CN108615609A - A kind of preparation method of graphene/carbon nano-tube two-dimensional layer combination electrode material for ultracapacitor - Google Patents
A kind of preparation method of graphene/carbon nano-tube two-dimensional layer combination electrode material for ultracapacitor Download PDFInfo
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- CN108615609A CN108615609A CN201810254816.5A CN201810254816A CN108615609A CN 108615609 A CN108615609 A CN 108615609A CN 201810254816 A CN201810254816 A CN 201810254816A CN 108615609 A CN108615609 A CN 108615609A
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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
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/38—Carbon pastes or blends; Binders or additives therein
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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 invention discloses a kind of preparation method of the graphene/carbon nano-tube two-dimensional layer combination electrode material for ultracapacitor, detailed process is：Ingredient nickel acetate and urea, thermal expansion and vacuum aided are inhibited by addition to open the lamellar structure of graphene paper, then graphene/carbon nano-tube two-dimensional layer combination electrode material is obtained by the deposition of carbon nanotubes in open interlayer structure that is vapor-deposited.Combination electrode material produced by the present invention has very high specific surface area and abundant pore passage structure, and three-dimensional conductive network structure is built into interlayer support by carbon nanotube, this novel graphene-based stratiform two-dimensional structure shows very high capacitive property, is a kind of outstanding electrode material for super capacitor.
Description
Technical field
The invention belongs to electrode material for super capacitor technical fields, and in particular to a kind of graphite for ultracapacitor
The preparation method of alkene/carbon nanotube two-dimensional layer combination electrode material.
Background technology
Graphene is a kind of material with unique two-dimension plane structure, it is connected in by single layer of carbon atom with sp2 hydridization
It forms together, unique structure imparts the excellent performance of graphene, it has good conductive capability, excellent mechanical property
Energy, the higher coefficient of heat conduction and very high specific surface area.Therefore, graphene has very strong answer in ultracapacitor field
Use potentiality.
Graphene is a kind of excellent structural unit, by that can obtain one-dimensional, two-dimentional and three-dimensional knot to the induction of its structure
Structure material, and show unique architectural characteristic.Graphene paper is the two-dimensional structure induced by graphene-structured, it has
Preferable mechanical property and flexibility characteristics have very strong application potential in energy storage field especially flexible energy storage device field.
However graphene paper lamella during preparation have occurred it is serious stack again, cause the specific surface area of material very low, together
When its remaining oxygen-containing functional group reduce the conductive capability of graphene paper, greatly limit the application of graphene paper.
The graphene paper electrode material for super capacitor of various documents and patent report mainly uses addition both at home and abroad at present
The methods of composite material and pore-creating improve the performance of graphene paper.Such as application No. is the patents of CN201510465231.4 to use
The method of thermo-contact constructs nano pore structure in graphene paper material, substantially increases the specific surface area of material.Application
Number for CN201410088987.7 patent report in graphene paper composition metal nano particle, significantly improve material
Conductive capability.But electrode material made from the above method is still not ideal enough for its chemical property in ultracapacitor,
Need to be further increased.
Invention content
The technical problem to be solved by the present invention is to provide a kind of graphene/carbon nano-tube two-dimensional layers for ultracapacitor
The preparation method of shape combination electrode material, graphene/carbon nano-tube two-dimensional layer combination electrode material made from this method have
The features such as specific surface area height and strong conductive capability, shows excellent performance in electrochemical property test, has wide answer
Use foreground.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of graphene for ultracapacitor/
The preparation method of carbon nanotube two-dimensional layer combination electrode material, it is characterised in that：Ingredient nickel acetate and urine are inhibited by addition
Element, thermal expansion and vacuum aided open the lamellar structure of graphene paper, then by being vapor-deposited in open interlayer structure
Deposition of carbon nanotubes obtains graphene/carbon nano-tube two-dimensional layer combination electrode material.
