CN103787320B - The Synthesis and applications of the carbon nanosheet material of one kind graphene sheet layer structure - Google Patents
The Synthesis and applications of the carbon nanosheet material of one kind graphene sheet layer structure Download PDFInfo
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- CN103787320B CN103787320B CN201410024281.4A CN201410024281A CN103787320B CN 103787320 B CN103787320 B CN 103787320B CN 201410024281 A CN201410024281 A CN 201410024281A CN 103787320 B CN103787320 B CN 103787320B
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- 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 the preparation method of the carbon nanosheet material of a kind graphene sheet layer structure, belong to carbon nanomaterial field.The present invention utilizes high molecular polymer cheap and easy to get for raw material, by mixing with inorganic salt after simple pre-treatment, carry out under nitrogen protection activating and carbonization, finally carry out re-activation in atmosphere, obtain the New Type of Carbon nanometer sheet of the class graphene film Rotating fields had compared with large specific surface sum superelevation pore volume, as electrode material for super capacitor, there is larger specific capacitance and excellent stable circulation performance, show good chemical property and higher cycle efficiency ratio; In addition, the present invention is with low cost, technique is simple, is conducive to industrialization.
Description
Technical field
The invention belongs to carbon nanomaterial field, relate to the preparation method of the carbon nanosheet material of a kind graphene sheet layer structure; The present invention also relates to the application of carbon nanosheet material as electrode material for super capacitor of such graphene film Rotating fields simultaneously.
Background technology
Ultracapacitor is a kind of Novel energy storage apparatus, and it has, and specific capacitance is large, the duration of charging is short, the feature such as long service life, good temp characteristic and environmental protection.It bridges the function of the high-power output of conventional electrostatic electrical condenser and the high energy storage of battery/fuel cell, is considered to future ideality chemical power source, so have broad application prospects and huge economic benefit.In electrode material for super capacitor, the earliest and most widely used be various forms of carbon materials.Studying the specific surface area, pore size distribution situation, the electroconductibility of material and the surface texture of material that find carbon material is the important factor affecting ultracapacitor performance.In addition, the cost of material is also the factor of required consideration.
Super capacitor carbon electrode material develops into carbon fiber, carbon nanotube and the Graphene etc. extensively studied at present gradually from the gac that specific surface area is the earliest large.Graphene is by the two dimensional crystal carbon material of monoatomic layer.But, its application in actual industrial that what expensive, the shortcoming such as productive rate is low, poor ductility, preparation process are loaded down with trivial details of grapheme material was very large limit.In recent years, there is the carbon nano flake being similar to graphene-structured (laminated layer structure) and present the physics and chemistry character that some are similar to Graphene too, as having high electric conductivity, large specific surface area, excellent chemical stability etc.At present, preparation method's mainly plasma enhanced chemical vapor deposition (PECVD), arc discharge method, template etc. of carbon nano flake, and these methods not only equipment requirements is higher, and output is still lower.
Summary of the invention
The object of the invention is for problems of the prior art, the preparation method of the carbon nanosheet material of a kind graphene sheet layer structure is provided;
Another object of the present invention is to provide a kind of application of carbon nanosheet material as electrode material for super capacitor of such graphene film Rotating fields.
One, the preparation of the carbon nanosheet material of class graphene film Rotating fields
The preparation method of the carbon nanosheet material of class graphene film Rotating fields of the present invention, by after organic high molecular polymer deionized water wash removing impurity, be 1 ~ 3 mol/L NaOH solution, deionized water and washing with alcohol by concentration respectively, remove a small amount of low-molecular-weight polymkeric substance and soluble impurity, fully mix with mineral compound, at N after dry
2pre-activate 1 ~ 4 h under protection, the condition of 250 ~ 450 DEG C, is warming up to 600 ~ 900 DEG C of carbonization 2 ~ 6 h, then in atmosphere, and re-activation 1 ~ 3 h at 200 ~ 300 DEG C; Gained carbon material soaks 6 ~ 48 h in the HCl solution (1 ~ 3 mol/L) of 50 ~ 80 DEG C, is cooled to room temperature, filters, and deionized water wash, to neutral, is drying to obtain.
Described organic high molecular polymer is as at least one in resol, ion exchange resin, urea-formaldehyde resin; Described mineral compound is KOH, Ca (OH)
2, ZnCl
2, NH
4at least one in Cl; The mass ratio of described organic high molecular polymer and mineral compound is 1:1 ~ 1:5.
Described drying is all carry out vacuum-drying at 40 ~ 70 DEG C.
