CN109887763A - A kind of multiple micro nano structure carbon material and preparation method having conductive energy storage effect - Google Patents
A kind of multiple micro nano structure carbon material and preparation method having conductive energy storage effect Download PDFInfo
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- CN109887763A CN109887763A CN201910066100.7A CN201910066100A CN109887763A CN 109887763 A CN109887763 A CN 109887763A CN 201910066100 A CN201910066100 A CN 201910066100A CN 109887763 A CN109887763 A CN 109887763A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of multiple micro nano structure carbon materials and preparation method thereof for having conductive energy storage effect, which includes nano-sized carbon lamella, and is distributed carbon nanotube thereon and the bowl-shape carbon of nanometer；The nano-sized carbon lamella with a thickness of 50-300nm, length and width are micron order；The diameter of the bowl-shape carbon structure of nanometer is 20-250nm, wall thickness 5-30nm.Raw material is not used only by the present invention, and cost is relatively low, and gained carbon material has superior electric conductivity compared to existing product, charging and discharging capabilities can be improved, higher power density is provided, improve cycle life, there is huge specific surface area simultaneously, substantially increase volumetric capacitance and quality specific capacitance, and then promote performance of the supercapacitor.
Description
Technical field
The invention belongs to electrode material for super capacitor fields, and in particular to a kind of multiple micro-nano for having conductive energy storage effect
Rice structure carbon material and preparation method.
Background technique
Supercapacitor is big by feat of its specific capacity, charge/discharge speed is fast, the features such as having extended cycle life becomes research now
Popular one of electrochemical energy storage field, the type and property of performance and composition electrode material have substantial connection.Super capacitor
Device is broadly divided into double layer capacitor and two kinds of fake capacitance capacitor, wherein common supercapacitor capacitance material is with leading
Metal oxide, conducting polymer and the carbon material etc. of electric energy storage property.Wherein carbon material is with its good chemical stability, good
Good conductivity, abundance, the features such as cost is relatively low, have been applied to already in the electrode system of energy storage device, for making
Standby double layer capacitor.
Active carbon is a kind of common carbon material, is most widely used work in the double layer capacitor of current business application
Property material.Active carbon be usually as obtained from carbon containing material roast under anaerobic environment and is carbonized, can be from a variety of more
(for example, lignocellulosic, pitch, coal etc.) is obtained in the carbonaceous presoma of sample, but is also needed by chemical activation, physically activated
Or both combine activation method increase its surface area after could use.Active carbon has high conductivity, high-specific surface area, change
The features such as property is stablized is learned, is the widest capacitor electrode material of current business application, however that there is also specific capacitances is lower
Problem.
Patent CN201710562960.0 " preparation method and active carbon of active carbon " discloses a kind of preparation of active carbon
Stalk is carbonized to obtain carbide by method under protective gas atmosphere at 300 DEG C~400 DEG C；By the carbide
It is uniformly mixed to obtain mixture with highly basic, the mass ratio of the carbide and highly basic is 1:3~1:4；In protective gas atmosphere
Under, the mixture is carried out to activation processing at 500 DEG C~800 DEG C and obtains pre-product within 1 hour~2 hours；And it will be described pre-
Product is immersed in inorganic acid, is kept the temperature 1 hour~2 hours at 80 DEG C~90 DEG C and is obtained active carbon.
As can be seen that the method for currently preparing absorbent charcoal material is needed using a variety of activation methods, and multistep is needed to heat
Processing, causes greatly to bear to environment.
In view of the deficiencies of the prior art, the technical issues of present invention intends to solve is to provide a kind of micro-nano with novel multiple
The complex carbon material of structure.The material preparation process is simple, environment protecting and power-saving, and has the structure and excellent property of innovation
Can, there is good prospect.
Summary of the invention
To solve the shortcomings and deficiencies of the prior art, the purpose of the present invention is to provide one kind to have conductive energy storage to act on
Multiple micro nano structure carbon material and preparation method.
Present invention design utilizes corncob composite carbon nanometer tube, and the carbon/carbon compound material with special surface pattern is made,
It can be used for preparing the electrode of supercapacitor.Corncob has natural hole configurations, is for preparing the good of active carbon
Raw material can obtain the carbon material of the porous spongy structure formed by the nano-sized carbon lamella to interlink, together after carbonization
When, it is the mesoporous of 2-50nm that aperture is dispersed on lamella.And after corncob enveloped carbon nanometer tube/EVA is allowed to carbonization again, both may be used
Retain corncob and be conducive to the activated carbon structure and the good chemical property of carbon nanotube of Ion transfer originally, and creates new
Nanoscale Surface bowl structure greatly improves the specific surface area of material, can promote the absorption of electrolyte on the surface of the material, increases
Add wetability, the performance of capacitor can be promoted applied to the electrode material of supercapacitor, there is broad mass market prospect.