Further preferably, the graphene/carbon nano-tube two-dimensional layer combination electrode material for ultracapacitor
Preparation method, it is characterised in that the specific steps are：Graphite oxide is prepared with Hummer ' s methods, graphite oxide is scattered in steaming
It is configured to the graphene oxide dispersion of 10mL, 2mg/mL in distilled water and the nickel acetate solution and 20- of 10mL, 7.5mg/mL is added
40mg urea, persistently stirs to get uniform dispersion, which is filtered by vacuum and obtains graphite oxide in 70 DEG C of dry 12h
Alkenyl class paper material, the graphene oxide base class paper material are heated up in hydrogen-argon-mixed with the heating rate of 15-30 DEG C/min
To 500-700 DEG C and air pressure is evacuated to as -0.1Mpa, and ethyl alcohol is continuously added into the rate of 0.5-3mL/min using peristaltic pump
Carbon nanotube is carried out as carbon source and deposits 5min, is vacuumized repeatedly and carbon nanotube deposition step 3 times, waits for that temperature is cooled to room temperature
It takes out sample and is cleaned repeatedly with dilute hydrochloric acid solution and distilled water, gained sample obtains final product in 70 DEG C of dry 12h and is used for
The graphene/carbon nano-tube two-dimensional layer combination electrode material of ultracapacitor.
Further preferably, the graphene oxide base class paper material in hydrogen-argon-mixed with the heating rate of 20 DEG C/min
It is warming up to 600 DEG C.
Further preferably, the volumn concentration of the hydrogen-argon-mixed middle hydrogen is 5%.
Further preferably, the adding rate of the ethyl alcohol is 2mL/min.
The present invention has the advantages that compared with prior art：The present invention by structure design by graphene oxide,
Nickel acetate and urea mix and filter to obtain composite graphite alkene paper, will be in composite graphite alkene paper with vacuum aided by thermally expanding
Lamellar structure is opened, and in open graphene paper interlayer structure be deposited carbon nanotube and obtained unique graphene/carbon and receive
Mitron two dimension composite construction, the structure have very high specific surface area and abundant pore passage structure, and by carbon nanotube in interlayer
Support is built into three-dimensional conductive network structure, and this novel graphene-based stratiform two-dimensional structure shows very high capacitive character
Can, it is a kind of outstanding electrode material for super capacitor.
Description of the drawings
Fig. 1 is the SEM figures that combination electrode material is made in pure graphene paper and embodiment 1；
Fig. 2 is the nitrogen adsorption desorption curve that combination electrode material is made in pure graphene paper and embodiment 1；
Fig. 3 is the constant current charge-discharge curve that combination electrode material is made in pure graphene paper and embodiment 1.
Specific implementation mode
With reference to specific embodiment, the invention will be further described, but simultaneously the invention is not limited in any way
Content.
Embodiment 1
Graphite oxide is prepared with Hummer ' s methods, graphite oxide is scattered in distilled water and is configured to 10mL, 2mg/mL
Graphene oxide dispersion and the nickel acetate solution and 20mg urea that 10mL, 7.5mg/mL is added persistently stir to get and uniformly divide
The dispersion liquid is filtered by vacuum and obtains graphene oxide base class paper material in 70 DEG C of dry 12h by dispersion liquid, the graphite oxide alkenyl
Class paper material hydrogen volume percentage composition be 5% it is hydrogen-argon-mixed in the heating rate of 20 DEG C/min be warming up to 600 DEG C simultaneously
It is -0.1Mpa to be evacuated to air pressure, and the rate using peristaltic pump using 2mL/min is continuously added into ethyl alcohol and carries out carbon nanometer as carbon source
Pipe deposits 5min, vacuumizes repeatedly and carbon nanotube deposition step 3 times, waits for that temperature is cooled to room temperature and takes out sample and use dilute hydrochloric acid
Solution and distilled water clean repeatedly, gained sample in 70 DEG C of dry 12h obtain final product for ultracapacitor graphene/
Carbon nanotube two-dimensional layer combination electrode material.
Fig. 1 is pure graphene paper（A and B）And combination electrode material is made in embodiment 1（C and D）SEM figure, can from Fig. 1
There is more regular, consolidation lamella arrangements structure without sample obtained by composite urea and nickel acetate to find out, without carbon nanometer
Pipe occurs, and the graphene sheet layer arrangement after urea and nickel acetate are compound in sample is loose, and deposited largely in interlayer
Carbon nanotube.