Two, stuctures and properties test
1, structural analysis
Fig. 1 is the microscopic appearance figure of the scanning electron microscope (SEM) of the carbon nanosheet of class graphene-structured prepared by the present invention.As can see from Figure 1, prepared macromolecular compound base carbon-based material is the flaky texture of larger area, its surface accordion in classification.Accordion carbon nano flake can increase the contact area between electrode materials and electrolytic solution as electrode materials, can provide larger electric capacity storage power.
Fig. 2 is nitrogen suction-desorption isotherm figure and the BET specific surface area data of the carbon nanosheet of class graphene-structured prepared by the present invention.This suction-desorption isotherm belongs to typical IV type thermoisopleth, belongs to the adsorpting type of mesopore material.Wherein hole characteristic shortens the transfer path of electronics in electrode materials and electrolytic solution and ion to a great extent, thus can improve the capacity high rate performance of electrode materials.BET test data shows, and the specific surface area of the carbon nanosheet of the class graphene-structured prepared by the present invention is 280 ~ 550 m
2g
-1, and the pore volume had is up to 1.3 ~ 3.2 cm
3g
-1.
2, electrochemical property test
Chemical property appraisement system completes in the three-electrode system of routine, adopts the CHI 660D type electrochemical workstation of Shanghai Chen Hua company limited to test; Cyclical stability test adopts the CT2001A type tester of Wuhan Lan electricity Electronics Co., Ltd..Working electrode is glass-carbon electrode, is platinum electrode to electrode, and reference electrode is saturated calomel electrode, and electrolytic solution is the 6 M KOH aqueous solution.The carbon nanosheet material of class graphene-structured is as the electrode materials of ultracapacitor, and ratio capacitance is 180 ~ 250 Fg
-1.
Fig. 3 is the carbon nanosheet of class graphene-structured prepared by the present invention is 3 A g in current density
-1the lower cyclical stability figure through 5000 charge/discharge test.X-coordinate in figure represents cycle index, and ordinate zou represents that in current density be 3 A g
-1test the ratio capacitance value calculated through charge/discharge down.500 circulations started are electrode materials reactivation process, and ratio capacitance value presents and rises gradually, and then tend towards stability state.After 5000 charge and discharge cycles, ratio capacitance only reduces 2%.Describe its charge and discharge circulation life long, cycle efficiency compares advantages of higher.
Fig. 4 is last 5 the charge/discharge curve figure in 5000 circulations of the class grapheme material prepared of the present invention.As can be seen from Figure 4, charge/discharge curve figure triangular shape symmetrically, illustrates that this material has good efficiency for charge-discharge and excellent capacitance behavior.
Above-mentioned electro-chemical test shows, this carbon nanosheet has large specific capacitance and excellent stable circulation performance as electrode material for super capacitor, is that one has high performance electrode material for super capacitor.
In sum, the present invention utilizes high molecular polymer cheap and easy to get for raw material, by mixing with inorganic salt after simple pre-treatment, carry out under nitrogen protection activating and carbonization, finally carry out re-activation in atmosphere, obtain the New Type of Carbon nanometer sheet of the class graphene film Rotating fields had compared with large specific surface sum superelevation pore volume, as electrode material for super capacitor, there is larger specific capacitance and excellent stable circulation performance, show good chemical property and higher cycle efficiency ratio; In addition, the present invention is with low cost, technique is simple, is conducive to industrialization.
Accompanying drawing explanation
The SEM figure of the carbon nanosheet of the class graphene-structured prepared by Fig. 1.
The nitrogen adsorption desorption isotherm figure of the carbon nanosheet of the class graphene-structured prepared by Fig. 2.
The cyclical stability figure of the carbon nanosheet of the class graphene-structured prepared by Fig. 3.
Fig. 4 is electrode materials is 3A g in current density
-1under charge/discharge curve.
Embodiment
Below by embodiment to the preparation of the carbon nanosheet of invention class graphene-structured be described in detail as the application performance of electrode material for super capacitor.
Embodiment 1
Take the resol of 3 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 1 mol/L, deionized water and washing with alcohol repeatedly respectively, fully mixes with 9g KOH after dry at 60 DEG C; Be placed in tube furnace, at N
2protection, pre-activate 4 h at 250 DEG C, is then warming up to 600 DEG C of carbonization 6h; Take out expose in atmosphere at 200 DEG C (in tube furnace, without N
2protection) carry out re-activation (calcining) 3 h.Gained carbon material is immersed in 12h, then cool to room temperature in the 1 mol/L HCl solution of 80 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 320 m
2g
-1, pore volume is up to 1.9cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 198Fg
-1.
