CN106783198A - A kind of carbon foam combination electrode material of three dimensional elasticity N doping and preparation method thereof - Google Patents
A kind of carbon foam combination electrode material of three dimensional elasticity N doping and preparation method thereof Download PDFInfo
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- CN106783198A CN106783198A CN201611015429.3A CN201611015429A CN106783198A CN 106783198 A CN106783198 A CN 106783198A CN 201611015429 A CN201611015429 A CN 201611015429A CN 106783198 A CN106783198 A CN 106783198A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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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- 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 provides a kind of carbon foam combination electrode material of three dimensional elasticity N doping, it is composited with melamine sponge by graphene oxide.Present invention also offers the preparation method of above-mentioned combination electrode material, graphene oxide is dissolved in deionized water under ultrasound condition at room temperature, obtains graphene oxide dispersion soln；Melamine sponge is soaked in above-mentioned solution, ultrasound causes that graphene oxide is scattered in melamine sponge；After by above-mentioned gained sample drying, 600 900 DEG C of heat treatments are warming up under inert atmosphere, then Temperature fall, obtain the carbon foam combination electrode material of three dimensional elasticity N doping.The present invention not only has big specific surface area, excellent circulation ability using the three dimensional elasticity nitrogen-doped carbon foam NCF RGO composites that ultrasound is obtained with high temperature cabonization facture, and it is carbon-nitrogen doped make surface charge store fast reaction, shorten transportation route, it is preferable new energy materialses, can be used as electrode material.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of combination electrode material of three-dimensional hierarchical structure, specifically one
Plant the carbon foam of three dimensional elasticity N doping（NCF-RGO）Combination electrode material and preparation method thereof.
Background technology
With the fast development of society, energy and environment are the two big subject matters that human kind sustainable development faces.With
Non-renewable energy resources such as oil, natural gas, coal etc. are slowly exhausted, and reproducible clean energy resource is rapidly developed.In new energy
While obtaining broad development, a key issue for being badly in need of solving also is faced with：How effectively to store and change these energy
Measure, therefore various save energy technologies, the development and utilization of Environmental Technology and clean reproducible new energy technology are received
More broadly pay close attention to, such as electric automobile, solar energy, wind energy and heat energy.The either development of electric automobile industry or two
The utilization of the secondary energy, it is wherein vital link to find suitable energy storage device.At present, the energy storage technology of ultracapacitor
Get growing concern for.Capacitor is a kind of new type of energy storage device between traditional capacitor and battery, mainly
Energy is stored by Physical Mechanism, with vast capacity, good cycling stability, discharge and recharge fast, high power density and to environment
Pollution-free the advantages of, it is fully utilized in fields such as traffic, military affairs, space flight and aviation, electronic devices now, as global new
One of study hotspot of energy field.
Current most commercialized electrode material is mainly based on carbon material, but its cyclical stability is poor, charge and discharge
The shortcomings of electric overlong time and too small specific surface area, limit it and use on a large scale.Graphene has big specific surface area, holds
The ionic weight received is big, and superpower electric conductivity and power density is big.And N doping porous carbon can provide the height for accommodating electric charge
The loose structure of surface area, the carbon atom of the nitrogen that adulterates provides enhanced electrolyte wettability and electron conduction, while having
High circulation ability so that have good application prospect in electrochemistry.But the nitrating porous carbon that current laboratory is studied
There is certain defect, the porous carbon skeleton that great drawback introduces NCF in the fabrication process inevitably hinders electro transfer
With its electro-chemical activity of weakening.
The content of the invention
It is multiple the invention provides a kind of carbon foam of three dimensional elasticity N doping for above-mentioned technical problem of the prior art
Composite electrode material and preparation method thereof, the carbon foam combination electrode material of described this three dimensional elasticity N doping and its preparation side
Method will solve nitrating porous carbon of the prior art and introduce the porous carbon skeleton obstruction electro transfer of NCF in the fabrication process and cut
The technical problem of weak its electro-chemical activity.
