CN107331537A - A kind of preparation method and application of three-dimensional grapheme/graphite-phase nitrogen carbide - Google Patents
A kind of preparation method and application of three-dimensional grapheme/graphite-phase nitrogen carbide Download PDFInfo
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- CN107331537A CN107331537A CN201710659399.8A CN201710659399A CN107331537A CN 107331537 A CN107331537 A CN 107331537A CN 201710659399 A CN201710659399 A CN 201710659399A CN 107331537 A CN107331537 A CN 107331537A
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- dimensional grapheme
- graphite
- preparation
- phase nitrogen
- nitrogen carbide
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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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- 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
-
- 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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- 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 an a kind of one step preparation method of the three-dimensional grapheme based on hydro-thermal method/graphite-phase nitrogen carbide.The preparation of the material is by using ultrasonic method by graphene oxide（GO）With graphite-phase nitrogen carbide（g‑C3N4）After mixing, hydro-thermal reaction is carried out, with g C while GO is reduced during the course of the reaction3N4Hydrogel post is assembled into, afterwards by freeze-drying, three-dimensional grapheme/g C are obtained3N4.Simple to operate the present invention relates in, environmental protection, cost is low, and process conditions are easily achieved, prepared three-dimensional grapheme/g C3N4Composite there is the higher pore structure of degree of orientation；In addition, the composite has higher specific capacitance, there is potential application value in terms of ultracapacitor.
Description
Technical field
The invention belongs to technical field of inorganic nano-material preparation, more particularly to a kind of three-dimensional grapheme/graphite-phase carbonization
The preparation method and application of nitrogen.
Background technology
Ultracapacitor is as a kind of emerging energy storage device, power density and good cycle life by its superelevation
Huge application potential is shown in green energy resource etc. advantage, the extensive concern of researcher is caused.Wherein, electrode material is
Influence the key factor of ultracapacitor chemical property, and graphene is as a kind of new carbon material, by high conductivity,
The features such as high theoretical specific surface area, excellent mechanical performance, shows excellent electrochemical properties in supercapacitor applications.
Grapheme material can be self-assembled into macroscopical graphene block with microscopic three-dimensional network structure by pi-pi bond, and can be direct
Electrode material as ultracapacitor improves the ratio shared by active material, simplified without binding agent and conductive agent
Number of assembling steps.However, the relatively low specific capacitance of graphene limits its further development.g-C3N4Possess similar graphenesp 2Two
Structure is tieed up, and with abundant nitrogen-atoms and defect, its higher electro-chemical activity is imparted, in recent years in catalysis, the energy
In terms of all arrived extensive concern.If by g-C3N4It is compound with graphene, strengthen composite wood using the synergy of the two
The chemical property of material, will be a frontier for being worth exploring and studying.
The content of the invention
It is an object of the invention to provide a kind of preparation method of three-dimensional grapheme/graphite-phase nitrogen carbide, for solving carbon
The relatively low technical problem of specific capacitance that based super capacitor material is present.
The step of a kind of preparation method of three-dimensional grapheme/graphite-phase nitrogen carbide, this method, is as follows：
（1）Graphene oxide is configured to graphene oxide solution according to a certain percentage in deionized water, concentration is 1-3 mg/
mL；
（2）By g-C3N4It is added to step（1）In graphene oxide solution in, afterwards using low temperature ultrasonic method by mixture point
Dissipate uniform, form mixed solution, g-C3N4Mass ratio with graphene oxide is：1:4-1:10；
（3）By step（2）The mixed solution is transferred in hydrothermal reaction kettle, in 150-200 DEG C of baking oven in air dry oven
Interior reaction 10-20 h, obtain graphene/g-C3N4；
（4）With deionized water cleaning step repeatedly（3）Products therefrom, freeze-drying, freeze-drying temperature is -40 DEG C, and freezing is dry
The dry time is 24h.
Further, step（2）Described in g-C3N42 h are calcined by melamine at 550 DEG C to obtain.
Further, step（2）The condition of low temperature ultrasonic mixing is 0 ~ 15 DEG C.
