CN108615609B - A kind of preparation method of the graphene/carbon nano-tube two-dimensional layer combination electrode material for supercapacitor - Google Patents
A kind of preparation method of the graphene/carbon nano-tube two-dimensional layer combination electrode material for supercapacitor Download PDFInfo
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- CN108615609B CN108615609B CN201810254816.5A CN201810254816A CN108615609B CN 108615609 B CN108615609 B CN 108615609B CN 201810254816 A CN201810254816 A CN 201810254816A CN 108615609 B CN108615609 B CN 108615609B
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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 methods of graphene/carbon nano-tube two-dimensional layer combination electrode material for supercapacitor, detailed process are as follows: the lamellar structure of graphene paper is opened by addition polymerization inhibitor ingredient nickel acetate and urea, thermal expansion and vacuum aided, 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 cellular structure abundant, 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 supercapacitor
Alkene/carbon nanotube two-dimensional layer combination electrode material preparation method.
Background technique
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 supercapacitor 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 the especially flexible energy storage device field of energy storage 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 performance of the methods of composite material and pore-creating raising 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 supercapacitor,
Need to be further increased.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of graphene/carbon nano-tube two-dimensional layers for supercapacitor
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 prospect.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of graphene for supercapacitor/
The preparation method of carbon nanotube two-dimensional layer combination electrode material, it is characterised in that: pass through addition polymerization inhibitor ingredient nickel acetate and urine
Element, thermal expansion and vacuum aided open the lamellar structure of graphene paper, then through vapor deposition 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 supercapacitor
Preparation method, it is characterised in that specific steps are as follows: graphite oxide is prepared with Hummer ' s method, disperses steaming for graphite oxide
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 with the heating rate of 15-30 DEG C/min in hydrogen-argon-mixed
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 and carbon nanotube deposition step 3 times, is cooled to room temperature repeatedly to 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 supercapacitor.
Further preferably, the graphene oxide base class paper material is 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.
Compared with the prior art, the invention has the following beneficial effects: 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 by thermal expansion and vacuum aided
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 cellular structure abundant, 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.
Detailed description of the invention
Fig. 1 is the SEM figure 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 embodiment
Combined with specific embodiments below, 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 method, disperses graphite oxide in distilled water and is configured to 10mL, 2mg/
The graphene oxide dispersion of mL and the nickel acetate solution and 20mg urea that 10mL, 7.5mg/mL is added persistently stir to get
The dispersion liquid is filtered by vacuum and obtains graphene oxide base class paper material, the graphite oxide in 70 DEG C of dry 12h by even dispersion liquid
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 and be evacuated to air pressure be -0.1Mpa, the rate for using peristaltic pump using 2mL/min be continuously added into ethyl alcohol as carbon source progress carbon
Nanotube deposition 5min, vacuumizes and carbon nanotube deposition step 3 times repeatedly, is cooled to room temperature to temperature and takes out sample and with dilute
Hydrochloric acid solution and distilled water clean repeatedly, and gained sample obtains stone of the final product for supercapacitor in 70 DEG C of dry 12h
Black alkene/carbon nanotube two-dimensional layer combination electrode material.
Fig. 1 is the SEM figure that combination electrode material (C and D) is made in pure graphene paper (A and B) and embodiment 1, 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
Brunauer-Emmett-Teller method carries out the ratio that pure graphene paper sample is calculated to the nitrogen adsorption desorption curve of sample
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 supercapacitor charge-discharge performance of different samples is characterized by constant current charge-discharge test.Use bipolar electrode body
System, the KOH solution of 6mol/L are that electrolyte is tested.It is pushed firstly, sample is cut into pressure of the suitable dimension in 10MPa
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.It can be carried out test using electrochemistry of the constant current charge-discharge to supercapacitor.Embodiment 1 is made sample and shows preferably
Charge-discharge performance, the charge and discharge time is much larger than pure graphene paper sample under identical current density, by carrying out to its capacitor
Embodiment 1 is calculated sample capacity under the current density of 0.5A/g is made and has reached 164.4F/g, capacitor with higher
Capacity.
Embodiment 2
Graphite oxide is prepared with Hummer ' s method, disperses graphite oxide in distilled water and is configured to 10mL, 2mg/
Simultaneously 10mL, 7.5mg/mL nickel acetate solution and 40mg urea is added in the graphene oxide dispersion of mL, persistently stirs to get uniformly
The dispersion liquid is filtered by vacuum and obtains graphene oxide base class paper material, the graphene oxide in 70 DEG C of dry 12h by dispersion liquid
Base 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
And being evacuated to air pressure is -0.1Mpa, the rate for using peristaltic pump using 2mL/min is continuously added into ethyl alcohol and receives as carbon source progress carbon
Nanotube deposition 5min, vacuumizes and carbon nanotube deposition step 3 times repeatedly, is cooled to room temperature to temperature and takes out sample and with dilute salt
Acid solution and distilled water clean repeatedly, and gained sample obtains graphite of the final product for supercapacitor in 70 DEG C of dry 12h
Alkene/carbon nanotube two-dimensional layer combination electrode material.