The invention provides a kind of carbon foam combination electrode material of three dimensional elasticity N doping, by graphene oxide and trimerization
Cyanamide sponge is composited.
Present invention also offers a kind of preparation method of the carbon foam combination electrode material of above-mentioned three dimensional elasticity N doping,
Comprise the following steps：
1) at room temperature, graphene oxide is dissolved in deionized water under ultrasound condition, graphite oxide is obtained after 5-30 minutes
Alkene dispersion soln, the molar concentration of graphene oxide is 1-4mol/L；
2) melamine sponge is soaked in step 1）Solution in, ultrasonic 0.5-2h so that graphene oxide is scattered in trimerization
In cyanamide sponge；
3) by step 2）After gained sample drying, it is heat-treated under inert atmosphere, in heat treatment process, first with 4-6 DEG C/min's
Speed is warming up to 600-900 DEG C, is incubated 0.5-2 hour afterwards, then Temperature fall, obtains the carbon bubble of three dimensional elasticity N doping
Foam combination electrode material.
Further, step 2）In, the volume of melamine sponge is 2 × 2 × 2-5 × 5 × 5 cm3。
Further, step 3）In, drying temperature is 50-80 DEG C, and the time is 3-6 hours.
The present invention is with graphene oxide（GO）It is carbon source, melamine sponge（MS）It is carbon nitrogen source, by ultrasonic infusion method,
So that graphene oxide is well-dispersed in MS, high temperature cabonization obtains nitrogen-doped carbon foam afterwards（NCF-RGO）.The present invention is used
The three dimensional elasticity nitrogen-doped carbon foam NCF-RGO composites that ultrasound is obtained with high temperature cabonization facture, are a kind of classifying porous
Structure NCF-RGO is combined, and not only with big specific surface area, excellent circulation ability, and carbon-nitrogen doped makes surface charge
Storage fast reaction, shortens transportation route, is one of preferable energy and material, can be used as electrode material.
The composite obtained by the method for the present invention has big specific surface area and hierarchical porous structure, increases material
With the contact area of electrolyte, be conducive to the quick transmission of electronics；Of a relatively high nitrogen content, increased reactivity site,
So as to improve the adsorption rate of electronics；The melamine sponge material for having resilient three-dimensional skeleton simultaneously has good electric conductivity
And cyclical stability, environment will not also be caused harm.
The present invention is compared with prior art, and its technological progress is significant.The present invention take full advantage of graphene oxide and
The coupling of melamine sponge, the NCF-RGO composites obtained with high-temperature process method using ultrasound, its specific surface area is high
Up to 563.4 m2 g-1And with prominent circulation ability, after the circle of circulation 10000, specific capacity stills remain in 96%.Meanwhile, carbon
N doping can make material surface electric charge store fast reaction, shorten transportation route, be one of preferable energy and material.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the NCF-RGO composites of the gained of embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the NCF-RGO composites of the gained of embodiment 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of the NCF-RGO composites of the gained of embodiment 2.
Fig. 4 is the scanning electron microscope (SEM) photograph of the NCF-RGO composites of the gained of embodiment 2.
Fig. 5 is the scanning electron microscope (SEM) photograph of the NCF-RGO composites of the gained of embodiment 3.
Fig. 6 is the scanning electron microscope (SEM) photograph of the NCF-RGO composites of the gained of embodiment 3.
Fig. 7 is the scanning electron microscope (SEM) photograph of the NCF-RGO composites of the gained of embodiment 4.
Fig. 8 is the scanning electron microscope (SEM) photograph of the NCF-RGO composites of the gained of embodiment 4.
Fig. 9 is the NCF-RGO composite chemical property figures obtained by embodiment 1-4.
Figure 10 is the NCF-RGO composite XRD spectrums of the gained of embodiment 3.
Specific embodiment
The present invention is expanded on further below by specific embodiment and with reference to accompanying drawing, but is not intended to limit the present invention.
Embodiment 1
A kind of preparation method of NCF-RGO three-dimensionals hierarchical structure electrode material, comprises the following steps：
（1）Graphene oxide（GO）Preparation use improved Hummers methods, synthesis step include pre-oxidation and secondary oxidation.
