CN108010734A - A kind of micro super capacitor production method based on graphene/carbon nano-tube aeroge - Google Patents
A kind of micro super capacitor production method based on graphene/carbon nano-tube aeroge Download PDFInfo
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- CN108010734A CN108010734A CN201810022749.4A CN201810022749A CN108010734A CN 108010734 A CN108010734 A CN 108010734A CN 201810022749 A CN201810022749 A CN 201810022749A CN 108010734 A CN108010734 A CN 108010734A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 43
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 43
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 42
- 239000003990 capacitor Substances 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 230000009467 reduction Effects 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002196 Pyroceram Substances 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 8
- 229910001882 dioxygen Inorganic materials 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002071 nanotube Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004964 aerogel Substances 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 241000446313 Lamella Species 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 238000000627 alternating current impedance spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000004758 underpotential deposition Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- 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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention relates to a kind of micro super capacitor production method based on graphene/carbon nano-tube aeroge, the mixed liquor of the graphene oxide configured and carbon nanotubes is injected into extruding device, three-dimensional micro-electrode is obtained by three-dimensionally shaped, by the reduction that is freeze-dried and anneals, obtain micro super capacitor product, carbon nanotubes, graphene oxide and deionized water in mass ratio 3 during making:1:15 are uniformly mixed.Manufacture craft of the present invention is easy and makes precision height, is adapted to large-scale production, and products obtained therefrom has the advantages that higher mechanical stability, light weight, specific capacity are high and cycle performance is excellent, has a good application prospect.
Description
Technical field
The present invention relates to the interleaving techniques field of nano material and increasing material manufacturing technique, and in particular to one kind is based on graphite
The micro super capacitor production method of alkene/carbon nanotube aerogel.
Background technology
Ultracapacitor, it is a kind of between battery and traditional capacitor to be that the seventies and eighties in 20th century grows up
New type of energy storage device, has the vast capacity of farad level, power 2000-6000 times bigger than the electrolytic capacitor capacity of same volume
Density ratio battery is 10-100 times high, while has long circulation life, it is considered to be a kind of new cleaning fuel efficiently, practical,
Currently as stand-by power supply, it is widely used in camera, video recorder, mobile phone, computer and other electronic products.As
A kind of ultracapacitor of small size, micro super capacitor not only possess ultracapacitor power density height, cyclical stability
The advantages of good, it is thus also avoided that the drawbacks of typical ultracapacitor needs membrane to isolate the contact of two electrodes.Micro super capacitor
The transport time of electrolyte ion can be shortened by design effectively, so as to improve charge/discharge rates.Current result of study
Show, micro super capacitor can realize 10 times higher than battery power density and 10-100 times of conventional capacitor energy it is close
Degree, just plays the effect to become more and more important in micro-nano device and system.
According to the difference of energy storage mechnism, ultracapacitor generally can be divided into double electric layers supercapacitor and the super electricity of fake capacitance
Container.The generation of electric double layer capacitance is based primarily upon on electrode/electrolyte interface electric double layer capacitance, such as carbon caused by separation of charge
Electrode capacitor;The generation of fake capacitance is that underpotential deposition occurs on noble metal electrode surface based on electroactive ion, or expensive
The adsorption capacitance that metal oxide electrode surface occurs redox reaction and produces.
The research of ultracapacitor at present is all the time to be lifted based on its stored energy capacitance, especially energy density, and protecting
Effectively mitigate its quality on the premise of demonstrate,proving its capacity, be to need one of major issue for solving at present.
The content of the invention
The object of the present invention is to provide a kind of micro super capacitor making side based on graphene/carbon nano-tube aeroge
Method, the mixed liquor of the graphene oxide configured and carbon nanotubes is injected into extruding device, and three are obtained by three-dimensionally shaped
Electrode is tieed up, reduction is made by being freeze-dried and annealing, and obtains micro super capacitor product, has light weight, specific capacity height
With cycle performance it is excellent the advantages that.
To achieve these goals, the technical solution adopted by the present invention is as follows:
A kind of micro super capacitor production method based on graphene/carbon nano-tube aeroge, the oxidation that will have been configured
Graphene and the mixed liquor of carbon nanotubes are injected into extruding device, and three-dimensional micro-electrode is obtained by three-dimensionally shaped, by freezing
Dry and reduction of annealing, obtain micro super capacitor product.
