and amendment all belong to protection scope of the present invention.
Embodiment 1
50mg single angle (Single wall carbon nanohorns) is added in 50mL red fuming nitric acid (RFNA), at 60 DEG C of temperature, stir process is after 12 hours, be separated, wash with water, be separated again, wash with water again, after repeating 2,3 times or more time, stand-by after dry in 70 DEG C of baking ovens.
Get out graphene oxide (or powdered graphite or graphite oxide first synthesize graphene oxide) in advance or redox graphene stand-by.
By above-mentioned ready 50mg graphene oxide and 10mg single angle, namely press the weight ratio of 5:1, be dispersed in 30mL water, ultrasonic wave dispersion treatment 3 hours, make graphene oxide and single angle in water, form uniform colloid or suspended matter.Again this colloidal solution or suspension are proceeded in hydrothermal reactor, at 180 DEG C of temperature, carry out hydro-thermal reaction 18 hours.After reaction terminates, naturally cool to room temperature.The product of the similar water gel (hydrogel) reaction generated is immersed in water, and after 5 minutes, suck moisture, soak the product of this similar gels again, repeat several times, the product of this similar gels is at room temperature placed a whole night, allows its natural drying, obtain the reaction product-Graphene/single angle composite material of similar gels (frozen glue).Finally, it to be flowed down in tube furnace with the programming rate of 5 DEG C per minute at nitrogen (or argon gas), is heated to 800 DEG C, and keeps 2 hours, namely obtain porous, electrically conductive Graphene/single angle composite material.
We are by the porous, electrically conductive Graphene/single angle composite material of water heat transfer, by a series of structural characterization and Electrochemical Properties, result shows, this composite material has about 0.6nm micropore and the mesoporous similar gels structure of about 2-12nm or loose structure, and its nano-pore volume is about 0.2cm
3/ g.Under room temperature, in 1M KOH solution, under fast charging and discharging, record the electric capacity of the Graphene/single angle composite material of synthesis up to 244F/g, and this composite material has good high rate performance, its chemical property particularly electrochemical energy storage performance is better than the composite material at graphene oxide, redox graphene, single angle and other single angle.Constant current charge-discharge is carried out under the current density of 10A/g, circulate can also keep for 1000 times 99% capacitance, therefore, have broad application prospects in the application such as energy storage device (as ultracapacitor), lithium ion battery, fuel cell of high-energy-density.
Embodiment 2
50mg single angle (Single wall carbon nanohorns) is added in 50mL red fuming nitric acid (RFNA), at 60 DEG C of temperature, stir process is after 12 hours, be separated, wash with water, be separated again, wash with water again, after repeating 2,3 times or more time, stand-by after dry in 70 DEG C of baking ovens.
Get out graphene oxide (or powdered graphite or graphite oxide first synthesize graphene oxide) in advance or redox graphene stand-by.
By above-mentioned ready 50mg graphene oxide and 20mg single angle, namely press the weight ratio of 2.5:1, be dispersed in 30mL water, ultrasonic wave dispersion treatment 3 hours, make graphene oxide and single angle in water, form uniform colloid or suspended matter.Again this colloidal solution or suspension are proceeded in hydrothermal reactor, at 180 DEG C of temperature, carry out hydro-thermal reaction 18 hours.After reaction terminates, naturally cool to room temperature.The product of the similar water gel (hydrogel) reaction generated is immersed in water, and after 5 minutes, suck moisture, soak the reaction product of this similar hydrogel again, repeat several times, this reaction product is at room temperature placed a whole night, allows its natural drying, obtain the Graphene/single angle composite material of similar gels (frozen glue).Finally, it to be flowed down in tube furnace with the programming rate of 5 DEG C per minute at nitrogen (or argon gas), is heated to 800 DEG C, and keeps 2 hours, namely obtain porous, electrically conductive Graphene/single angle composite material.
We are by the porous, electrically conductive Graphene/single angle composite material of water heat transfer, by a series of structural characterization and Electrochemical Properties, result shows, under room temperature, in 1M KOH solution, under fast charging and discharging, the composite material recording the capacitance ratio 1 of the Graphene/single angle composite wood of synthesis is low, be about 133F/g, this composite material has good high rate performance, and its chemical property such as electrochemical energy storage performance is better than the composite material at graphene oxide, redox graphene, single angle and other single angle.
Embodiment 3
By 50mg graphene oxide (or powdered graphite or graphite oxide first synthesize graphene oxide) or redox graphene and 10-20mg single angle, namely the weight ratio of 5:1-2.5:1 is pressed, be dispersed in 30mL water, ultrasonic wave dispersion treatment, makes graphene oxide or redox graphene and single angle in water, form uniform colloid or suspended matter.Again this colloidal solution or suspension are proceeded in hydrothermal reactor, at 180 DEG C of temperature, carry out hydro-thermal reaction 18 hours.After reaction terminates, naturally cool to room temperature.The product of the similar water gel (hydrogel) reaction generated is immersed in water, and after 5 minutes, suck moisture, soak the reaction product of this similar hydrogel again, repeat several times, the product of similar water gel is at room temperature placed a whole night, allows its natural drying, obtain the Graphene/single angle composite material of similar gels (frozen glue).Finally, it to be flowed down in tube furnace with the programming rate of 5 DEG C per minute at nitrogen (or argon gas), is heated to 800 DEG C, and keeps 2 hours, namely obtain porous, electrically conductive Graphene/single angle composite material.