（2）Melamine sponge is thoroughly washed with ethanol and deionized water first, standby after then drying for a period of time.
（3）Prepare GO dispersion solns：
A. 3mL graphene oxides (1mol/L) are taken in 100mL beakers；
B. 20mL deionized waters are added in the beaker of a steps and ultrasonic 5 min, obtain graphene oxide dispersion soln.
（4）Prepare NCF-RGO：
A. first, 2 × 2 × 2 cm for above-mentioned steps (2) being obtained3MS is added to above-mentioned（3）The GO dispersions of gained are molten
In liquid, and ultrasonic 0.5 h；
B. then a gained raw materials are put into 50 DEG C of baking ovens and are dried, the dry time is 3 hours；
C. the mixture obtained by b is put into nitrogen furnace, 600 DEG C, insulation 0.5 is warming up to the speed of 4 DEG C/min under a nitrogen
Hour, Temperature fall had both obtained three-dimensional graphite alkenyl N doping porous carbon composite.
Using field emission scanning electron microscope（German Zeiss ultra 55）Instrument, sweeps to NCF-RGO samples
Retouch, the scanning electron microscope (SEM) photograph of gained as shown in Figure 1, 2, can be seen that the three-dimensional sheet structure of composite, thus table from Fig. 1,2
Clear graphene oxide is supported on three-dimensional melamine sponge well, and successfully preparing NCF-RGO has big specific surface
Product, while having larger aperture.
Embodiment 2
A kind of preparation method of NCF-RGO three-dimensionals hierarchical structure electrode material, comprises the following steps：
（1）Graphene oxide（GO）Preparation use improved Hummers methods, synthesis step include pre-oxidation and secondary oxidation.
（2）Melamine sponge is thoroughly washed with ethanol and deionized water first, standby after then drying for a period of time.
（3）Prepare GO dispersion solns：
A. 3mL graphene oxides (2mol/L) are taken in 100mL beakers；
B. 30mL deionized waters are added in the beaker of a steps and ultrasonic 10 min, obtain graphene oxide dispersion soln.
（4）Prepare NCF-RGO：
A. first, 3 × 3 × 3 cm for above-mentioned steps (2) being obtained3MS is added to above-mentioned（3）The GO dispersions of gained are molten
In liquid, and ultrasound 1h；
B. then a gained raw materials are put into 60 DEG C of baking ovens and are dried, the dry time is 4 hours；
C. the mixture obtained by b is put into nitrogen furnace, is warming up to 700 DEG C with the speed of 5 DEG C/min under a nitrogen, insulation 1 is small
When, Temperature fall had both obtained three-dimensional graphite alkenyl N doping porous carbon composite.
Using field emission scanning electron microscope（German Zeiss ultra 55）Instrument, sweeps to NCF-RGO samples
Retouch, the scanning electron microscope (SEM) photograph of gained as shown in Figure 3,4, can be seen that the three-dimensional sheet structure of composite, thus table from Fig. 3,4
Clear graphene oxide is supported on three-dimensional melamine sponge well, and successfully preparing NCF-RGO has big specific surface
Product, while having larger aperture.
Embodiment 3
A kind of preparation method of NCF-RGO three-dimensionals hierarchical structure electrode material, comprises the following steps：
（1）Graphene oxide（GO）Preparation use improved Hummers methods, synthesis step include pre-oxidation and secondary oxidation.
（2）Melamine sponge is thoroughly washed with ethanol and deionized water first, standby after then drying for a period of time.
（3）Prepare GO dispersion solns：
A. 3mL graphene oxides (3mol/L) are taken in 100mL beakers；
B. 40mL deionized waters are added in the beaker of a steps and ultrasonic 20 min, obtain graphene oxide dispersion soln.