According to above scheme, comprise the following specific steps that:
1) it is respectively washed pyroceram substrate with isopropanol, acetone, ethanol and deionized water;
2) by carbon nanotubes, graphene oxide and deionized water in mass ratio 3:1:15 mixing, are stirred at room temperature 1-
24h, the graphene/carbon nano-tube mixed solution stirred evenly;
3) pyroceram substrate, processing time 10- are handled under 150-200W power using oxygen gas plasma
20min;
4) the graphene/carbon nano-tube mixed solution of step 2) is injected into extruding device, be expressed into through step 3) place
On pyroceram substrate after reason, three-dimensional micro-electrode is obtained by three-dimensionally shaped;
5) after the moisture evaporation of graphene/carbon nano-tube mixed solution in three-dimensional micro-electrode, freeze-drying process is carried out,
Obtain aeroge interdigitation microelectrode;
6) annealing reduction treatment is carried out to the aeroge interdigitation microelectrode obtained by step 5), reduction-oxidation graphite is made
Alkene/carbon nanotube aerogel micro super capacitor.
According to above scheme, the pyroceram substrate is that specification is 1.5cm × 1.5cm.
According to above scheme, the cleaning pyroceram substrate concretely comprises the following steps:Isopropanol is cleaned by ultrasonic 1 time, when
Between be 15min;EtOH Sonicate cleans 2 times, each 1min;Acetone is cleaned by ultrasonic 2 times, each 1min;Deionized water is cleaned by ultrasonic 2
It is secondary, each 1min;Oxygen gas plasma is handled 1 time, time 5min.
According to above scheme, the freeze-drying process carries out in freeze drier, using liquid nitrogen that sample is cold rapidly
But and drying process 3-4d.
According to above scheme, the annealing reduction treatment is to toast 2h under 400 ο C in tube furnace.
The beneficial effects of the invention are as follows:
1) it is and micro- the present invention provides a kind of production method based on graphene/carbon nano-tube aeroge three-dimensional micro-electrode
The common manufacture craft of type ultracapacitor is compared to having great advantage, using three-dimensionally shaped technological forming microelectrode, and will
The material of graphene oxide and compound and manufactured this high porosity of aeroge of carbon nanotubes improves miniature super as microelectrode
It can also effectively mitigate its quality while level capacitor stored energy capacitance;
2) graphene/carbon nano-tube aeroge of the invention has very high porosity, and specific surface area is larger, so as to
The stored energy capacitance of capacitor is lifted to a certain extent, and after tested, the micro super capacitor is in 10mV s-1Sweep under speed, capacity
For 16.25mF cm-2, after the circulation for carrying out 5000 circles, capacity retention ratio 89.46%, there is excellent energy-storage property;
3) micro super capacitor of the invention can be used for needing in the electronic equipment of fast charging and discharging, proposed by the invention
Manufacture craft precision it is high, the micro super capacitor of obtained this based on graphene/carbon nano-tube aeroge with present
The micro super capacitor developed is compared, and has larger specific capacity and higher mechanical stability, suitable for large-scale production.
Brief description of the drawings
Fig. 1 is the technical process schematic diagram of the present invention;
Fig. 2 is the scanning electron microscope image of 1 product of the embodiment of the present invention;
Fig. 3 is the chemical property collection of illustrative plates of 1 product of the embodiment of the present invention;
Fig. 4 is the Raman spectrum test result figure of 1 product of the embodiment of the present invention.
Embodiment
Technical scheme is illustrated with embodiment below in conjunction with the accompanying drawings.
Embodiment 1, is shown in Fig. 1 to Fig. 4:
The present invention provides a kind of micro super capacitor production method based on graphene/carbon nano-tube aeroge, including
Following specific steps (see Fig. 1):
1) it is respectively washed the pyroceram that specification is 1.5cm × 1.5cm with isopropanol, acetone, ethanol and deionized water
Substrate:Isopropanol is cleaned by ultrasonic 1 time, time 15min;EtOH Sonicate cleans 2 times, each 1min;Acetone is cleaned by ultrasonic 2 times,
Each 1min;Deionized water is cleaned by ultrasonic 2 times, each 1min;Oxygen gas plasma is handled 1 time, time 5min;
2) by carbon nanotubes, graphene oxide and deionized water in mass ratio 3:1:15 mixing, are stirred at room temperature 10h,
The graphene/carbon nano-tube mixed solution stirred evenly;
3) pyroceram substrate, processing time 15min are handled under 180W power using oxygen gas plasma;
4) the graphene/carbon nano-tube mixed solution of step 2) is injected into extruding device, be expressed into through step 3) place
On pyroceram substrate after reason, three-dimensional micro-electrode is obtained by three-dimensionally shaped;
5) after the moisture evaporation of graphene/carbon nano-tube mixed solution in three-dimensional micro-electrode, it is placed in freeze drier
It is dried, sample is cooled down rapidly to simultaneously drying process 3d using liquid nitrogen, obtains aeroge interdigitation microelectrode;
6) under 400 ο C 2h is toasted in tube furnace to the aeroge interdigitation microelectrode obtained by step 5), annealed
Reduction treatment, is made redox graphene/carbon nanotube aerogel micro super capacitor.