Pass through three-dimensional grapheme/g-C of above-mentioned acquisition3N4With clear advantage.With three-dimensional grapheme/g-C3N4As
Electrode material for super capacitor, can play following advantage：g-C3N4Addition cause product have height-oriented property hole tie
Structure, can fully and electrolyte contacts so that electrochemical reaction can be carried out fully, and the connected three-dimensional grapheme of hole
Network structure can provide a quick conductive channel for electric transmission, with three-dimensional grapheme/g-C3N4It is used as ultracapacitor
Material has good capacitive property.
The present invention has advantages below compared with prior art：
1. the present invention prepares three-dimensional grapheme/g-C using hydro-thermal method3N4, using water as reducing agent, method environmental protection.
2. present invention process is simple, a step is to realize three-dimensional grapheme/g-C3N4, required instrument and equipment is simple, it is easy to grasp
Make, production cost is low, has a wide range of application, beneficial to industrialization promotion.
Brief description of the drawings
Fig. 1 is three-dimensional grapheme/g-C prepared by embodiment 13N4Hydrogel post（a）And after section is lyophilized（b）Optics shine
Piece.
Fig. 2 is three-dimensional grapheme/g-C prepared by embodiment 13N4Scanning electron microscopic picture.
Fig. 3 is three-dimensional grapheme/g-C prepared by embodiment 13N4In 5,10,20 mV s-1The cyclic voltammetric swept under speed is bent
Line chart（a）With 0.5,1,2A g-1Constant current charge-discharge curve map under current density（b）.
Fig. 4 is three-dimensional grapheme/g-C prepared by embodiment 23N4In 5,10,20 mV s-1The cyclic voltammetric swept under speed is bent
Line chart（a）With in 0.5,1,2 A g-1Constant current charge-discharge curve map under current density（b）.
Embodiment
Specific embodiment is chosen according to technical scheme of the present invention to be described as follows：
The microscopic appearance of prepared sample is observed in the present invention using Tai Siken Mira3-LMH types SEM；Adopt
Surveyed with A Meiteke-Princeton PMC-2000 multi-channel electrochemicals work station come the chemical property to prepared sample
Examination.
Embodiment 1：
40 mg graphene oxides are dispersed in 20mL deionized waters, low temperature at 10 mg graphite-phase nitrogen carbides, 10 DEG C is added and surpasses
Sound mixing 3h, mixed solution is transferred in stainless steel hydrothermal reaction kettle, in being incubated 12h at 180 DEG C, naturally cools to room temperature,
Graphene/graphite-phase nitrogen carbide hydrogel post is obtained, cuts into slices, product is washed with deionized 3 times, after -40 DEG C of freeze-dryings i.e.
Obtain three-dimensional grapheme/g-C3N4。
Fig. 1 is three-dimensional grapheme/g-C prepared by embodiment 13N4Hydrogel post（a）And after section is lyophilized（b）Optics shine
Piece, by Fig. 1（a）（b）In it can be seen that three-dimensional grapheme/g-C for being obtained of the present embodiment3N4Hydrogel post has well-regulated post
Shape pattern, regular edges；And shape keeps preferable after lyophilized, can directly as ultracapacitor electrode material.Fig. 2 is real
Apply three-dimensional grapheme/g-C prepared by example 13N4Scanning electron microscope diagram piece, as can be seen from the figure the present embodiment obtained
Three-dimensional grapheme/the g-C obtained3N4With three-dimensional network structure.Fig. 3（a）,（b）Graphene/g- that respectively prepared by embodiment 1
C3N4In 5,10,20 mV s-1Sweep cyclic voltammetry curve figure under speed and in 0.5,1,2 A g-1Constant current under current density fills
Discharge curve.From Fig. 3（a）As can be seen that above-mentioned three-dimensional grapheme/g-C3N4With good high rate performance；From Fig. 3（b）In
It can be seen that charging and discharging curve has typical electric double layer capacitance characteristic, be respectively 0.5 A g in current density-1, 1 A g-1, 2A
g-1Under, specific capacitance can be obtained by calculating, be respectively：135 F g-1, 116 F g-1, 102 F g-1, with higher specific capacitance；
It can be used as electrode material for super capacitor.