（4）Prepare NCF-RGO：
A. first, 4 × 4 × 4 cm for above-mentioned steps (2) being obtained3MS is added to above-mentioned（3）The GO dispersions of gained are molten
In liquid, and ultrasonic 1.5 h；
B. then a gained raw materials are put into 70 DEG C of baking ovens and are dried, the dry time is 5 hours；
C. the mixture obtained by b is put into nitrogen furnace, 800 DEG C, insulation 1.5 is warming up to the speed of 5 DEG C/min under a nitrogen
Hour, Temperature fall had both obtained three-dimensional graphite alkenyl N doping porous carbon composite.
Using field emission scanning electron microscope（German Zeiss ultra 55）Instrument, sweeps to NCF-RGO samples
Retouch, the scanning electron microscope (SEM) photograph of gained as shown in Figure 5,6, can be seen that the three-dimensional sheet structure of composite, thus table from Fig. 5,6
Clear graphene oxide is supported on three-dimensional melamine sponge well, and successfully preparing NCF-RGO has big specific surface
Product, while having larger aperture.
Embodiment 4
A kind of preparation method of NCF-RGO three-dimensionals hierarchical structure electrode material, comprises the following steps：
（1）Graphene oxide（GO）Preparation use improved Hummers methods, synthesis step include pre-oxidation and secondary oxidation.
（2）Melamine sponge is thoroughly washed with ethanol and deionized water first, standby after then drying for a period of time.
（3）Prepare GO dispersion solns：
A. 3mL graphene oxides (4mol/L) are taken in 100mL beakers；
B. 50mL deionized waters are added in the beaker of a steps and ultrasonic 30 min, obtain graphene oxide dispersion soln.
（4）Prepare NCF-RGO：
A. first, 5 × 5 × 5 cm for above-mentioned steps (2) being obtained3MS is added to above-mentioned（3）The GO dispersions of gained are molten
In liquid, and ultrasonic 2 h；
B. then a gained raw materials are put into 80 DEG C of baking ovens and are dried, the dry time is 6 hours；
C. the mixture obtained by b is put into nitrogen furnace, is warming up to 900 DEG C with the speed of 6 DEG C/min under a nitrogen, insulation 2 is small
When, Temperature fall had both obtained three-dimensional graphite alkenyl N doping porous carbon composite.
Using field emission scanning electron microscope（German Zeiss ultra 55）Instrument, sweeps to NCF-RGO samples
Retouch, the scanning electron microscope (SEM) photograph of gained as shown in Figure 7,8, can be seen that the three-dimensional sheet structure of composite, thus table from Fig. 7,8
Clear graphene oxide is supported on three-dimensional melamine sponge well, and successfully preparing NCF-RGO has big specific surface
Product, while having larger aperture.
In sum, the present invention prepare a kind of NCF-RGO three-dimensional hierarchical structure electrode material have big specific surface area,
Prominent circulation ability, and it is carbon-nitrogen doped make surface charge store fast reaction.Tested using three electrode capacitors,
Electrolyte is 6mol/L KOH, and normal electrode is inertia Pt electrodes, and reference electrode is Ag/AgCl electrodes, and working electrode is load
The Pt nets of active material.Prepared chemical property as shown in figure 9, under the sweep speed of 10mV/s, the electricity of every kind of material
The area of chemical window is different, and the wherein electrochemical window of NCF-RGO-800 is more bigger than other different materials, so
The chemical property of 800 DEG C of calcining gained NCF-RGO three-dimensional hierarchical structure electrode materials is best；As shown in Figure 10,800 DEG C of calcinings
The XRD spectrum of gained NCF-RGO-800 three-dimensional hierarchical structure electrode materials, it can be seen that the successful preparation of the composite, and
And have good crystallinity；By the electron microscope of comparison diagram 1-8,800 DEG C of calcining gained NCF-RGO three-dimensionals stratum knots
Structure electrode material with substantial amounts of microgap hole, while N doping porous carbon can be well echoed one with graphene oxide
Rise.
The above is only specifically enumerating for embodiments of the present invention, and according to appointing that technical scheme is made
What equivalent transformation, all should belong to protection scope of the present invention.