The purpose of the invention is achieved by the following technical solution:
A kind of multiple micro nano structure carbon material having conductive energy storage effect, including nano-sized carbon lamella, and it is distributed in it
On the bowl-shape carbon of carbon nanotube and nanometer；The nano-sized carbon lamella with a thickness of 50-300nm, length and width are micron order；The nanometer
The diameter of bowl-shape carbon structure is 20-300nm, wall thickness 5-30nm.
Preferably, the meso-hole structure of 2-20nm is dispersed on the nano-sized carbon lamella.
Preferably, the carbon nanotube is single wall or multi-walled carbon nanotube, diameter 15-50nm.
Preferably, the multiple micro nano structure carbon material specific capacitance be 80-300F/g (in alkaline electrolyte, permanent electricity
Stream charge and discharge electrical method is under the current density of 1A/g subject to data measured).
A kind of preparation method for the multiple micro nano structure carbon material having conductive energy storage effect, includes the following steps:
Corncob is added in CNT/CTAB/EVA dispersion liquid and is impregnated；Soaking corncob is taken out, heats carbon after dry
Change, the cooling multiple micro nano structure carbon material that conductive energy storage effect can be obtained；
The corncob, CNT, CTAB, EVA mass ratio be 5:(0.5-1): (0.5-2): 1.
Preferably, the CNT/CTAB/EVA dispersion liquid preparation steps are as follows: it is added CNT into CTAB solution, ultrasonic vibration,
Disperse CNT tentatively；EVA solution is added, obtains CNT/CTAB/EVA dispersion liquid after ultrasonic vibration.
Preferably, the soaking time is 3-48h.
Preferably, the corncob is first pre-processed, the pre-treatment step are as follows: corncob is successively used to clear water, nothing
After water-ethanol, clear water washing, is dried at 70 DEG C, be broken into the fritter of 1-3mm.
Preferably, the heating carbonization refers to is heated to 800-1000 DEG C in a nitrogen atmosphere, keeps the temperature 0.5-4h.
The principle of the present invention is:
Corn core itself contains natural porous structure, and pure corncob can form packet after high-temperature heating carbonization
Porous structure carbon containing many micron order apertures, and after the carbonization of the structures such as original cell wall, it is the lamella of thickness 50-200nm
Structure.
Multi-walled carbon nanotube (MWCNT) is under field conditions (factors) since specific surface area is minimum, and surface can be high, it may occur that naturally
Reunite, be not easy to disperse, it is difficult to be constructed to stablize the dispersion liquid of preservation.CTAB is a kind of cationic surfactant, is dissolved
After in a solvent, CNT can adsorb CTAB molecule in dispersion process, can tentatively disperse in a solvent after ultrasonic disperse.EVA is dissolved in
After solvent, the macromolecular chain of dispersion in the solution is formed, after two kinds of dispersion liquids are mixed simultaneously ultrasonic disperse, EVA macromolecular chain meeting
It is inserted between the CNT tentatively dispersed, CNT is steadily suspended in the solution, reach monodispersed state.
After corncob is immersed among CNT/CTAB/EVA dispersion liquid, since the biological tissue of corncob has polarity,
EVA strand also has polarity, and EVA strand occurs absorption with biological tissue and combine in which will be slow, at the same by part CNT and
CTAB is also secured on corncob, after taking out drying, forms corncob/CNT/CTAB/EVA compound.Solvent volatilization, EVA is not
It will form the film for completely covering corn chip layer, but form the bulge-structure of distribution.
Compound is put into Muffle furnace, is slowly heated to that a period of time is heated and kept the temperature in the high temperature of 800-1000 degree,
Biological tissue in corncob can be carbonized with EVA, wherein corncob is carbonized to form porous sheet carbon material.And EVA exists
During heating is heated to 300 degree or so, liquid can be changed into first, while CTAB can form chondritic wherein.?
EVA molten liquid is gathered in CTAB micellar surface and forms small vesica under the action of surface tension, with temperature continue increase and
Carbonization takes place.When between 300-400 degree, Surfactant CTAB is decomposed, and discharges gas, and EVA vesica occurs broken
It damages and collapses, then continue that carbonization occurs, shrink, form the carbon with the bowl-shape carbon triplen of carbon plate layer/carbon nanotube/nano
Material.