Morphology characterization is carried out using scanning electron microscope to the present embodiment products obtained therefrom, as a result as shown in Figure 2.Fig. 2 (a) is graphite
The cross-sectional image of alkene/carbon nanotubes microelectrode, it can be seen that obvious lamination, it was demonstrated that this moulding process is folded for making
The validity of Rotating fields.Fig. 2 (b), (c) and (d) are the cross-section image of graphene/carbon nano-tube microelectrode, graphene in sample
The aeroge microelectrode that lamella and carbon nanotubes are self-assembly of, possesses abundant pore structure and very big specific surface area, is
Ionic adsorption provides abundant site.By scanning electron microscope image it can be found that graphene oxide solution can be very as solvent
Carbon nanotubes is dissolved well, in addition, the carbon nanotubes between being scattered in graphene sheet layer can block between lamella well
Inter-adhesive, both interacts, and the aeroge of net structure can be formed in freezing dry process.
Electrochemical Characterization is carried out to the micro super capacitor of the present embodiment, the result is shown in Fig. 3.Fig. 3 (a) is in 10-
50mV s-1Sweep the cyclic voltammetry curve under speed, the CV curves in Fig. 3 (a) are all class rectangle shapes, illustrate its electric charge storage mechanism
It is the electric double layer capacitance of standard, and response current substantially increases identical multiple with the increase for sweeping speed, this also further body
The electric charge storage mechanism of its electric double layer is showed.Fig. 3 (b) is the micro super capacitor of the present embodiment in 0.2-1.0mAcm-2Electric current
Constant current charge-discharge curve under density, the charging and discharging curve in Fig. 3 (b) are all, and same electric currents triangular shaped compared with standard
The symmetry of charge and discharge curve under density is fine, this has also absolutely proved the electric double layer energy storage mechanism of the microelectrode.Through meter
Calculate, the micro super capacitor is in 10mV s-1Sweep under speed, capacity is 16.25mF cm-2.Fig. 3 (c) is in the present embodiment
Ac impedance spectroscopy (EIS collection of illustrative plates) of the micro super capacitor under 0-500000Hz frequencies, near figure medium-high frequency area
Curve, can estimate its interface resistance for 384 Ω or so;And the low frequency range behind Wa Erbao regions, its slope of curve value is larger, says
It is bright in the case of electrode internal resistance is less, electrolyte ion can quickly be spread between electrode material hole, show carbon-based material
Unique advantage.Fig. 3 (d) is the micro super capacitor of the present embodiment in 500mV s-1The cyclic curve under speed is swept, in 0-
Under the frequency of 500000Hz, it is computed understanding, after the circle of circulation 5000, the capacity retention ratio of the device is 89.46%, shows it
Stable cycle performance.
Raman spectrum test is carried out to the microelectrode in the present embodiment, the result is shown in Fig. 4.As shown in Figure 4:Raman shift
1353cm-1Reply should material unformed peak (D peaks), show the vibration of graphitic carbon crystal edge edge, this peak position is by graphite
What disordered structure and defect produced;Raman shift 1588cm-1Reply should material graphitization peak (G peaks), which is by crystalline state
Graphite SP2Caused by hydridization, crystalline size can be embodied.The intensity ratio for understanding its D peak and G peaks is 1.04 (ID/IG=1.04),
Show after 400 DEG C of annealing reduction, the reducing degree of graphene oxide is higher.
Embodiment 2:
The present invention provides a kind of micro super capacitor production method based on graphene/carbon nano-tube aeroge, makes
Substantially with embodiment 1, difference is step:5h is stirred at room temperature in step 2);Step 3) is existed using oxygen gas plasma
Pyroceram substrate, processing time 20min are handled under 150W power.
Embodiment 3:
The present invention provides a kind of micro super capacitor production method based on graphene/carbon nano-tube aeroge, makes
Substantially with embodiment 1, difference is step:24h is stirred at room temperature in step 2);Step 3) is existed using oxygen gas plasma
Pyroceram substrate, processing time 10min are handled under 200W power.
Above example only to illustrative and not limiting technical scheme, although above-described embodiment to the present invention into
Detailed description is gone, the related technical personnel of this area should be understood:It can modify to the present invention or replace on an equal basis, but
Any modification and local replacement for not departing from spirit and scope of the invention should all be covered in scope of the presently claimed invention.
Claims (6)
1. a kind of micro super capacitor production method based on graphene/carbon nano-tube aeroge, it is characterised in that will configure
Good graphene oxide and the mixed liquor of carbon nanotubes are injected into extruding device, and three-dimensional micro-electrode is obtained by three-dimensionally shaped,
By the reduction that is freeze-dried and anneals, micro super capacitor product is obtained.