Embodiment 2：
50 mg graphene oxides are dispersed in 20mL deionized waters, low temperature ultrasonic at 5mg graphite-phase nitrogen carbides, 12 DEG C is added
3h is mixed, mixed solution is transferred in stainless steel hydrothermal reaction kettle, in being incubated 10h at 160 DEG C, room temperature is naturally cooled to and obtains
Three-dimensional grapheme/g-C3N4Hydrogel post, section, is washed with deionized product 3 times, and three-dimensional is obtained after -40 DEG C of freeze-dryings
Graphene/g-C3N4。
Above example is served only for being further described in detail technical scheme, and not the present invention is appointed
What is limited, and some nonessential modifications and adaptations that those skilled in the art makes according to the above of the present invention are belonged to
The protection domain of technical solution of the present invention.
Claims (5)
1. the preparation method of a kind of three-dimensional grapheme/graphite-phase nitrogen carbide, it is characterised in that this method comprises the following steps：
（1）Graphene oxide is configured to graphene oxide solution according to a certain percentage in deionized water, concentration is 1-3 mg/
mL；
（2）By g-C3N4It is added to step（1）In graphene oxide solution in, afterwards using low temperature ultrasonic method by mixture point
Dissipate uniform, form mixed solution, g-C3N4Mass ratio with graphene oxide is：1:4-1:10；
（3）By step（2）The mixed solution is transferred in hydrothermal reaction kettle, in 150-200 DEG C of baking oven in air dry oven
Interior reaction 10-20 h, obtain graphene/g-C3N4；
（4）With deionized water cleaning step repeatedly（3）Products therefrom, freeze-drying, freeze-drying temperature is -40 DEG C, and freezing is dry
The dry time is 24h.
2. a kind of preparation method of three-dimensional grapheme/graphite-phase nitrogen carbide according to claim 1, it is characterised in that：Step
Suddenly（2）Described in g-C3N42 h are calcined by melamine at 550 DEG C to obtain.
3. a kind of preparation method of three-dimensional grapheme/graphite-phase nitrogen carbide according to claim 1 or 2, it is characterised in that：
Step（2）The condition of low temperature ultrasonic mixing is 0 ~ 15 DEG C.
4. a kind of preparation method of three-dimensional grapheme/graphite-phase nitrogen carbide according to claim 1 or 2, it is characterised in that：
Prepared graphene/g-C3N4With the higher three-dimensional network of orientation.
5. the three-dimensional grapheme obtained by claim 1/application of the graphite-phase nitrogen carbide in ultracapacitor.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108198697A (en) * | 2018-01-22 | 2018-06-22 | 上海理工大学 | A kind of electrode material for super capacitor and preparation method thereof |
| CN108311172A (en) * | 2018-02-09 | 2018-07-24 | 江苏大学 | A kind of nonmetallic 1D/2D composite material and preparation methods and application |
| CN108624195A (en) * | 2018-06-07 | 2018-10-09 | 西南石油大学 | A kind of g-C3N4The preparation method of-G/ water-base epoxy composite coatings |
| CN109003831A (en) * | 2018-07-25 | 2018-12-14 | 重庆交通大学 | A kind of carbonitride/graphene combination electrode material and preparation method thereof |
| CN111659451A (en) * | 2020-07-14 | 2020-09-15 | 中国科学院山西煤炭化学研究所 | Preparation method and application of nitrogen vacancy-containing few-layer porous carbon nitride photocatalyst |
| CN112435859A (en) * | 2020-11-12 | 2021-03-02 | 西北工业大学 | Super capacitor adopting superstructure graphene foam and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103021662A (en) * | 2012-12-11 | 2013-04-03 | 常州大学 | Nanometer multilayer mesoporous metal nitride/graphene composite materials for super capacitor and preparation method thereof |
| CN103769187A (en) * | 2013-12-18 | 2014-05-07 | 江苏悦达新材料科技有限公司 | Preparation method of graphene/g-C3N4 compound photocatalyst |