Fig. 2 is the nitrogen adsorption desorption curve that combination electrode material is made in pure graphene paper and embodiment 1, is used
The ratio that Brunauer-Emmett-Teller methods to the nitrogen adsorption desorption curve of sample carry out that pure graphene paper sample is calculated
Surface area is 3.2m2/ g, and the specific surface area that sample is made in embodiment 1 is promoted to 262.1m2/ g, higher specific surface office assign
Embodiment 1 is made the more energy storage active sites of sample.
The ultracapacitor charge-discharge performance of different samples is characterized by constant current charge-discharge test.Use bipolar electrode body
The KOH solution of system, 6mol/L is that electrolyte is tested.First, sample pressure of the suitable dimension in 10MPa is cut into push
Pole piece is made on circular metal nickel screen.It assembles two panels pole piece and diaphragm electrolyte to obtain bipolar electrode super capacitor in a mold
Device.The chemical property of ultracapacitor is tested using constant current charge-discharge.Embodiment 1 is made sample and shows preferably
Charge-discharge performance, under identical current density the charge and discharge time be much larger than pure graphene paper sample, by its capacitance carry out
Embodiment 1 is calculated sample capacity under the current density of 0.5A/g is made and reached 164.4F/g, there is higher capacitance
Capacity.
Embodiment 2
Graphite oxide is prepared with Hummer ' s methods, graphite oxide is scattered in distilled water and is configured to 10mL, 2mg/mL
Simultaneously 10mL, 7.5mg/mL nickel acetate solution and 40mg urea is added in graphene oxide dispersion, persistently stirs to get evenly dispersed
The dispersion liquid is filtered by vacuum and obtains graphene oxide base class paper material in 70 DEG C of dry 12h by liquid, the graphene oxide base class
Paper material hydrogen volume percentage composition be 5% it is hydrogen-argon-mixed in be warming up to 600 DEG C with the heating rate of 20 DEG C/min and take out
Vacuum to air pressure is -0.1Mpa, and the rate using peristaltic pump using 2mL/min is continuously added into ethyl alcohol and carries out carbon nanotube as carbon source
5min is deposited, is vacuumized repeatedly and carbon nanotube deposition step 3 times, waits for that temperature is cooled to room temperature and takes out sample and molten with dilute hydrochloric acid
Liquid and distilled water clean repeatedly, and gained sample obtains graphene/carbon of the final product for ultracapacitor in 70 DEG C of dry 12h
Nanotube two-dimensional layer combination electrode material.
Embodiment 3
Graphite oxide is prepared with Hummer ' s methods, graphite oxide is scattered in distilled water and is configured to 10mL, 2mg/mL
Simultaneously 10mL, 7.5mg/mL nickel acetate solution and 20mg urea is added in graphene oxide dispersion, persistently stirs to get evenly dispersed
The dispersion liquid is filtered by vacuum and obtains graphene oxide base class paper material in 70 DEG C of dry 12h by liquid, the graphene oxide base class
Paper material hydrogen volume percentage composition be 5% it is hydrogen-argon-mixed in be warming up to 500 DEG C with the heating rate of 15 DEG C/min and take out
Vacuum to air pressure is -0.1Mpa, and the rate using peristaltic pump using 0.5mL/min is continuously added into ethyl alcohol and carries out carbon nanometer as carbon source
Pipe deposits 5min, vacuumizes repeatedly and carbon nanotube deposition step 3 times, waits for that temperature is cooled to room temperature and takes out sample and use dilute hydrochloric acid
Solution and distilled water clean repeatedly, gained sample in 70 DEG C of dry 12h obtain final product for ultracapacitor graphene/
Carbon nanotube two-dimensional layer combination electrode material.