Embodiment 2
Take the ion exchange resin of 2 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 2 mol/L, deionized water and washing with alcohol repeatedly respectively, with 4 g Ca (OH) after dry at 60 DEG C
2abundant mixing; Be placed in tube furnace, at N
2protection, pre-activate 4h at 350 DEG C, is then warming up to 700 DEG C of carbonization 6 h; Take out expose in atmosphere at 200 DEG C (ditto) carry out re-activation 3 h.Gained carbon material is immersed in 24h, then cool to room temperature in the HCl solution (3 mol/L) of 80 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 420 m
2g
-1, pore volume is up to 2.3 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 225Fg
-1.
Embodiment 3
Take the urea-formaldehyde resin of 3 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 2mol/L, deionized water and washing with alcohol repeatedly respectively, with 6 g Ca (OH) after dry at 60 DEG C
2abundant mixing; Be placed in tube furnace, at N
2protection, pre-activate 4h at 450 DEG C, is then warming up to 750 DEG C of carbonization 6 h; After taking out char-forming material expose in atmosphere at 200 DEG C (the same) carry out re-activation 3 h.Gained carbon material is immersed in 12h, then cool to room temperature in the HCl solution (3 mol/L) of 80 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 450 m
2g
-1, pore volume is up to 2.5 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 248Fg
-1.
Embodiment 4
Take the urea-formaldehyde resin of 2 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 3 mol/L, deionized water and washing with alcohol repeatedly respectively, with 8 g ZnCl after dry at 60 DEG C
2abundant mixing; Be placed in tube furnace, at N
2protection, pre-activate 4h at 400 DEG C, is then warming up to 700 DEG C of carbonization 6 h; Take out after expose in atmosphere at 250 DEG C (ditto) carry out re-activation 3 h.Gained carbon material is immersed in 24h, then cool to room temperature in the HCl solution (3 mol/L) of 80 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 490 m
2g
-1, pore volume is up to 3.0 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 246Fg
-1.
Embodiment 5
Take the urea-formaldehyde resin of 2 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 3 mol/L, deionized water and washing with alcohol repeatedly respectively, with 10 g NH after dry at 60 DEG C
4cl fully mixes; Be placed in tube furnace, at N
2protection, pre-activate 4h at 350 DEG C, is then warming up to 900 DEG C of carbonization 2 h; Take out after expose in atmosphere at 300 DEG C (ditto) carry out re-activation 1 h.Gained carbon material is immersed in 12h, then cool to room temperature in the HCl solution (3 mol/L) of 80 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 540 m
2g
-1, pore volume is up to 3.1 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 243Fg
-1.
Embodiment 6
Take the resol of 5g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 3 mol/L, deionized water and washing with alcohol repeatedly respectively, with 7.5 g NH after dry at 60 DEG C
4cl fully mixes; Be placed in tube furnace, at N
2protection, pre-activate 4h at 350 DEG C, is then warming up to 900 DEG C of carbonization 3 h; Take out after expose in atmosphere at 300 DEG C (ditto) carry out re-activation 3 h.Gained carbon material is immersed in 48h, then cool to room temperature in the HCl solution (3 mol/L) of 50 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 470 m
2g
-1, pore volume is up to 1.7 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 247Fg
-1.
Embodiment 7
Take the resol of 5 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 2 mol/L, deionized water and washing with alcohol repeatedly respectively, with 10 g ZnCl after dry at 60 DEG C
2abundant mixing; Be placed in tube furnace, at N
2protection, pre-activate 1 h at 450 DEG C, is then warming up to 900 DEG C of carbonization 4 h; Take out expose in atmosphere at 200 DEG C (ditto) carry out re-activation 3 h.Gained carbon material is immersed in 6 h, then cool to room temperature in the HCl solution (2 mol/L) of 80 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 520 m
2g
-1, pore volume is up to 3.0 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 249Fg
-1.
Embodiment 8
Take the resol of 3 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 3 mol/L, deionized water and washing with alcohol repeatedly respectively, with 9 g Ca (OH) after dry at 60 DEG C
2abundant mixing; Be placed in tube furnace, at N
2protection, pre-activate 3h at 350 DEG C, is then warming up to 800 DEG C of carbonization 5.5 h; Take out expose in atmosphere at 200 DEG C (ditto) carry out re-activation 3 h.Gained carbon material is immersed in 12h, then cool to room temperature in the HCl solution (3 mol/L) of 80 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 480 m
2g
-1, pore volume is up to 2.9 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 231Fg
-1.