Claims (4)
1. a kind of carbon foam combination electrode material of three dimensional elasticity N doping, it is characterised in that：By graphene oxide and melamine
Amine sponge is composited.
2. a kind of preparation method of the carbon foam combination electrode material of the three dimensional elasticity N doping described in claim 1, its feature
It is to comprise the following steps：
1）At room temperature, graphene oxide is dissolved in deionized water under ultrasound condition, graphite oxide is obtained after 5-30 minutes
Alkene dispersion soln, the molar concentration of graphene oxide is 1-4 mol/L；
2）Melamine sponge is soaked in step 1）Solution in, ultrasonic 0.5-2 h so that graphene oxide is scattered in trimerization
In cyanamide sponge；
3）By step 2）After gained sample drying, it is heat-treated under inert atmosphere, in heat treatment process, first with 4-6 DEG C/min's
Speed is warming up to 600-900 DEG C, is incubated 0.5-2 hour afterwards, then Temperature fall, obtains the carbon bubble of three dimensional elasticity N doping
Foam combination electrode material.
3. preparation method according to claim 2, it is characterised in that step 2）In, the volume of melamine sponge is 2
× 2 × 2 -5 × 5 × 5 cm3。
4. preparation method according to claim 2, it is characterised in that step 3）In, drying temperature is 50-80 DEG C, time
It is 3-6 hours.
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Cited By (13)
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| CN107802261A (en) * | 2017-11-14 | 2018-03-16 | 复旦大学 | Dry disposable flexible electrocardioelectrode and preparation method thereof |
| CN107895786A (en) * | 2017-11-15 | 2018-04-10 | 晋中学院 | Flexible self-supporting SnS/ carbon foam composites and its preparation method and application |
| CN108074751A (en) * | 2017-12-08 | 2018-05-25 | 中北大学 | A kind of flexible 3 D porous carbon materials and its preparation method and application |
| CN108199014A (en) * | 2017-12-07 | 2018-06-22 | 银隆新能源股份有限公司 | A kind of porous nitrogen-doped carbon/Fe2O3/ grapheme foam flexible composite, preparation method and applications |
| CN108400023A (en) * | 2018-03-15 | 2018-08-14 | 上海应用技术大学 | A kind of three-dimensional nitrogen-doped carbon foam combination electrode material and preparation method thereof |
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| CN108545797A (en) * | 2018-04-11 | 2018-09-18 | 吉林大学 | A kind of flexible composite and preparation method thereof for sea water desalination |
| CN108609603A (en) * | 2018-05-27 | 2018-10-02 | 南京航空航天大学 | A kind of carbon foam and preparation method thereof containing graphite ene coatings |
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| CN109437147A (en) * | 2018-10-31 | 2019-03-08 | 石狮市川大先进高分子材料研究中心 | A kind of preparation method of multifunctional C foam |
| CN109943066A (en) * | 2019-04-17 | 2019-06-28 | 河南科技大学 | Monomer cast nylon polymeric material with three dimensional network structure, preparation method and applications |
| CN109943066B (en) * | 2019-04-17 | 2021-07-16 | 河南科技大学 | Cast nylon polymeric material with three-dimensional grid structure, preparation method and application thereof |
| CN112397320A (en) * | 2020-11-06 | 2021-02-23 | 大连理工大学 | Nitrogen-doped hierarchical pore integral carbon material applied to supercapacitor and preparation method thereof |
| CN113398970A (en) * | 2021-06-07 | 2021-09-17 | 武汉工程大学 | ZnO nanowire array/three-dimensional nitrogen-doped rGO nanotube composite material and preparation method and application thereof |
| CN113551814A (en) * | 2021-06-23 | 2021-10-26 | 浙江工业大学 | Preparation method and application of electrode material with carbon/MOF three-dimensional continuum structure |
| CN115193409A (en) * | 2022-07-15 | 2022-10-18 | 中国石油大学(华东) | Photo-thermal adsorption heavy oil material based on modified melamine sponge, and preparation and application thereof |
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Application publication date: 20170531 |