Embodiment 4
Graphite oxide is prepared with Hummer ' s methods, graphite oxide is scattered in distilled water and is configured to 10mL, 2mg/mL
Simultaneously 10mL, 7.5mg/mL nickel acetate solution and 20mg urea is added in graphene oxide dispersion, persistently stirs to get evenly dispersed
The dispersion liquid is filtered by vacuum and obtains graphene oxide base class paper material in 70 DEG C of dry 12h by liquid, the graphene oxide base class
Paper material hydrogen volume percentage composition be 5% it is hydrogen-argon-mixed in be warming up to 700 DEG C with the heating rate of 30 DEG C/min and take out
Vacuum to air pressure is -0.1Mpa, and the rate using peristaltic pump using 3mL/min is continuously added into ethyl alcohol and carries out carbon nanotube as carbon source
5min is deposited, is vacuumized repeatedly and carbon nanotube deposition step 3 times, waits for that temperature is cooled to room temperature and takes out sample and molten with dilute hydrochloric acid
Liquid and distilled water clean repeatedly, and gained sample obtains graphene/carbon of the final product for ultracapacitor in 70 DEG C of dry 12h
Nanotube two-dimensional layer combination electrode material.
Embodiment above describes the basic principles and main features and advantage of the present invention, and the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the originals of the present invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (5)
1. a kind of preparation method of graphene/carbon nano-tube two-dimensional layer combination electrode material for ultracapacitor, special
Sign is：Ingredient nickel acetate and urea, thermal expansion and vacuum aided are inhibited by addition to open the lamellar structure of graphene paper,
Graphene/carbon nano-tube two-dimensional layer compound electric is obtained by the deposition of carbon nanotubes in open interlayer structure that is vapor-deposited again
Pole material.
2. the graphene/carbon nano-tube two-dimensional layer combination electrode material according to claim 1 for ultracapacitor
Preparation method, it is characterised in that the specific steps are：Graphite oxide is prepared with Hummer ' s methods, graphite oxide is scattered in
The graphene oxide dispersion of 10mL, 2mg/mL are configured in distilled water and be added 10mL, 7.5mg/mL nickel acetate solution and
20-40mg urea, persistently stirs to get uniform dispersion, which is filtered by vacuum and is aoxidized in 70 DEG C of dry 12h
Graphene base class paper material, the graphene oxide base class paper material is in hydrogen-argon-mixed with the heating rate of 15-30 DEG C/min
It is -0.1Mpa to be warming up to 500-700 DEG C and be evacuated to air pressure, is continuously added into the rate of 0.5-3mL/min using peristaltic pump
Ethyl alcohol carries out carbon nanotube as carbon source and deposits 5min, vacuumizes repeatedly and carbon nanotube deposition step 3 times, waits for that temperature is down to room
Sample is taken out after temperature and is cleaned repeatedly with dilute hydrochloric acid solution and distilled water, and gained sample obtains final product in 70 DEG C of dry 12h
Graphene/carbon nano-tube two-dimensional layer combination electrode material for ultracapacitor.
3. the graphene/carbon nano-tube two-dimensional layer combination electrode material according to claim 2 for ultracapacitor
Preparation method, it is characterised in that：The graphene oxide base class paper material is in hydrogen-argon-mixed with the heating of 20 DEG C/min
Rate is warming up to 600 DEG C.
4. the graphene/carbon nano-tube two-dimensional layer combination electrode material according to claim 2 for ultracapacitor
Preparation method, it is characterised in that：The volumn concentration of the hydrogen-argon-mixed middle hydrogen is 5%.
5. the graphene/carbon nano-tube two-dimensional layer combination electrode material according to claim 2 for ultracapacitor
Preparation method, it is characterised in that：The adding rate of the ethyl alcohol is 2mL/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109755025A (en) * | 2019-01-14 | 2019-05-14 | 清华大学 | A kind of electrode for capacitors, preparation method and capacitor |
| CN113818039A (en) * | 2021-09-29 | 2021-12-21 | 西安交通大学 | Three-dimensional carbon material/molybdenum diselenide electrocatalytic hydrogen evolution material and preparation method thereof |
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Cited By (3)
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| CN109755025A (en) * | 2019-01-14 | 2019-05-14 | 清华大学 | A kind of electrode for capacitors, preparation method and capacitor |
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| CN113818039A (en) * | 2021-09-29 | 2021-12-21 | 西安交通大学 | Three-dimensional carbon material/molybdenum diselenide electrocatalytic hydrogen evolution material and preparation method thereof |
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