Embodiment 9
Take the resol of 5 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 3 mol/L, deionized water and washing with alcohol repeatedly respectively, with 10 g ZnCl after dry at 60 DEG C
2abundant mixing; Be placed in tube furnace, at N
2protection, pre-activate 1h at 450 DEG C, is then warming up to 700 DEG C of carbonization 6 h; Take out expose in atmosphere at 250 DEG C (ditto) carry out re-activation 2 h.Gained carbon material is immersed in 24h, then cool to room temperature in the HCl solution (3 mol/L) of 70 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 350 m
2g
-1, pore volume reaches 1.3 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 243Fg
-1.
Embodiment 10
Take the ion exchange resin of 3 g, remove impurity with deionized water wash, then after using the NaOH solution of concentration 3 mol/L, deionized water and washing with alcohol repeatedly respectively, with 15 g ZnCl after dry at 60 DEG C
2abundant mixing; Be placed in tube furnace, at N
2protection, pre-activate 2h at 300 DEG C, is then warming up to 600 DEG C of carbonization 6 h; Take out expose in atmosphere at 200 DEG C (ditto) carry out re-activation 3 h.Gained carbon material is immersed in 12h, then cool to room temperature in the HCl solution (3 mol/L) of 80 DEG C, filters, with deionized water wash to neutral, dry at 60 DEG C, obtain the carbon nanosheet of class graphene-structured.The specific surface area of carbon nanosheet is 280 m
2g
-1, pore volume reaches 1.6 cm
3g
-1.After testing, using this carbon nanosheet as electrode material for super capacitor, the ratio capacitance in 6mol/L KOH electrolytic solution is 216Fg
-1.
Claims (5)
1. the preparation method of the carbon nanosheet material of a kind graphene sheet layer structure, by after organic high molecular polymer deionized water wash removing impurity, be 1 ~ 3 mol/L NaOH solution, deionized water and washing with alcohol by concentration respectively, fully mix with mineral compound, at N after dry
2pre-activate 1 ~ 4 h under protection, the condition of 250 ~ 450 DEG C, is warming up to 600 ~ 900 DEG C of carbonization 2 ~ 6 h, then in atmosphere, and re-activation 1 ~ 3 h at 200 ~ 300 DEG C; Gained carbon material soaks 6 ~ 48 h in the HCl solution of 50 ~ 80 DEG C, is cooled to room temperature, filters, and deionized water wash, to neutral, is drying to obtain; Described organic high molecular polymer is at least one in resol, ion exchange resin, urea-formaldehyde resin; Described mineral compound is KOH, Ca (OH)
2, ZnCl
2, NH
4at least one in Cl.
2. the preparation method of the carbon nanosheet material of class graphene film Rotating fields as claimed in claim 1, is characterized in that: the mass ratio of organic high molecular polymer and mineral compound is 1:1 ~ 1:5.
3. the preparation method of the carbon nanosheet material of class graphene film Rotating fields as claimed in claim 1, is characterized in that: the concentration of described HCl solution is 1 ~ 3 mol/L.
4. the preparation method of the carbon nanosheet material of class graphene film Rotating fields as claimed in claim 1, is characterized in that: described drying is vacuum-drying at 40 ~ 60 DEG C.
5. as claimed in claim 1 the carbon nanosheet material of class graphene film Rotating fields prepared of method as the application of electrode material for super capacitor.
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Cited By (1)
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| US11824198B2 (en) | 2018-01-03 | 2023-11-21 | Samsung Electronics Co., Ltd. | Silicon composite cluster and carbon composite thereof, and electrode, lithium battery, and electronic device each including the same |
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| CN104495796B (en) * | 2014-11-25 | 2016-08-17 | 武汉科技大学 | The method preparing porous class grapheme material for raw material with Herba Eichhorniae |
| CN104445177B (en) * | 2014-12-16 | 2016-09-28 | 中国科学院宁波材料技术与工程研究所 | The preparation method of a kind of Graphene and Graphene |
| CN105645399B (en) * | 2016-03-15 | 2017-12-12 | 南京大学（苏州）高新技术研究院 | A kind of preparation method of the high-performance super capacitor three-dimensional few layer porous graphene of classification self-similarity |
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| CN108648925A (en) * | 2018-04-17 | 2018-10-12 | 东华大学 | A kind of carbon nanotube-carbon nanosheet nano-hybrid material and its preparation and application |
| CN108751164B (en) * | 2018-05-30 | 2020-02-07 | 湘潭大学 | Red petal-string-based graphene porous carbon nanosheet and preparation method and application thereof |
| CN109592676B (en) * | 2018-12-14 | 2021-12-21 | 东华大学 | Preparation method of carbon nano composite material derived from carbon nanosheet matrix grown on graphene oxide |
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Cited By (1)
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