| CN104843680A (en) * | 2015-04-03 | 2015-08-19 | 北京理工大学 | Method for batch preparation of graphene from microcrystalline graphite |
| CN105498821A (en) * | 2015-12-17 | 2016-04-20 | 苏州大学 | Composite material used for catalyzing and degrading nitrogen oxide and preparation method and application thereof |
| CN106540732A (en) * | 2016-10-20 | 2017-03-29 | 中国石油大学(北京) | A kind of redox graphene/mesoporous graphitization carbon nitride material and preparation method |
| CN106732738A (en) * | 2017-02-15 | 2017-05-31 | 东华大学 | A kind of Graphene/g C3N4Three-dimensional network laminated film and its preparation and application |
-
2017
- 2017-08-04 CN CN201710659399.8A patent/CN107331537A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103021662A (en) * | 2012-12-11 | 2013-04-03 | 常州大学 | Nanometer multilayer mesoporous metal nitride/graphene composite materials for super capacitor and preparation method thereof |
| CN103769187A (en) * | 2013-12-18 | 2014-05-07 | 江苏悦达新材料科技有限公司 | Preparation method of graphene/g-C3N4 compound photocatalyst |
| CN104843680A (en) * | 2015-04-03 | 2015-08-19 | 北京理工大学 | Method for batch preparation of graphene from microcrystalline graphite |
| CN105498821A (en) * | 2015-12-17 | 2016-04-20 | 苏州大学 | Composite material used for catalyzing and degrading nitrogen oxide and preparation method and application thereof |
| CN106540732A (en) * | 2016-10-20 | 2017-03-29 | 中国石油大学(北京) | A kind of redox graphene/mesoporous graphitization carbon nitride material and preparation method |
| CN106732738A (en) * | 2017-02-15 | 2017-05-31 | 东华大学 | A kind of Graphene/g C3N4Three-dimensional network laminated film and its preparation and application |
Non-Patent Citations (3)
| Title |
|---|
| JUNHUA SONG等: ""Tuning the structure and composition of graphite-phase polymeric carbon nitride/reduced graphene oxide composites towards enhanced lithium-sulfur batteries performance"", 《ELECTROCHIMICA ACTA》 * |
| QING CHEN等: ""Three-dimensional graphitic carbon nitride functionalized graphene-based high-performance supercapacitors"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| YANGBIN DING等: ""Porous nitrogen-rich carbon materials from carbon self-repairing g-C3N4 assembled with graphene for high-performance supercapacitor"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108198697A (en) * | 2018-01-22 | 2018-06-22 | 上海理工大学 | A kind of electrode material for super capacitor and preparation method thereof |
| CN108198697B (en) * | 2018-01-22 | 2019-07-23 | 上海理工大学 | A kind of electrode material for super capacitor and preparation method thereof |
| CN108311172A (en) * | 2018-02-09 | 2018-07-24 | 江苏大学 | A kind of nonmetallic 1D/2D composite material and preparation methods and application |
| CN108311172B (en) * | 2018-02-09 | 2019-12-31 | 江苏大学 | Nonmetal 1D/2D composite material and preparation method and application thereof |
| CN108624195A (en) * | 2018-06-07 | 2018-10-09 | 西南石油大学 | A kind of g-C3N4The preparation method of-G/ water-base epoxy composite coatings |
| CN109003831A (en) * | 2018-07-25 | 2018-12-14 | 重庆交通大学 | A kind of carbonitride/graphene combination electrode material and preparation method thereof |
| CN111659451A (en) * | 2020-07-14 | 2020-09-15 | 中国科学院山西煤炭化学研究所 | Preparation method and application of nitrogen vacancy-containing few-layer porous carbon nitride photocatalyst |
| CN111659451B (en) * | 2020-07-14 | 2023-03-24 | 中国科学院山西煤炭化学研究所 | Preparation method and application of nitrogen vacancy-containing few-layer porous carbon nitride photocatalyst |
| CN112435859A (en) * | 2020-11-12 | 2021-03-02 | 西北工业大学 | Super capacitor adopting superstructure graphene foam and preparation method thereof |
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Application publication date: 20171107 |