The present invention has the following advantages and effects with respect to the prior art:
The production cost of electrode material for super capacitor can be greatly reduced in the present invention.
1. cost is relatively low for raw material used herein.Current industrialization application electrode material for super capacitor be mainly
The cocoanut active charcoal and activity of bitumen charcoal being modified.Primary raw material used in the present invention includes that the corncob inside corn ear is useless
Material, ethylene-vinyl acetate plastics (EVA) and multi-walled carbon nanotube.Wherein, there are few need cost for corncob waste material；EVA plastics are
The extremely mature general-purpose plastics of development, price are very low；Multi-walled carbon nanotube passes through the development of many years, and present price has been reduced to
Within 2000 yuan/kilogram, has industrial application value, and carbon nanotube dosage is less in the present invention, improves into not too highly
This.In contrast, the material prices such as the graphene being often used in research are also in the high price of 500 yuan/gram or more, are not used to
Industrial production.
2. electric conductivity is the primary condition that electrode material for super capacitor plays capacitive property, products obtained therefrom of the present invention is carbon
Material, compared to the conducting polymers such as polyaniline, polypyrrole or MnO2Equal transition metal oxides, have superior conduction
Property, charging and discharging capabilities can be improved, higher power density is provided, improve cycle life；Meanwhile compared to the carbon of simple tubulose
There is micron order lamellar structure carbon-to-carbon to receive for nanotube, graphene on chip or spherical polyaniline particles, products therefrom of the present invention
The special MULTIPLE COMPOSITE structure of mitron-nanoscale bowl structure carbon has huge specific surface area, substantially increases volume ratio electricity
Appearance and quality specific capacitance, and then promote performance of the supercapacitor.
3. present invention process is simple, step is less, can shorten the production cycle, reduces energy consumption.In the present invention, by solution
The corncob of immersion treatment only needs that the carbon with special multiplet can be obtained by the heat treatment of a step inert atmosphere
Material does not need multistep heat treatment, does not need to play simplified technique, reduction using the activator harmful to environment yet
The effect of cost.
Detailed description of the invention
Fig. 1 (a)-(c) is the surface topography map of 1 resulting materials of embodiment.
Fig. 2 is the cyclic voltammetry curve of 1 resulting materials of embodiment.
Fig. 3 is the cycle charge-discharge curve of 1 resulting materials of embodiment.
Fig. 4 is the AC impedance spectral curve of 1 resulting materials of embodiment.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
A kind of preparation method for the multiple micro nano structure carbon material having conductive energy storage effect, includes the following steps:
1. after 0.25g corncob is successively washed with clear water, dehydrated alcohol, clear water, being dried at 70 DEG C, being broken into 1-
The fritter of 3mm；
2. 0.05g CTAB is added in tetrahydrofuran, 0.05g CNT is then added, ultrasonic vibration divides CNT tentatively
It dissipates, obtains CTAB/CNT solution；The 0.05g EVA particle that VA content is 32% is dissolved in dimethylbenzene again, with the CTAB/CNT
Solution mixes, and 50mL CNT/CTAB/EVA dispersion liquid is obtained after ultrasonic vibration；
Taken out afterwards for 24 hours 3. 0.25g corncob is added in the CNT/CTAB/EVA dispersion liquid to impregnate, it is dry, and by with
The resulting corncob of lower parameter carbonization: 25 DEG C of initial temperature；800 DEG C of pyrolysis temperature；5 DEG C/min of heating rate；Holding temperature 800
℃；Soaking time 2h.
Figure of description 1 (a)-(c) is the surface topography map of 1 resulting materials of embodiment, and (a) is nano-sized carbon lamella, thickness
About 200nm, length and width reach a few micrometers；It (b) is shape appearance figure of the bowl-shape structure growth of nanometer on nanoscale twins；It (c) is nano bowl
The enlarged drawing of shape structure.Wherein, the diameter of bowl structure carbon is 20-300nm, and wall thickness 10-30nm, lamellar structure thickness is about
200nm, a few micrometers of length and width.
Fig. 2-4 is that the cyclic voltammetry curve of 1 resulting materials of embodiment, cycle charge-discharge curve and AC impedance are set a song to music respectively
Line.
As seen from Figure 2, volt-ampere curve is the symmetrical image close to rectangle, illustrates that providing capacitor is good electric double layer
Capacitor.
As seen from Figure 3, charging and discharging curve almost symmetry, calculate specific capacitance be 200F/g.