2. the micro super capacitor production method according to claim 1 based on graphene/carbon nano-tube aeroge, its
It is characterized in that, comprises the following specific steps that:
1) it is respectively washed pyroceram substrate with isopropanol, acetone, ethanol and deionized water;
2) by carbon nanotubes, graphene oxide and deionized water in mass ratio 3:1:15 mixing, are stirred at room temperature 1-24h, obtain
To the graphene/carbon nano-tube mixed solution stirred evenly;
3) pyroceram substrate, processing time 10-20min are handled under 150-200W power using oxygen gas plasma;
4) the graphene/carbon nano-tube mixed solution of step 2) is injected into extruding device, be expressed into after step 3) processing
Pyroceram substrate on, obtain three-dimensional micro-electrode by three-dimensionally shaped;
5) after the moisture evaporation of graphene/carbon nano-tube mixed solution in three-dimensional micro-electrode, freeze-drying process is carried out, is obtained
Aeroge interdigitation microelectrode;
6) annealing reduction treatment is carried out to the aeroge interdigitation microelectrode obtained by step 5), redox graphene/carbon is made
Nanotube aeroge micro super capacitor.
3. the micro super capacitor production method according to claim 2 based on graphene/carbon nano-tube aeroge, its
It is characterized in that, the pyroceram substrate is that specification is 1.5cm × 1.5cm.
4. the micro super capacitor production method according to claim 2 based on graphene/carbon nano-tube aeroge, its
It is characterized in that, the cleaning pyroceram substrate concretely comprises the following steps:Isopropanol is cleaned by ultrasonic 1 time, time 15min;Second
Alcohol is cleaned by ultrasonic 2 times, each 1min;Acetone is cleaned by ultrasonic 2 times, each 1min;Deionized water is cleaned by ultrasonic 2 times, each 1min;
Oxygen gas plasma is handled 1 time, time 5min.
5. the micro super capacitor production method according to claim 2 based on graphene/carbon nano-tube aeroge, its
It is characterized in that, the freeze-drying process carries out in freeze drier, and sample is cooled down rapidly to simultaneously drying process using liquid nitrogen
3-4d。
6. the micro super capacitor production method according to claim 2 based on graphene/carbon nano-tube aeroge, its
It is characterized in that, the annealing reduction treatment is to toast 2h under 400 ο C in tube furnace.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108584937A (en) * | 2018-07-11 | 2018-09-28 | 济南开发区星火科学技术研究院 | A kind of preparation method of the graphene aerogel of novel compressible rebound |
CN111653436A (en) * | 2020-06-10 | 2020-09-11 | 贵州梅岭电源有限公司 | Application of carbon aerogel/graphene film in flexible supercapacitor |
CN111785918A (en) * | 2020-08-13 | 2020-10-16 | 武汉理工大学 | Preparation method of three-dimensional graphene-based nickel-molybdenum nanowire water-based battery anode |
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CN102074371A (en) * | 2010-12-30 | 2011-05-25 | 清华大学 | Three-dimensional miniature super capacitor electrode manufactured from nano porous composite material and manufacturing method thereof |
CN105161312A (en) * | 2015-09-24 | 2015-12-16 | 复旦大学 | Carbon nano fiber-graphene composite aerogel and cooperative assembly preparation method thereof |
CN107393724A (en) * | 2017-08-11 | 2017-11-24 | 武汉理工大学 | A kind of micro super capacitor preparation method based on graphene/carbon nano-tube aeroge |
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2018
- 2018-01-10 CN CN201810022749.4A patent/CN108010734A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102074371A (en) * | 2010-12-30 | 2011-05-25 | 清华大学 | Three-dimensional miniature super capacitor electrode manufactured from nano porous composite material and manufacturing method thereof |
CN105161312A (en) * | 2015-09-24 | 2015-12-16 | 复旦大学 | Carbon nano fiber-graphene composite aerogel and cooperative assembly preparation method thereof |
CN107393724A (en) * | 2017-08-11 | 2017-11-24 | 武汉理工大学 | A kind of micro super capacitor preparation method based on graphene/carbon nano-tube aeroge |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108584937A (en) * | 2018-07-11 | 2018-09-28 | 济南开发区星火科学技术研究院 | A kind of preparation method of the graphene aerogel of novel compressible rebound |
CN111653436A (en) * | 2020-06-10 | 2020-09-11 | 贵州梅岭电源有限公司 | Application of carbon aerogel/graphene film in flexible supercapacitor |
CN111653436B (en) * | 2020-06-10 | 2022-07-05 | 贵州梅岭电源有限公司 | Application of carbon aerogel/graphene film in flexible supercapacitor |
CN111785918A (en) * | 2020-08-13 | 2020-10-16 | 武汉理工大学 | Preparation method of three-dimensional graphene-based nickel-molybdenum nanowire water-based battery anode |
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