We are to the Graphene/single angle composite material of water heat transfer, by a series of structural characterization and Electrochemical Properties, result shows, under room temperature, in 1M KOH solution, under fast charging and discharging, the composite material recording the capacitance ratio 1 of the Graphene/single angle composite wood of synthesis is low, but this composite material has good high rate performance, its chemical property such as electrochemical energy storage performance is better than the composite material at graphene oxide, redox graphene, single angle and other single angle.
Claims (8)
1. have conductive graphene/carbon nanohorn composite material of porous, it is characterized in that, described carbon nanohorn is distributed in graphene film interlayer or graphene sheet layer on the surface.
2. composite material according to claim 1, wherein, described Graphene is selected from graphene oxide, redox graphene, Graphene, thin layer graphite or oxide thin layer graphite.
Preferably, described carbon nanohorn is selected from carbon nanohorn, carbon nanohorn particle, carbon nanohorn micelle, carbon nanohorn assembly or carbon nanohorn, carbon nanohorn particle, carbon nanohorn micelle, carbon nanohorn assembly containing nano-pore; Described carbon nanohorn is single angle or multi-wall carbon nano-tube angle, preferred single angle.
3. according to the composite material of claim 1 or 2, wherein, the mass ratio of described Graphene or graphene oxide and the carbon nanohorn carbon nanohorn of red fuming nitric acid (RFNA) process (or through) is 20:1-1:1, preferred 5:1-5:2.
4. according to the composite material of any one of claim 1-3, it is characterized in that, the porosity (pore volume) of described composite material is for being greater than 0.08cm
3/ g, is preferably greater than 0.1cm
3/ g.The specific area of described composite material is for being greater than 100m
2/ g, is preferably greater than 180m
2/ g.
Preferably, described composite material tape has levels structure hole, preferably includes micropore and mesoporous.
Described mesoporous aperture, at 2-50nm, preferably at 2-20nm, is more preferably 2-5nm.
More preferably, the aperture of described micropore at 0.4-2nm, between preferred 0.5-1nm.
Also more preferably, described composite material is similar gels structure or loose structure.Described composite material is conductive network structure.
5. the preparation method of the composite material described in an any one of claim 1-4, it is characterized in that, graphene oxide (or redox graphene or Graphene or thin layer graphite or oxide thin layer graphite) and single angle the carbon nanohorn of red fuming nitric acid (RFNA) process (or through) is first dispersed in solvent or water, again by hydro-thermal reaction, synthesizing graphite alkene/single angle composite material.
6. preparation method according to claim 5, is characterized in that, described solvent is selected from organic solvent, acid, water, and composition thereof, preferred acid, water, and composition thereof.
Preferably, described organic solvent is selected from toluene, phenol, dimethylbenzene.
Preferably, described acid-soluble dose is selected from red fuming nitric acid (RFNA).
7. according to the preparation method of claim 5 or 6, it is characterized in that, ultrasonic wave dispersion or dispersed with stirring process are carried out to the material be dispersed in solvent or water.
Preferably, the graphene oxide after process or redox graphene or Graphene and single the angle carbon nanohorn of red fuming nitric acid (RFNA) process (or through) form uniform colloid or suspended matter in solvent or water.
8. the application of the composite material described in any one of claim 1-4, is characterized in that, described application is used for the additive of the electrode material such as ultracapacitor, lithium ion battery, fuel cell or ultracapacitor, lithium ion battery, fuel cell.
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Cited By (15)
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| CN105185599A (en) * | 2015-10-16 | 2015-12-23 | 中国科学院福建物质结构研究所 | Super-capacitor carbon composite material, preparation method therefor, and application of super-capacitor carbon composite material |
| CN105552371A (en) * | 2016-01-20 | 2016-05-04 | 福州大学 | Preparation and application of nitrogen-doped graphene-carbon nanohorn composite material |
| CN105845914A (en) * | 2016-05-26 | 2016-08-10 | 江苏深苏电子科技有限公司 | Method for preparing lithium ion battery negative electrode composite material |
| CN106449129A (en) * | 2016-09-29 | 2017-02-22 | 成都新柯力化工科技有限公司 | Graphene self-assembled electrode material for super-capacitor and preparation method |
| CN107417910A (en) * | 2017-06-14 | 2017-12-01 | 福州大学 | The preparation method and application of carbon nanohorn/grapheme/polyaniline composite material |
| CN108538638A (en) * | 2018-03-28 | 2018-09-14 | 深圳新源柔性科技有限公司 | A kind of ultracapacitor preparation method and ultracapacitor |
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| CN113980311A (en) * | 2021-11-26 | 2022-01-28 | 江苏清大际光新材料有限公司 | Heat dissipation film containing carbon nanohorns, preparation method and application |
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