As seen from Figure 4, curve is typical double layer capacitor image, and material resistance is minimum, i.e. good conductivity.
Embodiment 2
In addition to solvent is 40mL dimethylbenzene+10mL tetrahydrofuran, remaining parameter and step ginseng in solution used in step 2
See embodiment 1.Resulting materials have structure similar to Example 1 in the present embodiment, and bowl structure diameter is 20-50nm, wall
Thickness is 5-10nm, and measuring specific capacitance is 140F/g.
Embodiment 3
In addition to soaking time is 48h in step 3, and pyrolysis temperature is 900 DEG C outer, remaining parameter and step are referring to embodiment
1.Resulting materials have structure similar to Example 1 in the present embodiment, and bowl structure diameter is 20-50nm, wall thickness 5-
10nm, measuring specific capacitance is 112F/g.
Embodiment 4
In addition to solvent is 45mL tetrahydrofuran+5mL water in solution used in step 2, remaining parameter and step are referring to reality
Apply example 1.Resulting materials have structure similar to Example 1 in the present embodiment, and bowl structure diameter is 100-150nm, wall thickness
For 10-20nm, and it is larger perpendicular to length on the direction of carbon plate, cylindrical, measuring specific capacitance is 170F/g.
Embodiment 5
In addition to solvent is 45mL tetrahydrofuran+5mL water, and the heating schedule in step 3 in solution used in step 2
Are as follows: 25 degree of initial temperature, 200 DEG C of heat preservation 30min are warming up to the speed of 5 DEG C/min, then be warming up to the speed of 5 DEG C/min
800 DEG C of heat preservation 120min.Remaining parameter and step are referring to embodiment 1.Resulting materials have similar to Example 1 in the present embodiment
Structure, bowl structure diameter is 100-150nm, wall thickness 10-30nm, and larger perpendicular to the length on carbon plate direction, is in
It is cylindric.Measuring specific capacitance is 220F/g.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of multiple micro nano structure carbon material for having conductive energy storage effect, which is characterized in that including nano-sized carbon lamella, and
It is distributed carbon nanotube thereon and the bowl-shape carbon of nanometer；The nano-sized carbon lamella with a thickness of 50-300nm, length and width are micron order；
The diameter of the bowl-shape carbon structure of nanometer is 20-300nm, wall thickness 5-30nm.
2. a kind of multiple micro nano structure carbon material for having conductive energy storage effect according to claim 1, which is characterized in that
The meso-hole structure of 2-20nm is dispersed on the nano-sized carbon lamella.
3. a kind of multiple micro nano structure carbon material for having conductive energy storage effect according to claim 1, which is characterized in that
The carbon nanotube is single wall or multi-walled carbon nanotube, diameter 15-50nm.
4. a kind of multiple micro nano structure carbon material for having conductive energy storage effect according to claim 1, which is characterized in that
The multiple micro nano structure carbon material specific capacitance is 80-300F/g.
5. a kind of preparation method for the multiple micro nano structure carbon material for having conductive energy storage effect, which is characterized in that including as follows
Step:
Corncob is added in CNT/CTAB/EVA dispersion liquid and is impregnated；Soaking corncob is taken out, carbonization is heated after dry, it is cold
But the multiple micro nano structure carbon material of conductive energy storage effect can be obtained；
The corncob, CNT, CTAB, EVA mass ratio be 5:(0.5-1): (0.5-2): 1.
6. a kind of preparation method of multiple micro nano structure carbon material for having conductive energy storage effect according to claim 5,
It is characterized in that, the CNT/CTAB/EVA dispersion liquid preparation steps are as follows: CNT is added into CTAB solution, ultrasonic vibration makes
CNT tentatively disperses；EVA solution is added, obtains CNT/CTAB/EVA dispersion liquid after ultrasonic vibration.
7. a kind of preparation method of multiple micro nano structure carbon material for having conductive energy storage effect according to claim 5,
It is characterized in that, the soaking time is 3-48h.
8. a kind of preparation method of multiple micro nano structure carbon material for having conductive energy storage effect according to claim 5,
It is characterized in that, the corncob is first pre-processed, the pre-treatment step are as follows: corncob is successively used to clear water, anhydrous second
After alcohol, clear water washing, is dried at 70 DEG C, be broken into the fritter of 1-3mm.
9. a kind of preparation method of multiple micro nano structure carbon material for having conductive energy storage effect according to claim 5,
It is characterized in that, the heating carbonization refers to is heated to 800-1000 DEG C in a nitrogen atmosphere, 0.5-4h is kept the temperature.
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