Embodiment 3
Graphite oxide is prepared with Hummer ' s method, disperses graphite oxide in distilled water and is configured to 10mL, 2mg/
Simultaneously 10mL, 7.5mg/mL nickel acetate solution and 20mg urea is added in the graphene oxide dispersion of mL, persistently stirs to get uniformly
The dispersion liquid is filtered by vacuum and obtains graphene oxide base class paper material, the graphene oxide in 70 DEG C of dry 12h by dispersion liquid
Base class paper material hydrogen volume percentage composition be 5% it is hydrogen-argon-mixed in the heating rate of 15 DEG C/min be warming up to 500 DEG C
And being evacuated to air pressure is -0.1Mpa, the rate for using peristaltic pump using 0.5mL/min is continuously added into ethyl alcohol as carbon source and carries out carbon
Nanotube deposition 5min, vacuumizes and carbon nanotube deposition step 3 times repeatedly, is cooled to room temperature to temperature and takes out sample and with dilute
Hydrochloric acid solution and distilled water clean repeatedly, and gained sample obtains stone of the final product for supercapacitor in 70 DEG C of dry 12h
Black alkene/carbon nanotube two-dimensional layer combination electrode material.
Embodiment 4
Graphite oxide is prepared with Hummer ' s method, disperses graphite oxide in distilled water and is configured to 10mL, 2mg/
Simultaneously 10mL, 7.5mg/mL nickel acetate solution and 20mg urea is added in the graphene oxide dispersion of mL, persistently stirs to get uniformly
The dispersion liquid is filtered by vacuum and obtains graphene oxide base class paper material, the graphene oxide in 70 DEG C of dry 12h by dispersion liquid
Base class paper material hydrogen volume percentage composition be 5% it is hydrogen-argon-mixed in the heating rate of 30 DEG C/min be warming up to 700 DEG C
And being evacuated to air pressure is -0.1Mpa, the rate for using peristaltic pump using 3mL/min is continuously added into ethyl alcohol and receives as carbon source progress carbon
Nanotube deposition 5min, vacuumizes and carbon nanotube deposition step 3 times repeatedly, is cooled to room temperature to temperature and takes out sample and with dilute salt
Acid solution and distilled water clean repeatedly, and gained sample obtains graphite of the final product for supercapacitor in 70 DEG C of dry 12h
Alkene/carbon nanotube two-dimensional layer combination electrode material.
Embodiment above describes basic principles and main features of the invention and advantage, 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 originals of the 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 (4)
1. a kind of preparation method of the graphene/carbon nano-tube two-dimensional layer combination electrode material for supercapacitor, special
Sign is: the lamellar structure of graphene paper opened by addition polymerization inhibitor ingredient nickel acetate and urea, thermal expansion and vacuum aided,
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;Specific steps are as follows: graphite oxide is prepared with Hummer ' s method, disperses graphite oxide in distilled water and is configured to
The graphene oxide dispersion of 10mL, 2mg/mL and the nickel acetate solution and 20-40mg urea that 10mL, 7.5mg/mL is added, hold
It is continuous to stir to get uniform dispersion, which is filtered by vacuum and obtains graphene oxide base class paper wood in 70 DEG C of dry 12h
Material, the graphene oxide base class paper material are warming up to 500-700 DEG C with the heating rate of 15-30 DEG C/min in hydrogen-argon-mixed
And being evacuated to air pressure is -0.1Mpa, the rate for using peristaltic pump using 0.5-3mL/min is continuously added into ethyl alcohol and carries out as carbon source
Carbon nanotube deposits 5min, vacuumizes repeatedly and carbon nanotube deposition step 3 times, is cooled to room temperature to temperature and takes out sample and be used in combination
Dilute hydrochloric acid solution and distilled water clean repeatedly, and gained sample obtains final product for supercapacitor in 70 DEG C of dry 12h
Graphene/carbon nano-tube two-dimensional layer combination electrode material.
2. the graphene/carbon nano-tube two-dimensional layer combination electrode material according to claim 1 for supercapacitor
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.
3. the graphene/carbon nano-tube two-dimensional layer combination electrode material according to claim 1 for supercapacitor
Preparation method, it is characterised in that: the volumn concentration of the hydrogen-argon-mixed middle hydrogen be 5%.
4. the graphene/carbon nano-tube two-dimensional layer combination electrode material according to claim 1 for supercapacitor
Preparation method, it is characterised in that: the adding rate of the ethyl alcohol be 2mL/min.
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CN106082198A (en) * | 2016-06-20 | 2016-11-09 | 山东欧铂新材料有限公司 | A kind of preparation method of Graphene |
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CN107141430A (en) * | 2017-06-27 | 2017-09-08 | 天津工业大学 | The preparation method of graphene-based Synergistic phase-change material |
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